CA1279795C - Oil filters using water-based latex binders - Google Patents
Oil filters using water-based latex bindersInfo
- Publication number
- CA1279795C CA1279795C CA000493253A CA493253A CA1279795C CA 1279795 C CA1279795 C CA 1279795C CA 000493253 A CA000493253 A CA 000493253A CA 493253 A CA493253 A CA 493253A CA 1279795 C CA1279795 C CA 1279795C
- Authority
- CA
- Canada
- Prior art keywords
- latex
- weight
- cross
- carbon atoms
- filter
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
- B01D39/1607—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
- B01D39/1623—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin
- B01D39/163—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin sintered or bonded
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/37—Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylates
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/38—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing crosslinkable groups
- D21H17/39—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing crosslinkable groups forming ether crosslinkages, e.g. alkylol groups
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/41—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing ionic groups
- D21H17/42—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing ionic groups anionic
- D21H17/43—Carboxyl groups or derivatives thereof
Abstract
ABSTRACT OF THE DISCLOSURE
This invention relates to impregnated oil filter substrate and to oil filters containing such impregnated substrates that require a single cure and can pass a hot oil immersion test, said filter substrate being impregnated with a water-based binder comprising a latex containing at least 20% polymerized vinyl chloride in the latex solids, said latex being a copolymer of vinyl chloride, 30 to 60% lower alkyl acrylate, and one or more comonomers selected from acrylic acid and N-methylol acrylamide, said comonomers being used in an amount of up to 5%, based on the weight of the monomers used to make the latex;
said binder also containing 5 to 20 parts of a cross-linking resin per 100 weight parts of latex solids and 5 to 20% catalyst for the cross-linking resin based on the weight of the cross-linking resin.
This invention relates to impregnated oil filter substrate and to oil filters containing such impregnated substrates that require a single cure and can pass a hot oil immersion test, said filter substrate being impregnated with a water-based binder comprising a latex containing at least 20% polymerized vinyl chloride in the latex solids, said latex being a copolymer of vinyl chloride, 30 to 60% lower alkyl acrylate, and one or more comonomers selected from acrylic acid and N-methylol acrylamide, said comonomers being used in an amount of up to 5%, based on the weight of the monomers used to make the latex;
said binder also containing 5 to 20 parts of a cross-linking resin per 100 weight parts of latex solids and 5 to 20% catalyst for the cross-linking resin based on the weight of the cross-linking resin.
Description
~ t~ 5 OIL FILTERS USING WATER-BASED LATEX B ~ DERS
BACKGROUND OF T~E INVENTIGN
_ The paper used as the filtration medium for automotive type filters has been traditionally treated with phenolic resole type resins. This has been done to improve the paper's strength properties and allow it to be pleated in an accordian-like shape and to hold this shape when the paper composite is cured.
The standard phenolic resin used to treat automotive filter paper had relatively low mol ratios, on the order of 1.0/1 to 1~3/1 formaldehyde to phenol. This has been necessary so that good final paper properties, especially flexibility, could be achieved. Higher mol ratio resins tend to result in brittle paper on curing.
The traditional method of making an automotive filter has been for a paper maker to treat a base filter sheet with an alcohol solution of these phenolic resole resins. The treated sheet was passed through an oven to drive off the solvent and make a so-called B-stage sheet. This sheet was then shipped to the filter maker where it was pleated and put through an oven to further cure the sheet and to hold the shape of the pleats.
With the onset of greater concern for environmental quality, the filter manufacturers have requested paper suppliers to supply a formaldehyde-free impregnated sheet that holds its pleat, and meets all of the requirements for oil filters.
This invention is directed to oil filters and oil filter media impregnated with a water-based latex containing polymerized vinyl chloride. Such oil filters are manufactured with only a single cure and ~;~
'' 1'`,' , ' , :
g~3~
do not impair the environment by emitting volatile solvents.
SUMMARY OF THE ~ VENTION
Impregnated oil filter media and oil filters incorporating same are made by impregnating an oil filter substra-te, for example paper or a suitable nonwoven, with an aqueous la-tex selected from homo-polymers of a vinyl halide or a vinylidene halide and copolymers wherein a vinyl halide and/or a vinylidene halide is polymerized with other co-monomers. Manufacture of such oil filters does not c~n-tr~bute to any air pollution through escape of a volatile solvent.
DETAILED DESCRIPTICN OF THE INVENTION
The use of a water-based binder in making impregnated paper or nonwoven for oil filters is desirable from at least one point of view: the elimination of the volatile solvent used in the past in connection with phenolic binders. The volatile solvent, such as an alcohol, was detrimental in that it contributed to air polution when the filter medium was dried thus releasing the alcohol into the atmosphere. The use of volatile solvents in such operations is bein~ curtailed in response to ever more stringent environmental controls.
In an attempt to produce oil filters with a water-based binder, several aqueous latexes were tried, all, however, unsuccessfully. Such binders included polyvinyl chloride, acrylonitrile/butadiene, butadiene/styrene/arylonitrile, acrylate/styrene, and other latexes. Composites based on these water-based binders lacked the necessary stability in the hot oil immersion test in that the resin binder was extracted into the hot oil.
Following the initial unsuccessful attempts with water-based binders, several additional composite ~>'~ 79 S
samples were prepared with various aqueous latexes cross-linked with a variety of cross-linking agents.
In carrying out these experiments, conventional unbonded filter paper was saturated with these crosslinkable binders, and the saturated filter paper was then evaluated by an outside party that commercially produces impregnated filter paper for the oil filter manufacturers. After a thorough evaluation, crosslinkable polyvinyl chloride latex was selected as a suitable binder in the production of impregnated oil filter medium whereas the other binders were not suitable.
Therefore, this invention is directed to oil filters and oil filter media selected from filter paper and nonwovens impregnated with a crosslinkable aqueous polyvinyl halide latex. The resulting impregnated oil filter media have the necessary resistance to hot oil and meet other physical properties. The latex described herein is admixed with a cross-linking resin and a catalyst for the cross-linking resin before it is used to impregnate filter paper or a nonwoven filter substrate which is then dried and cured at an elevated temperature. The latex solids, prior to impregnation, are adjusted with water to a solids content of about 5 to 70~, preferably 10 to 30~, and pH thereof is adjusted to about 4 to 12, preferably to the alkaline side oE 7 to 9. ..
Suitable polymeric aqueous latexes ~or saturating or impregnating filter paper or a nonwoven filter medium are selected from homopolymers of a vinyl halide or a vinylidene halide and copolymers of a vinyl halide and/or vinylidene halide with other copolymerizable monomers. In a preEerred embodiment, suitable latexes are selected from homopolymers of 3 7 g 3 vinyl chloride and copolymers of vinyl chloride with other copolymerizable monomers. Amount of polymerized vinyl chloride in such latexes can vary from a minimum oE about 5% by weight up to 100% for the homopolymers, -5 but preEerably the copolymers contain at least about 20% of polymerized vinyl chlori~e and most preferably contain in excess of about 40% polymerized vinyl chloride. Preerred polymers in the latexes have Tg in the range of 0C to 100C but more preferabïy 20C
to 50C.
There is a large variety of comonomers that can be polymerized with a vinyl halide in producing aqueous copolymer latexes. The term "copolymer", for purposes herein, defines a polymer of two or more 15 monomers. On the basis of this definition, vinyl halide and/or vinylidene halide, preferably vinyl chloride, can be copolymerized with one or more of comonomers such as ~ olefinically unsaturated carboxylic acids containing 3 to 5 carbon atoms, such as acrylic, methacrylic, ethacrylic and cyanoacrylic acids; monounsaturated dicarboxylic acids containing 4 to 8 carbon atoms, such as fumaric and maleic acids;
esters of ~ olefinically unsaturated carboxylic acids containing 3 to 5 carbon atoms and monounsaturated dicarboxylic acids containing 4 to 20 but preferably 4 to 12 carbon atoms, such as methyl acrylate, ethyl acrylate, butyl acrylate, 2-ethylhexyl acrylate, octyl acrylate, ethyleneglycol dimethacrylate, diethylene glycol diacrylate, cyanoethyl acrylate, methyl methacrylate, butyl methacrylate, hydroxypropyl methacrylate, ethyl maleate, butyl fumarate, maleic dimethyl ester, maleic acid mono-(2-ethylhexyl)ester, fumaric acid diethyl ester, and fumaric acid dilauryl ester;
~,~-olefinically unsaturated nitriles containing 3 to .
: ' :, ' ' ,;' ' ' ' ~
~ 79 5 carbon atoms, such as acrylonitrile and methacrylonitrile; acrylamides derived from acrylic and methacrylic acids and their N-alkylol and ~-alkoxyalkyl derivatives containing l to 20 but preferably l to 12 carbon atoms, such as acrylamide itself, ~-methylol acrylamide, N-butoxy methacrylamide, methylenebisacrylamide, methacrylamide, ~l-octyl acrylamide, diacetone acrylamide, and hydroxymethyl diacetone acrylamide;
vinyl ethers containing 4 to 22 caron atoms, such as ethyl vinyl ether, chloroethyl vinyl ether, isobutyl vinyl ether, cetyl vinyl ether, and lauryl vinyl ether; vinyl ketones containing 3 to 12 carbon atoms, such as methyl vinyl ketone; vinyl esters of carboxylic acids containing 4 to 22 carbon atoms, such as vinyl acetate, vinyl propionate, vinyl formate, vinyl stearate, vinyl benzoate, and vinyl and allyl chloroacetate; ~-ole~ins containing 2 to 12 carbon atoms, such as ethylene, propylene, isobutylene, and butene-l; styrene and styrene derivatives such as ~-methyl styrene, vinyl toluene, and chlorostyrene;
and othér polyfunctional monomers such as vinyl naphthalene, vinyl pyridine, divinyl benzene, and allyl pentaerythritol.
Preferred latexes are copolymers of vinyl chloride, a lower alkyl acryate, and an acrylic acid.
Amount of vinyl chloride in such latexes generally exceeds 40% by weight of the monomer weight, preEerably being in the range of about 40 to 70 dry weight parts, whereas the lower alkyl acrylate is used in an amount exceeding 20~ of the total monomer weight, preferably being in the range of about 30 to 60 dry weight parts. Amount of an acrylic acid, preferably acrylic acid itself, is use in an amount of up to about 5~ of total monomer weight, preferably 3 7~`~
about 0.5 to 3 weight parts. The amounts given herein in weight parts are based on a total of 100 weight parts of all monomers in the latex. As used herein, the "lower" alkyl acrylate monomer is defined as containing about 1 to 8 carbon atoms in the alkyl moiety. The preferred latexes can also contain about 0.5 to 2 weight parts of an alkylol acrylamidé
containing 1 to 4 carbon atoms in the alkylol group.
Amount of the alkylol acrylamide is based on 100 weight part of all the monomers in the latex.
Preferred latexes are prepared by emulsion polymeriæation of vinyl chloride and one or more comonomers. Comonomers for the preferred latexes include acrylic and methacrylic acids and alkyl esters derived therefrom which contain 1 to 20 carbon atoms, preferably 2 to 12, in the alkyl group; amides derived from ,~-olefinically unsaturated carboxylic acids and their N-alkylol and N-alkoxyalkyl derivatives such as acrylamide, N-octyl acrylamide, and hydroxymethyl diacetone acrylamide; and vinylidene halides, such as vinylidene chloride. Specific examples of preferred latexes containing polyvinyl chloride are copolymers of the following monomers: vinyl chloride, 2-ethylhexyl acrylate, vinylidene chloride, and acrylic acid; vinyl chloride, 2-ethylhexyl acrylate, vinylidene chloride, and hydroxymethyl diacetone acrylamide; vinyl chloride and methyl acrylate; vinyl chloride, butyl acrylate, acrylic acid, and N-methylol acrylamide; and vinyl chloride, 2-ethylhexyl acrylate, vinylidene chloride, and hydroxypropyl methacrylate.
The latexes can be plasticized or unplasticized.
The polymer latexes embodied herein are prepared employing conventional polymerization techniques in an aqueous medium with a suitable polymerization catalyst. Overpolymerization of the , '' .
monomers may also be employed. A~ueous dispersions of solution polymers may be used.
The a~ueous medium may be emulsifier-Eree or it may contain an emulsifier. When emulsifiers are used to prepare the latexes of this invention, the usual types of anionic and non-ionic emulsifiers may be employed. Useful anionic emulsifiers include alkali metal or ammonium salts of the sulfates of alcohols having from 8 to 18 carbon atoms such as sodium lauryl sulfate; ethanolamine lauryl sulEate, ethylamine lauryl sulfate; alkali metal and ammonium salts of sulfonated petroleum and paraffin oils;
sodium salts of sulfonic acids such as dodecane-l-sulfonic acid and octadiene-l-sulfonic acid; aralkyl sulfonates such as sodium isopropyl benzene sulfonate, sodium dodecyl benzene sulfonate and sodium isobutyl naphthalene sulfonate; alkali metal and ammonium salts of sulfonated dicarboxylic acid esters such as sodium dioctyl sulfosuccinate, disodium-n-octadecyl sulfosuccinamate; alkali metal or ammonium salts of the free acid of complex organic mono- and diphosphate esters; and the like. Non-ionic emulsifiers such as octyl- or nonylphenyl polyethoxyethanol may also be used. Latexes having excellent stability are obtained with the alkali metal and ammonium salts of aromatic sulfonic acids, aralkyl sulfonates, long chain alkyl sulfonates and poly(oxyalkylene~sulfcnates.
If an emulsifier is used, this may range up to about 6~ or more by weight based on the rnonomers, but it preferably is less than 6~, and excellent results have been obtained with less than 1%. The emulsifier may be entirely added at the outset of the polymerization or it may be added incrementally or by proportioning throughout the run. Typically, a ~nall ' , .
. .
9-~
amount of the emulsifier is added at the outset of the polymerization and the remainder charged incrementally or proportionately to the reactor as the monomers are proportioned.
S The polymerization may be conducted at temperatures from about 0C or less to about 100C in the presence of a compound capable of initiating the polymerizations. Commonly used free radical initiators include the various peroxygen compounds such as persulfate, benzoyl peroxide, t-butyl hydroperoxide, cumene hydroperoxide, t-butyl diperphthalate, pelargonyl peroxide and l-hydroxycyclohexyl hydroperoxide; azo compounds such as azodiisobutyronitrile and dimethylazodiisobutyrate;
and the like. Particularly useful initiators are the water-soluble peroxygen compounds such as hydrogen peroxide and the sodium, potassium and ammonium persulfates used by themselves or in an activated redoY system. Typical redox systems include alkali metal persulfates in combination with a reducing substance such as polyhydroxyphenols and oxidizable sulfur compounds such as sodium sulfite or sodium bisulfide, a reducing sugar, dimethylamino propionitrile, a diazomercapto compound and a water-soluble ferricyanide compound, or the like.
Heavy metal ions may also be used to activate the persulfate catalyzed polymerization. Polymer latices having e~cellent stability are obtained with alkali metal and ammonium persul~ate polymerizations. The amount of initiator used will generally be in the range between about 0.1~ to 3% by weight based on the total monomers and preferably is between about 0.15%
and 1~ by weight. The initiator may be charged completely at the outset oE the polymerization, however, incremental addition or proportioning of the .
.. . .
t~95;
_9_ initiator throughout the polymerization may also be employed and is often advantageous.
Typical polymerizations for the preparation of the latexes herein are conducted by charging the reactor with the appropriate amount of water and electrolyte, if any is to be employed, a portion of the emulsifier, if any, and a portion of the initator sufficient to initiate the polymerization. The reactor is then evacuated, heated to the initiation temperature and charged with a portion of the monomer premix which is previously prepared by mixing water, emulsifier, the monomers and polymerization modifiers, if any are employed. After the initial monomer charye has been allowed to react for a period of time, the lS proportioning of the remaining monomer premix is begun, the rate of proportioning being varied depending on the polymerization temperature, the particular initiator employed and the amount of vinyl halide monomer being polymerized. After all the monomer premix has been charged, the final addition of initiator is made and the reaction continued with agitation for a length of time necessary to achieve the desired conversion.
In the latex, the particle size may be in the range of about 0.1 micrometer. A generally satisfactory particle size may be, however, from about 0.05 to about 5 micrometers. The total solids of the latexes may be varied widely and may relate to the fluidity wanted in the composition, with a 10% total solids latex providing more water than a 50 or 65 total solids latéx.
Latexes suitable for the use described herein must coalesce at process conditions. This is easily determined by placing a latex in an oven and drying it to see whether a continuous film or a discontinuous :
.
, r7 ~
powder resin is formed. Film forming latexes from a powder resin type latex by the above test can be made by uniformly blending with the latex about 10 to 100 parts by weight of one or more plasticizers per 100 S parts by weight of the resin. The useful plasticizers may be described as the alkyl and alkoxy alkyl esters of dicarboxylic acids or the esters of a polyhydric alcohol and a monobasic acid. As examples of such materials, there may be named dibutyl phthalate, dioctyl phthalate, dibutyl sebacate, dinonyl phthalate, di(2-ethyl hexyl)phthalate, di(2-ethyl hexyl)adipate, dilauryl phthalate, dimethyl tetrachlorophthalate, butyl phthalate, butyl glycollate, glyceryl stearate, and the like. The preferred plasticizers are the liquid diesters of aliphatic alcohols having from 4 to 20 carbon atoms and dibasic carboxylic acids having from 6 to 14 carbon atoms.
A suitable latex that can be prepared as described herein, has the following formulation, in parts by weight:
demineralized water 77 vinyl chloride 50 ethyl acrylate 48 acrylic acid 2 sodium persulfate 0.4 tetrasodi~m pyrophosphate 0.3 sodium alpha olefin sulfonate 1.7 (40~) caustic to alkaline pH
The above latex has Tg of 37C, total solids of 54~, and a pH of 7.5 which is adjusted with addition of a sufficient amount of caustic. The latexes containing polymerized vinyl halide and/or vinylidene halide may be compounded with, or have mixed herein, other known .
~,~t~ 9~
ingredients, such as fillers, plasticizers, antioxidants or stabilizers, antifoaming agents, pigments, or other compounding aids. Furthermore, thickeners or bodying agents may be added to the polymer latices so as to control the viscosity of the latexes and thereby achieve the proper flow properties for the particular application desired.
The polyester nonwovens, which can be used as a filter substrate, are generally sold in batt form which are made of fibers about 2.5 to 5 centimeters long and weigh about 6 to 600 grams per square meter.
Cellulosic substrates, such as filter paper, can also be used as a filter substrate. A specific type of paper that is eminently suitable for use as a filter substrate is 280 micrometers bleached kraft filter paper weighing 31 grams per square meter with a density of 3.6 kilograms per cubic meter.
A latex o~ a water-insoluble homopolymer or copolymer of the present invention may be applied to the web or mat of fibers in any suitable fashion such as by spraying, dipping, roll-transfer~ or the like.
Application of the latex to the fibers is preferably made at room temperature to facilitate cleaning of the associated apparatus. The solids concentration of the latex is in the range of S~ to 60% by weight, and preferably from 5% to 25% when applied by dipping.
When applied by roll-transfer, solids concentration of the latex is generaly about 50% whereas with the spraying technique, it can range widely.
An acid catalyst in an amount of about 0~1 to 5, preferably 0.5 to 3 weight parts per 100 weight parts of the latex solids, is preferably included in the latex at the time it is applied to the substrate.
Examples of acidic catalysts that may be employed include oxalic acid, dichloracetic acid, ammoniu~
r;;lg~~
--12 ~
chloride, p-toluenesulfonic acid, and ammonium sulfate and amine salts such as the hydrochloride of 2-methyl-2-aminopropanol-1.
The proportion of the latex polymer that is applied to the filter paper or a nonwoven substrate is such as to provide 15 to 100%, preferably about 20~, by weight of the polymer, based on the total weight of the substrate. After application of the latexes to the subskrate, the impregnated or saturated substrate can be dried either at room temperature or at elevated temperature. The substrate is subjected, either after completion of the drying or as the final portion of the drying stage itself, to a baking or curing operation which may be effected at a temperature of about 100 to about 400C for a period which may range from about one-half hour at the lower temperatures to as low as five seconds at the upper temperatures. The conditions of ~aking and curing are controlled so that no appreciable deterioration or degradation of the substrate or polymer occurs. Preferably, the curing is effected at a temperature of 120 to 165C for a period of 2 to 10 minutes.
Several different cross-linking resins have been found to provide the desired degree oE
cross-linking of the basic latex polymer and render it stiffer and resistant to hot oil. Amount of the cross-linking resins recommended for use herein is in the range of 1 to 30 weight parts, preferably 5 to 20 parts, per 100 weight parts oE latex solids. Examples of suitable cross-linking agents include water-dispersible or water-soluble resins, which, with the aid of a catalyst, promote the cross-linking of the principal polymer in the latex. Examples of suitable cross-linking resins include emulsified epoxy resins, melamine-formaldehyde resins, ' ' ' ~ ' .
': " - , , ' r~ 9 ~ 3 urea-formaldehyde resins, lower alkoxy lower alkyl melamine resins, phenol-formaldehyde resins, polyacrylate resins containing pendant unsaturatiOn, and other cross-linking resins. Certain of these resins are rendered water-dispersible, as by emulsification, so that they are compatible with the aqueous latex.
A specific example of a suitable epoxy resin that can be used to promote cross-linking of the late~, is the CMD 35201 epoxy resin dispersion available from Celanese Plastics and Specialties Company. This is an emulsified resin so that it can be compatible with the aqueous latex. Its epoxide equivalent is in the range of 550-650 and it has a Durran's melting point of 75-85C. The dispersion is mechanically stable and no organic solvents are present. This epoxy dispersion and other cross-linking resins can be cured through both epoxy functionality and hydroxyl functionality. Curing agents most conveniently employed are those which are water soluble or dispersible and are stable in an aqueous medium. Examples of such agents include dicyandiamide, various substituted imidazoles, alipnatic and aromatic amines, melamine resins, and urea-formaldehyde resins. Viscosity of this dispersion is about 12,000 cps measured at 25C and at 10 rpm, Brookfield RVT.
To promote the action of the cross-linkin~
resins, a suitable catalyst is used in amount oE 1 to 30% by weight of the cross-linkin~ resin, preferably 5 to 20~. S~itable catalysts include ammonium chloride, tridimethyl aminoethyl phenol, and the like. The ammonium chloride is a useful acid catalyst for the melamine and phenol-formaldehyde cross-linking resins whereas tridimethyl aminoethyl phenol is an especially ~ ~ ~9 7 9 .~
suitable catalyst in conjunction with the emulsified epoxy cross-linking resins.
The invention disclosed herein is illustrated with the following examples that demonstrate impregnation of conventional unbonded filter paper with various binders and subsequent evaluation for suitability in oil filters.
Samples of binder formulations were prepared using different binders to impregnate unbonded filter paper for use in oil filters. The binders were latexes and resins with and without cross-linking agents and catalysts for the cross-linking agents. In samples 1 to 7, water was added to the binder to adjust total solids to 15% whereas in samples 8 to 10, total solids was 20%. Ammonium hydroxide was used to adjust pH of the binders to 8.5, whenever needed. The formulations for samples 1 to 10, in weight parts, are set forth in Table I, below:
79.J
o o o .
o ~ I ~ I I I I I I
~r a~ o . CO
o 1` ~ .
oo o~
q~
o CO o 1--~ 1 ~1 0 ~ , I`O CO ~ O
~,o ~-- o ~1 ~1 1 1 1 1 1 ~1 0 ,1 DO 00 ~ ~ ~D
~01-- 0 ' ~, Lno a~
. ~or~ o ~ .~
: ~ ~ro 1- . ~ .
$~~_1 1 1 1 ~1~ 1 E~ ~
~
oc~ ~ o ~o l-- o ' .
::
o~
o CO ~ o o~ o , o o _Io ) ~~1 1` 1 1 1 1 1 1 ~1 1 _I _I In o o o o ~n~ o o E~~ co ~1 u~ ~n o o o o dP11'~ ~1'el' 00 ~D ~O _l ~1 ~t . ~ :a C) X aJ .IJ V
-1aJ 4 ~ 1 C
~15 v a~
.,, la 4' ~ ~ ra ~ ~ X X C ~ C~1 C ,~
vcJ ~ ~ ~ ~ ~
a~~ IN ~:U m ~ ~ c x x~ ~; x 2 .: ' ~ 9~
Table I, above, presents formulations for samples 1 to 10. The percent total solids (% TS) is given for each component of the formulation, and amounts of each component are given on dry and wet basis, i.e., 100/178.3 indicates 100 wei~ht parts on dry basis and 178.3 indicates 178.3 weight parts on wet basis. The PVC Latex A was prepared by emulsion pol~merization in an aqueous medium and the polymeric product consisted of 50 weight parts vinyl chloride, 48 parts ethyl acrylate, and 2 parts acrylic acid prepared in the presence of sodium persulfate, tetrasodium pyrophosphate, sodium alpha olefin sulfonate, and caustic. The pH of the PVC latex was 7.5 and its Tg was 37C. Latex B was also a water-based latex of 50 weight parts ethyl acrylate, 15 parts butyl acrylate, 30 parts acrylonitrile, 3 parts acrylamide, and 2 parts N-methylol acrylamide.
Latex C was also a water-based latex of 34 parts butadiene, 31 parts styrene, and 35 parts acrylonitrile. X-linker A was a modified melamine-formaldehyde resin, more specifically, hexamethoxy methyl melamine, i.e., Cymel 373, ~
available from American Cyanamid. X-linker B was a water-dispersible phenol-formaldehyde resin, l.e., Durez 14798, available from Occidental Petroleum Company. X-linker C was a non-ionic aqueous dispersion of a solid Bisphenol A epoxy resin, i.e., CMD 35201, available from Celanese Plastics and Specialties Company~ Ammonium chloride served as an acid catalyst for the modified melamine-formaldehyde resin or X-linker A, whereas the amine catalyqt, which was tridimethyl aminoethyl phenol, served as a catalyst for the emulsified epoxy resin or X-linker C. The aziridine resin served as a low temperature curing agent.
*trade marks ' , ' :
.
7 9 i ~
.~, ~.
In preparing the impregnated filter paper with the various binders, strips of unbonded filter paper were placed on a wire screen and immersed in a binder and then pulled across a vacuum slot to remove excess binder. The impregnated filter paper samples were then dried on a photoprint drier at 100C for 5 minutes and then cured at 177C for 5 minutes. Pickup of latex solids varied from about 17 to 23%.
Samples of filter paper impregnated with the various binders disclosed in Table I were then submitted t~ an outside party for e~aluatlon for oil filter use. The impregnated filter paper samples were evaluated for strength, resistance to hot oil, stiffness, and flexibility. On the basis o~ the evaluation, only the PVC latex A was selected as an acceptable water-based latex as a binder for filter paper for use in an oil filter, especially with the emulsified epoxy resin as the x-linking resin and the amine catalyst therefor.
Additional samples of binder formulations 11 to 18 were prepared, as in Example 1. Ammonium hydroxide was used to adjust pH of the binders to 8.5 and water was added to reach 15~ total solids. The binders were then used to impregnate 280 micrometer flat filter paper, in the manner described in Example 1, to obtain 20% pickup. The impregnated sheets were dried at 100C for 5 minutes, cured at 149C for 5 minutes, and evaluated ~or dry and wet tensile strength. Lastl~, the impregnated sheets were immersed in 10/40W oil at 177C for 96 hours and again tested Eor tensile strength. Formulations of binder samples 11 to 18, tensile strength data for impregnated shee-ts aEter single curing, and tensile strength data for the impregnated sheets after single 7~3~
curing and after hot oil immersion test, are given in Table II, below:
' ' , ~ 79:`~
'~) d' ~O
o I~ O I I I I I CC ~ r~
#~ t'`l O L~ ~ O O
_ O o ~o ~ o U7 C;~
#~ O
N
U~
~D O ~ ~ ~ O
~1 O d' o u~ ~1 ~J ) ~ I ~/O I ~
~ ~ ~ 0 ~1 O ~ ~ ~1 ~1 ~ 2~ ~3 .
Ilt o ~ro ~1 ~ Ei c:~
~/ I ~1 0~1 ~ I I ~1 I ~ ~ ~ d' C ~1 .,1 r~
_, O
el' -1 O N ,~ ~r # ~l~o I I I I I I ~ Ci~ ~ ~ ' H . CS .,.
~ r~ O o ~ ~ ~ o o~
~I co I I I ~1 1 'I ~ ~ ~ ~ 1-U~
. ~ 1 ~ o ~J
:~O N O Ln U~ Ll~ a~
1 1 I C co t~) a I_ ' O C) r--l ~ ~1 ~ V~ N N ~1 ~0 IO N O --1 ~ ~ N tl~ 1_ ~ 1 1 ~ I ~ a) ~
E-' u~ o~ a~o '- o o o E~ . . . . . o d~ ~t'co Ul ~ O O o m X X
,~ ~ a~ u ~ J~ ~ ~ a) a) o t~ O
.,, I ~ C C C
I ~ ~ I I I ~
~ ~ ~ x x x æ ~: a ~: ~
~1 .
:
BACKGROUND OF T~E INVENTIGN
_ The paper used as the filtration medium for automotive type filters has been traditionally treated with phenolic resole type resins. This has been done to improve the paper's strength properties and allow it to be pleated in an accordian-like shape and to hold this shape when the paper composite is cured.
The standard phenolic resin used to treat automotive filter paper had relatively low mol ratios, on the order of 1.0/1 to 1~3/1 formaldehyde to phenol. This has been necessary so that good final paper properties, especially flexibility, could be achieved. Higher mol ratio resins tend to result in brittle paper on curing.
The traditional method of making an automotive filter has been for a paper maker to treat a base filter sheet with an alcohol solution of these phenolic resole resins. The treated sheet was passed through an oven to drive off the solvent and make a so-called B-stage sheet. This sheet was then shipped to the filter maker where it was pleated and put through an oven to further cure the sheet and to hold the shape of the pleats.
With the onset of greater concern for environmental quality, the filter manufacturers have requested paper suppliers to supply a formaldehyde-free impregnated sheet that holds its pleat, and meets all of the requirements for oil filters.
This invention is directed to oil filters and oil filter media impregnated with a water-based latex containing polymerized vinyl chloride. Such oil filters are manufactured with only a single cure and ~;~
'' 1'`,' , ' , :
g~3~
do not impair the environment by emitting volatile solvents.
SUMMARY OF THE ~ VENTION
Impregnated oil filter media and oil filters incorporating same are made by impregnating an oil filter substra-te, for example paper or a suitable nonwoven, with an aqueous la-tex selected from homo-polymers of a vinyl halide or a vinylidene halide and copolymers wherein a vinyl halide and/or a vinylidene halide is polymerized with other co-monomers. Manufacture of such oil filters does not c~n-tr~bute to any air pollution through escape of a volatile solvent.
DETAILED DESCRIPTICN OF THE INVENTION
The use of a water-based binder in making impregnated paper or nonwoven for oil filters is desirable from at least one point of view: the elimination of the volatile solvent used in the past in connection with phenolic binders. The volatile solvent, such as an alcohol, was detrimental in that it contributed to air polution when the filter medium was dried thus releasing the alcohol into the atmosphere. The use of volatile solvents in such operations is bein~ curtailed in response to ever more stringent environmental controls.
In an attempt to produce oil filters with a water-based binder, several aqueous latexes were tried, all, however, unsuccessfully. Such binders included polyvinyl chloride, acrylonitrile/butadiene, butadiene/styrene/arylonitrile, acrylate/styrene, and other latexes. Composites based on these water-based binders lacked the necessary stability in the hot oil immersion test in that the resin binder was extracted into the hot oil.
Following the initial unsuccessful attempts with water-based binders, several additional composite ~>'~ 79 S
samples were prepared with various aqueous latexes cross-linked with a variety of cross-linking agents.
In carrying out these experiments, conventional unbonded filter paper was saturated with these crosslinkable binders, and the saturated filter paper was then evaluated by an outside party that commercially produces impregnated filter paper for the oil filter manufacturers. After a thorough evaluation, crosslinkable polyvinyl chloride latex was selected as a suitable binder in the production of impregnated oil filter medium whereas the other binders were not suitable.
Therefore, this invention is directed to oil filters and oil filter media selected from filter paper and nonwovens impregnated with a crosslinkable aqueous polyvinyl halide latex. The resulting impregnated oil filter media have the necessary resistance to hot oil and meet other physical properties. The latex described herein is admixed with a cross-linking resin and a catalyst for the cross-linking resin before it is used to impregnate filter paper or a nonwoven filter substrate which is then dried and cured at an elevated temperature. The latex solids, prior to impregnation, are adjusted with water to a solids content of about 5 to 70~, preferably 10 to 30~, and pH thereof is adjusted to about 4 to 12, preferably to the alkaline side oE 7 to 9. ..
Suitable polymeric aqueous latexes ~or saturating or impregnating filter paper or a nonwoven filter medium are selected from homopolymers of a vinyl halide or a vinylidene halide and copolymers of a vinyl halide and/or vinylidene halide with other copolymerizable monomers. In a preEerred embodiment, suitable latexes are selected from homopolymers of 3 7 g 3 vinyl chloride and copolymers of vinyl chloride with other copolymerizable monomers. Amount of polymerized vinyl chloride in such latexes can vary from a minimum oE about 5% by weight up to 100% for the homopolymers, -5 but preEerably the copolymers contain at least about 20% of polymerized vinyl chlori~e and most preferably contain in excess of about 40% polymerized vinyl chloride. Preerred polymers in the latexes have Tg in the range of 0C to 100C but more preferabïy 20C
to 50C.
There is a large variety of comonomers that can be polymerized with a vinyl halide in producing aqueous copolymer latexes. The term "copolymer", for purposes herein, defines a polymer of two or more 15 monomers. On the basis of this definition, vinyl halide and/or vinylidene halide, preferably vinyl chloride, can be copolymerized with one or more of comonomers such as ~ olefinically unsaturated carboxylic acids containing 3 to 5 carbon atoms, such as acrylic, methacrylic, ethacrylic and cyanoacrylic acids; monounsaturated dicarboxylic acids containing 4 to 8 carbon atoms, such as fumaric and maleic acids;
esters of ~ olefinically unsaturated carboxylic acids containing 3 to 5 carbon atoms and monounsaturated dicarboxylic acids containing 4 to 20 but preferably 4 to 12 carbon atoms, such as methyl acrylate, ethyl acrylate, butyl acrylate, 2-ethylhexyl acrylate, octyl acrylate, ethyleneglycol dimethacrylate, diethylene glycol diacrylate, cyanoethyl acrylate, methyl methacrylate, butyl methacrylate, hydroxypropyl methacrylate, ethyl maleate, butyl fumarate, maleic dimethyl ester, maleic acid mono-(2-ethylhexyl)ester, fumaric acid diethyl ester, and fumaric acid dilauryl ester;
~,~-olefinically unsaturated nitriles containing 3 to .
: ' :, ' ' ,;' ' ' ' ~
~ 79 5 carbon atoms, such as acrylonitrile and methacrylonitrile; acrylamides derived from acrylic and methacrylic acids and their N-alkylol and ~-alkoxyalkyl derivatives containing l to 20 but preferably l to 12 carbon atoms, such as acrylamide itself, ~-methylol acrylamide, N-butoxy methacrylamide, methylenebisacrylamide, methacrylamide, ~l-octyl acrylamide, diacetone acrylamide, and hydroxymethyl diacetone acrylamide;
vinyl ethers containing 4 to 22 caron atoms, such as ethyl vinyl ether, chloroethyl vinyl ether, isobutyl vinyl ether, cetyl vinyl ether, and lauryl vinyl ether; vinyl ketones containing 3 to 12 carbon atoms, such as methyl vinyl ketone; vinyl esters of carboxylic acids containing 4 to 22 carbon atoms, such as vinyl acetate, vinyl propionate, vinyl formate, vinyl stearate, vinyl benzoate, and vinyl and allyl chloroacetate; ~-ole~ins containing 2 to 12 carbon atoms, such as ethylene, propylene, isobutylene, and butene-l; styrene and styrene derivatives such as ~-methyl styrene, vinyl toluene, and chlorostyrene;
and othér polyfunctional monomers such as vinyl naphthalene, vinyl pyridine, divinyl benzene, and allyl pentaerythritol.
Preferred latexes are copolymers of vinyl chloride, a lower alkyl acryate, and an acrylic acid.
Amount of vinyl chloride in such latexes generally exceeds 40% by weight of the monomer weight, preEerably being in the range of about 40 to 70 dry weight parts, whereas the lower alkyl acrylate is used in an amount exceeding 20~ of the total monomer weight, preferably being in the range of about 30 to 60 dry weight parts. Amount of an acrylic acid, preferably acrylic acid itself, is use in an amount of up to about 5~ of total monomer weight, preferably 3 7~`~
about 0.5 to 3 weight parts. The amounts given herein in weight parts are based on a total of 100 weight parts of all monomers in the latex. As used herein, the "lower" alkyl acrylate monomer is defined as containing about 1 to 8 carbon atoms in the alkyl moiety. The preferred latexes can also contain about 0.5 to 2 weight parts of an alkylol acrylamidé
containing 1 to 4 carbon atoms in the alkylol group.
Amount of the alkylol acrylamide is based on 100 weight part of all the monomers in the latex.
Preferred latexes are prepared by emulsion polymeriæation of vinyl chloride and one or more comonomers. Comonomers for the preferred latexes include acrylic and methacrylic acids and alkyl esters derived therefrom which contain 1 to 20 carbon atoms, preferably 2 to 12, in the alkyl group; amides derived from ,~-olefinically unsaturated carboxylic acids and their N-alkylol and N-alkoxyalkyl derivatives such as acrylamide, N-octyl acrylamide, and hydroxymethyl diacetone acrylamide; and vinylidene halides, such as vinylidene chloride. Specific examples of preferred latexes containing polyvinyl chloride are copolymers of the following monomers: vinyl chloride, 2-ethylhexyl acrylate, vinylidene chloride, and acrylic acid; vinyl chloride, 2-ethylhexyl acrylate, vinylidene chloride, and hydroxymethyl diacetone acrylamide; vinyl chloride and methyl acrylate; vinyl chloride, butyl acrylate, acrylic acid, and N-methylol acrylamide; and vinyl chloride, 2-ethylhexyl acrylate, vinylidene chloride, and hydroxypropyl methacrylate.
The latexes can be plasticized or unplasticized.
The polymer latexes embodied herein are prepared employing conventional polymerization techniques in an aqueous medium with a suitable polymerization catalyst. Overpolymerization of the , '' .
monomers may also be employed. A~ueous dispersions of solution polymers may be used.
The a~ueous medium may be emulsifier-Eree or it may contain an emulsifier. When emulsifiers are used to prepare the latexes of this invention, the usual types of anionic and non-ionic emulsifiers may be employed. Useful anionic emulsifiers include alkali metal or ammonium salts of the sulfates of alcohols having from 8 to 18 carbon atoms such as sodium lauryl sulfate; ethanolamine lauryl sulEate, ethylamine lauryl sulfate; alkali metal and ammonium salts of sulfonated petroleum and paraffin oils;
sodium salts of sulfonic acids such as dodecane-l-sulfonic acid and octadiene-l-sulfonic acid; aralkyl sulfonates such as sodium isopropyl benzene sulfonate, sodium dodecyl benzene sulfonate and sodium isobutyl naphthalene sulfonate; alkali metal and ammonium salts of sulfonated dicarboxylic acid esters such as sodium dioctyl sulfosuccinate, disodium-n-octadecyl sulfosuccinamate; alkali metal or ammonium salts of the free acid of complex organic mono- and diphosphate esters; and the like. Non-ionic emulsifiers such as octyl- or nonylphenyl polyethoxyethanol may also be used. Latexes having excellent stability are obtained with the alkali metal and ammonium salts of aromatic sulfonic acids, aralkyl sulfonates, long chain alkyl sulfonates and poly(oxyalkylene~sulfcnates.
If an emulsifier is used, this may range up to about 6~ or more by weight based on the rnonomers, but it preferably is less than 6~, and excellent results have been obtained with less than 1%. The emulsifier may be entirely added at the outset of the polymerization or it may be added incrementally or by proportioning throughout the run. Typically, a ~nall ' , .
. .
9-~
amount of the emulsifier is added at the outset of the polymerization and the remainder charged incrementally or proportionately to the reactor as the monomers are proportioned.
S The polymerization may be conducted at temperatures from about 0C or less to about 100C in the presence of a compound capable of initiating the polymerizations. Commonly used free radical initiators include the various peroxygen compounds such as persulfate, benzoyl peroxide, t-butyl hydroperoxide, cumene hydroperoxide, t-butyl diperphthalate, pelargonyl peroxide and l-hydroxycyclohexyl hydroperoxide; azo compounds such as azodiisobutyronitrile and dimethylazodiisobutyrate;
and the like. Particularly useful initiators are the water-soluble peroxygen compounds such as hydrogen peroxide and the sodium, potassium and ammonium persulfates used by themselves or in an activated redoY system. Typical redox systems include alkali metal persulfates in combination with a reducing substance such as polyhydroxyphenols and oxidizable sulfur compounds such as sodium sulfite or sodium bisulfide, a reducing sugar, dimethylamino propionitrile, a diazomercapto compound and a water-soluble ferricyanide compound, or the like.
Heavy metal ions may also be used to activate the persulfate catalyzed polymerization. Polymer latices having e~cellent stability are obtained with alkali metal and ammonium persul~ate polymerizations. The amount of initiator used will generally be in the range between about 0.1~ to 3% by weight based on the total monomers and preferably is between about 0.15%
and 1~ by weight. The initiator may be charged completely at the outset oE the polymerization, however, incremental addition or proportioning of the .
.. . .
t~95;
_9_ initiator throughout the polymerization may also be employed and is often advantageous.
Typical polymerizations for the preparation of the latexes herein are conducted by charging the reactor with the appropriate amount of water and electrolyte, if any is to be employed, a portion of the emulsifier, if any, and a portion of the initator sufficient to initiate the polymerization. The reactor is then evacuated, heated to the initiation temperature and charged with a portion of the monomer premix which is previously prepared by mixing water, emulsifier, the monomers and polymerization modifiers, if any are employed. After the initial monomer charye has been allowed to react for a period of time, the lS proportioning of the remaining monomer premix is begun, the rate of proportioning being varied depending on the polymerization temperature, the particular initiator employed and the amount of vinyl halide monomer being polymerized. After all the monomer premix has been charged, the final addition of initiator is made and the reaction continued with agitation for a length of time necessary to achieve the desired conversion.
In the latex, the particle size may be in the range of about 0.1 micrometer. A generally satisfactory particle size may be, however, from about 0.05 to about 5 micrometers. The total solids of the latexes may be varied widely and may relate to the fluidity wanted in the composition, with a 10% total solids latex providing more water than a 50 or 65 total solids latéx.
Latexes suitable for the use described herein must coalesce at process conditions. This is easily determined by placing a latex in an oven and drying it to see whether a continuous film or a discontinuous :
.
, r7 ~
powder resin is formed. Film forming latexes from a powder resin type latex by the above test can be made by uniformly blending with the latex about 10 to 100 parts by weight of one or more plasticizers per 100 S parts by weight of the resin. The useful plasticizers may be described as the alkyl and alkoxy alkyl esters of dicarboxylic acids or the esters of a polyhydric alcohol and a monobasic acid. As examples of such materials, there may be named dibutyl phthalate, dioctyl phthalate, dibutyl sebacate, dinonyl phthalate, di(2-ethyl hexyl)phthalate, di(2-ethyl hexyl)adipate, dilauryl phthalate, dimethyl tetrachlorophthalate, butyl phthalate, butyl glycollate, glyceryl stearate, and the like. The preferred plasticizers are the liquid diesters of aliphatic alcohols having from 4 to 20 carbon atoms and dibasic carboxylic acids having from 6 to 14 carbon atoms.
A suitable latex that can be prepared as described herein, has the following formulation, in parts by weight:
demineralized water 77 vinyl chloride 50 ethyl acrylate 48 acrylic acid 2 sodium persulfate 0.4 tetrasodi~m pyrophosphate 0.3 sodium alpha olefin sulfonate 1.7 (40~) caustic to alkaline pH
The above latex has Tg of 37C, total solids of 54~, and a pH of 7.5 which is adjusted with addition of a sufficient amount of caustic. The latexes containing polymerized vinyl halide and/or vinylidene halide may be compounded with, or have mixed herein, other known .
~,~t~ 9~
ingredients, such as fillers, plasticizers, antioxidants or stabilizers, antifoaming agents, pigments, or other compounding aids. Furthermore, thickeners or bodying agents may be added to the polymer latices so as to control the viscosity of the latexes and thereby achieve the proper flow properties for the particular application desired.
The polyester nonwovens, which can be used as a filter substrate, are generally sold in batt form which are made of fibers about 2.5 to 5 centimeters long and weigh about 6 to 600 grams per square meter.
Cellulosic substrates, such as filter paper, can also be used as a filter substrate. A specific type of paper that is eminently suitable for use as a filter substrate is 280 micrometers bleached kraft filter paper weighing 31 grams per square meter with a density of 3.6 kilograms per cubic meter.
A latex o~ a water-insoluble homopolymer or copolymer of the present invention may be applied to the web or mat of fibers in any suitable fashion such as by spraying, dipping, roll-transfer~ or the like.
Application of the latex to the fibers is preferably made at room temperature to facilitate cleaning of the associated apparatus. The solids concentration of the latex is in the range of S~ to 60% by weight, and preferably from 5% to 25% when applied by dipping.
When applied by roll-transfer, solids concentration of the latex is generaly about 50% whereas with the spraying technique, it can range widely.
An acid catalyst in an amount of about 0~1 to 5, preferably 0.5 to 3 weight parts per 100 weight parts of the latex solids, is preferably included in the latex at the time it is applied to the substrate.
Examples of acidic catalysts that may be employed include oxalic acid, dichloracetic acid, ammoniu~
r;;lg~~
--12 ~
chloride, p-toluenesulfonic acid, and ammonium sulfate and amine salts such as the hydrochloride of 2-methyl-2-aminopropanol-1.
The proportion of the latex polymer that is applied to the filter paper or a nonwoven substrate is such as to provide 15 to 100%, preferably about 20~, by weight of the polymer, based on the total weight of the substrate. After application of the latexes to the subskrate, the impregnated or saturated substrate can be dried either at room temperature or at elevated temperature. The substrate is subjected, either after completion of the drying or as the final portion of the drying stage itself, to a baking or curing operation which may be effected at a temperature of about 100 to about 400C for a period which may range from about one-half hour at the lower temperatures to as low as five seconds at the upper temperatures. The conditions of ~aking and curing are controlled so that no appreciable deterioration or degradation of the substrate or polymer occurs. Preferably, the curing is effected at a temperature of 120 to 165C for a period of 2 to 10 minutes.
Several different cross-linking resins have been found to provide the desired degree oE
cross-linking of the basic latex polymer and render it stiffer and resistant to hot oil. Amount of the cross-linking resins recommended for use herein is in the range of 1 to 30 weight parts, preferably 5 to 20 parts, per 100 weight parts oE latex solids. Examples of suitable cross-linking agents include water-dispersible or water-soluble resins, which, with the aid of a catalyst, promote the cross-linking of the principal polymer in the latex. Examples of suitable cross-linking resins include emulsified epoxy resins, melamine-formaldehyde resins, ' ' ' ~ ' .
': " - , , ' r~ 9 ~ 3 urea-formaldehyde resins, lower alkoxy lower alkyl melamine resins, phenol-formaldehyde resins, polyacrylate resins containing pendant unsaturatiOn, and other cross-linking resins. Certain of these resins are rendered water-dispersible, as by emulsification, so that they are compatible with the aqueous latex.
A specific example of a suitable epoxy resin that can be used to promote cross-linking of the late~, is the CMD 35201 epoxy resin dispersion available from Celanese Plastics and Specialties Company. This is an emulsified resin so that it can be compatible with the aqueous latex. Its epoxide equivalent is in the range of 550-650 and it has a Durran's melting point of 75-85C. The dispersion is mechanically stable and no organic solvents are present. This epoxy dispersion and other cross-linking resins can be cured through both epoxy functionality and hydroxyl functionality. Curing agents most conveniently employed are those which are water soluble or dispersible and are stable in an aqueous medium. Examples of such agents include dicyandiamide, various substituted imidazoles, alipnatic and aromatic amines, melamine resins, and urea-formaldehyde resins. Viscosity of this dispersion is about 12,000 cps measured at 25C and at 10 rpm, Brookfield RVT.
To promote the action of the cross-linkin~
resins, a suitable catalyst is used in amount oE 1 to 30% by weight of the cross-linkin~ resin, preferably 5 to 20~. S~itable catalysts include ammonium chloride, tridimethyl aminoethyl phenol, and the like. The ammonium chloride is a useful acid catalyst for the melamine and phenol-formaldehyde cross-linking resins whereas tridimethyl aminoethyl phenol is an especially ~ ~ ~9 7 9 .~
suitable catalyst in conjunction with the emulsified epoxy cross-linking resins.
The invention disclosed herein is illustrated with the following examples that demonstrate impregnation of conventional unbonded filter paper with various binders and subsequent evaluation for suitability in oil filters.
Samples of binder formulations were prepared using different binders to impregnate unbonded filter paper for use in oil filters. The binders were latexes and resins with and without cross-linking agents and catalysts for the cross-linking agents. In samples 1 to 7, water was added to the binder to adjust total solids to 15% whereas in samples 8 to 10, total solids was 20%. Ammonium hydroxide was used to adjust pH of the binders to 8.5, whenever needed. The formulations for samples 1 to 10, in weight parts, are set forth in Table I, below:
79.J
o o o .
o ~ I ~ I I I I I I
~r a~ o . CO
o 1` ~ .
oo o~
q~
o CO o 1--~ 1 ~1 0 ~ , I`O CO ~ O
~,o ~-- o ~1 ~1 1 1 1 1 1 ~1 0 ,1 DO 00 ~ ~ ~D
~01-- 0 ' ~, Lno a~
. ~or~ o ~ .~
: ~ ~ro 1- . ~ .
$~~_1 1 1 1 ~1~ 1 E~ ~
~
oc~ ~ o ~o l-- o ' .
::
o~
o CO ~ o o~ o , o o _Io ) ~~1 1` 1 1 1 1 1 1 ~1 1 _I _I In o o o o ~n~ o o E~~ co ~1 u~ ~n o o o o dP11'~ ~1'el' 00 ~D ~O _l ~1 ~t . ~ :a C) X aJ .IJ V
-1aJ 4 ~ 1 C
~15 v a~
.,, la 4' ~ ~ ra ~ ~ X X C ~ C~1 C ,~
vcJ ~ ~ ~ ~ ~
a~~ IN ~:U m ~ ~ c x x~ ~; x 2 .: ' ~ 9~
Table I, above, presents formulations for samples 1 to 10. The percent total solids (% TS) is given for each component of the formulation, and amounts of each component are given on dry and wet basis, i.e., 100/178.3 indicates 100 wei~ht parts on dry basis and 178.3 indicates 178.3 weight parts on wet basis. The PVC Latex A was prepared by emulsion pol~merization in an aqueous medium and the polymeric product consisted of 50 weight parts vinyl chloride, 48 parts ethyl acrylate, and 2 parts acrylic acid prepared in the presence of sodium persulfate, tetrasodium pyrophosphate, sodium alpha olefin sulfonate, and caustic. The pH of the PVC latex was 7.5 and its Tg was 37C. Latex B was also a water-based latex of 50 weight parts ethyl acrylate, 15 parts butyl acrylate, 30 parts acrylonitrile, 3 parts acrylamide, and 2 parts N-methylol acrylamide.
Latex C was also a water-based latex of 34 parts butadiene, 31 parts styrene, and 35 parts acrylonitrile. X-linker A was a modified melamine-formaldehyde resin, more specifically, hexamethoxy methyl melamine, i.e., Cymel 373, ~
available from American Cyanamid. X-linker B was a water-dispersible phenol-formaldehyde resin, l.e., Durez 14798, available from Occidental Petroleum Company. X-linker C was a non-ionic aqueous dispersion of a solid Bisphenol A epoxy resin, i.e., CMD 35201, available from Celanese Plastics and Specialties Company~ Ammonium chloride served as an acid catalyst for the modified melamine-formaldehyde resin or X-linker A, whereas the amine catalyqt, which was tridimethyl aminoethyl phenol, served as a catalyst for the emulsified epoxy resin or X-linker C. The aziridine resin served as a low temperature curing agent.
*trade marks ' , ' :
.
7 9 i ~
.~, ~.
In preparing the impregnated filter paper with the various binders, strips of unbonded filter paper were placed on a wire screen and immersed in a binder and then pulled across a vacuum slot to remove excess binder. The impregnated filter paper samples were then dried on a photoprint drier at 100C for 5 minutes and then cured at 177C for 5 minutes. Pickup of latex solids varied from about 17 to 23%.
Samples of filter paper impregnated with the various binders disclosed in Table I were then submitted t~ an outside party for e~aluatlon for oil filter use. The impregnated filter paper samples were evaluated for strength, resistance to hot oil, stiffness, and flexibility. On the basis o~ the evaluation, only the PVC latex A was selected as an acceptable water-based latex as a binder for filter paper for use in an oil filter, especially with the emulsified epoxy resin as the x-linking resin and the amine catalyst therefor.
Additional samples of binder formulations 11 to 18 were prepared, as in Example 1. Ammonium hydroxide was used to adjust pH of the binders to 8.5 and water was added to reach 15~ total solids. The binders were then used to impregnate 280 micrometer flat filter paper, in the manner described in Example 1, to obtain 20% pickup. The impregnated sheets were dried at 100C for 5 minutes, cured at 149C for 5 minutes, and evaluated ~or dry and wet tensile strength. Lastl~, the impregnated sheets were immersed in 10/40W oil at 177C for 96 hours and again tested Eor tensile strength. Formulations of binder samples 11 to 18, tensile strength data for impregnated shee-ts aEter single curing, and tensile strength data for the impregnated sheets after single 7~3~
curing and after hot oil immersion test, are given in Table II, below:
' ' , ~ 79:`~
'~) d' ~O
o I~ O I I I I I CC ~ r~
#~ t'`l O L~ ~ O O
_ O o ~o ~ o U7 C;~
#~ O
N
U~
~D O ~ ~ ~ O
~1 O d' o u~ ~1 ~J ) ~ I ~/O I ~
~ ~ ~ 0 ~1 O ~ ~ ~1 ~1 ~ 2~ ~3 .
Ilt o ~ro ~1 ~ Ei c:~
~/ I ~1 0~1 ~ I I ~1 I ~ ~ ~ d' C ~1 .,1 r~
_, O
el' -1 O N ,~ ~r # ~l~o I I I I I I ~ Ci~ ~ ~ ' H . CS .,.
~ r~ O o ~ ~ ~ o o~
~I co I I I ~1 1 'I ~ ~ ~ ~ 1-U~
. ~ 1 ~ o ~J
:~O N O Ln U~ Ll~ a~
1 1 I C co t~) a I_ ' O C) r--l ~ ~1 ~ V~ N N ~1 ~0 IO N O --1 ~ ~ N tl~ 1_ ~ 1 1 ~ I ~ a) ~
E-' u~ o~ a~o '- o o o E~ . . . . . o d~ ~t'co Ul ~ O O o m X X
,~ ~ a~ u ~ J~ ~ ~ a) a) o t~ O
.,, I ~ C C C
I ~ ~ I I I ~
~ ~ ~ x x x æ ~: a ~: ~
~1 .
:
3 7 9 ;~
In the above table, PVC latex A was an aqueous latex of 50 weight parts vinyl chloride, 48 parts ethyl acrylate, and 2 parts acrylic acid prepared in an aqueous medium in the presence of sodium persulfate, tetrasodium pyrophosphate, sodlum alpha olefin sulfonate, and caustic. Its pH was 7.5 and Tg 37C. PVC latex B was also an aqueous latex of 63 weight parts vinyl chloride, 35 parts n-butyl acrylate, 1 part acrylic acid, and 1 part N-methylol acrylamide (48%), prepared in an aqueous medium in the presence of sodium persulfate, tetrasodium pyrophosphate, sodium alpha olefin sulfonate, and hydroxyl amine sulfate. Its pH was 5.0 and its Tg was 37C. X-linker A was a modified melamine-formaldehyde resin, more specifically, hexametho~ymethyl melamine, i.e., Cymel 373, available from American Cyanamid.
X-linker B was a water-dispersible phenol-formaldeh~de resin, i~e., Durez 14798, available from Occidental Petroleum Company. X-linker C was a non-ionic aqueous dispersion of a solid Bisphenol A epoxy resinr i.e., CMD 35201, available from Celanese Plastics and Specialties Company. Ammonium chloride served as an acid catalyst for the modified melamine-formaldehyde resin or the x-linker A, whereas the amine catalyst, tridimethyl arninoethyl phenol, served as a catalyst for the emulsified epoxy resin or x-linker C.
l~ore samples of binder formulations 19 to 29 were prepared, as in Example 1. Ammonium hydroxide was used to adjust pH of the binders to 8.5 and watèr was added to reach 15% total solids. The binders were then used to impregnate the same weight filter paper to obtain 20% pickup of latex solids. The impregnated sheets were dried at 100~C for 5 minutes, cured at 1~9C for 5 minutes, and evaluated for dry and wet ' . ' ~ - ': .
',' '' ~ ', ' tensile strength. Lastly, the impregnated sheets were immersed in 10/40W oil at 177C for 96 hours and again tested for tensile strength. Formulations of binder samples 19 to 29, tensile strength data for impregnated sheets after a single curing, and tensile strength data after single curing and after the hot oil immersion test, are given in Tahle III, below.
~' gt795 22 ,, cn o ~ co ~ ~
~ I O O I I I I I I a~ ~ ~r CO ~ ~
o ~ ~ ~ ,_ o oo Ct~
CO
~ ~ . ~ a~
r~ o ~ u~
o ~ ~ ~ ~ o t~ ~ oo ~r ~, ~ ~ ~ ~ .,.
~o o ~ ~ . ~ t` o ~
IO O O 1~ O ~ ~1 i , , ~ ~ , oo ~ U~ ~
~ ~ c~
u~ o ~ ~ . ~ co ~r ~1 ,' ~ Io o o ~ S N ~ ~r I I ~ ~ r~ _1 . ._, d' ~ O
. er o ~ ~ ~ ~r ~r o ~ ~ . o I O O o u~ ~ ~D ~ ' I _~ ~ I I II a) cO ~r H er O
1_1 ~ ' ~ . ~ ~O Ll H r~ O t~ ~) ~ --IO O O _I ~ ~ c~ ) f~
~: ~ ~ ,~ 1 5 CO
:: m _l au ~ ~ ~ c~ ~r : ~ ~ o~ ~ . ~ ~ o ~ ~
~ o coI o r~ cn ~ ~ ~: r--:~ ~ ,~ ,~ I I I ~ ~ .1 1 a~ ~ ~ ~
~1 ~1 J-~ ~ i O O ~ In _I o ~ ~ . ~ ~n ~ d~
D C ~ ~ a~
I I~ ~ I I ~ a) ~ ~ ~J
~ ~ ~ r~
o o~ ~ . o ~ ~ o O ~ I O u~ O ~r ~ ~D
,~ n o ~, Co . U~ o aJ ~
O ~ ~ ~ ~1 ~I Ln ~ r7 o CO I o ~
a~~r o o o o o o U~
E~ er a In U O ~O O O
d~ ~ D ~ O
~ ~ .
m o a U(~ E~ E
~ ~ ~ QJ a) al ~ o v C) ,1 ~ Y
~1) ~ V E~
~, ~ x x x x z ~ a ~ o U~ o .
..
In the above table, PVC latex A was an aqueous latex of 50 weight parts vinyl chloride, 48 parts ethyl acrylate, and 2 parts acrylic acid prepared in an aqueous medium in the presence of -5 sodium persulfate, tetrasodium pyrophosphate, sodium alpha olefin sulfonate, and caustic. Its pH was 7.5 and Tg 37C. PVC latex B was also an aqueous latex of 63 weight parts vinyl chloride, 35 parts n-butyl acrylate, 1 part acrylic acid, and 1 part N-methylol acrylamide ~48%), prepared in an aqueous medium in the presence of sodium persulfate, tetrasodium pyrophosphate, sodium alpha olefin sulfonate, and hydroxyl amine sulfate. Its pH was 5.0 and its Tg was 37C. X-linker A was a modified melamine-formaldehyde resin, more specifically, hexamethoxymethyl melamine, i.e., Cymel 373, available from American Cyanamid.
X-linker B was a water-dispersible phenol-formaldehyde resin, i.e., Durez 14798, available from Occidental Petroleum Company. X-linker C was a non-ionic aqueous dispersion of a solid Bisphenol A epoxy resin, i.e., CMD 35201, available from Celanese Plastics and Specialties Company. X-linker D was an aqueous acrylate resin of 55 weight parts ethyl acrylate, 30 parts methyl methacrylate, and 15 parts N-methylol acrylamide, available from The BFGoodrich Cornpany as Carboset 533H resin. Ammonium chloride served as an acid catalyst for the modiEied melamine-Eormaldehyde resin or the x-linker A, whereas the amine catalyst, tridimethyl aminoethyl phenol, served as a catalyst for the emulsified epoxy resin or x-linker C.
, , ' . ' ....... . . .
~ 3 The data in Table III shows that the latexes by themselves without crosslinkers, as in samples #28 and #29, have very poor tensile strength after oil immersion for 96 hours in lOW-40 oil at 177C of filter paper samples impregnated therewith.
. .
In the above table, PVC latex A was an aqueous latex of 50 weight parts vinyl chloride, 48 parts ethyl acrylate, and 2 parts acrylic acid prepared in an aqueous medium in the presence of sodium persulfate, tetrasodium pyrophosphate, sodlum alpha olefin sulfonate, and caustic. Its pH was 7.5 and Tg 37C. PVC latex B was also an aqueous latex of 63 weight parts vinyl chloride, 35 parts n-butyl acrylate, 1 part acrylic acid, and 1 part N-methylol acrylamide (48%), prepared in an aqueous medium in the presence of sodium persulfate, tetrasodium pyrophosphate, sodium alpha olefin sulfonate, and hydroxyl amine sulfate. Its pH was 5.0 and its Tg was 37C. X-linker A was a modified melamine-formaldehyde resin, more specifically, hexametho~ymethyl melamine, i.e., Cymel 373, available from American Cyanamid.
X-linker B was a water-dispersible phenol-formaldeh~de resin, i~e., Durez 14798, available from Occidental Petroleum Company. X-linker C was a non-ionic aqueous dispersion of a solid Bisphenol A epoxy resinr i.e., CMD 35201, available from Celanese Plastics and Specialties Company. Ammonium chloride served as an acid catalyst for the modified melamine-formaldehyde resin or the x-linker A, whereas the amine catalyst, tridimethyl arninoethyl phenol, served as a catalyst for the emulsified epoxy resin or x-linker C.
l~ore samples of binder formulations 19 to 29 were prepared, as in Example 1. Ammonium hydroxide was used to adjust pH of the binders to 8.5 and watèr was added to reach 15% total solids. The binders were then used to impregnate the same weight filter paper to obtain 20% pickup of latex solids. The impregnated sheets were dried at 100~C for 5 minutes, cured at 1~9C for 5 minutes, and evaluated for dry and wet ' . ' ~ - ': .
',' '' ~ ', ' tensile strength. Lastly, the impregnated sheets were immersed in 10/40W oil at 177C for 96 hours and again tested for tensile strength. Formulations of binder samples 19 to 29, tensile strength data for impregnated sheets after a single curing, and tensile strength data after single curing and after the hot oil immersion test, are given in Tahle III, below.
~' gt795 22 ,, cn o ~ co ~ ~
~ I O O I I I I I I a~ ~ ~r CO ~ ~
o ~ ~ ~ ,_ o oo Ct~
CO
~ ~ . ~ a~
r~ o ~ u~
o ~ ~ ~ ~ o t~ ~ oo ~r ~, ~ ~ ~ ~ .,.
~o o ~ ~ . ~ t` o ~
IO O O 1~ O ~ ~1 i , , ~ ~ , oo ~ U~ ~
~ ~ c~
u~ o ~ ~ . ~ co ~r ~1 ,' ~ Io o o ~ S N ~ ~r I I ~ ~ r~ _1 . ._, d' ~ O
. er o ~ ~ ~ ~r ~r o ~ ~ . o I O O o u~ ~ ~D ~ ' I _~ ~ I I II a) cO ~r H er O
1_1 ~ ' ~ . ~ ~O Ll H r~ O t~ ~) ~ --IO O O _I ~ ~ c~ ) f~
~: ~ ~ ,~ 1 5 CO
:: m _l au ~ ~ ~ c~ ~r : ~ ~ o~ ~ . ~ ~ o ~ ~
~ o coI o r~ cn ~ ~ ~: r--:~ ~ ,~ ,~ I I I ~ ~ .1 1 a~ ~ ~ ~
~1 ~1 J-~ ~ i O O ~ In _I o ~ ~ . ~ ~n ~ d~
D C ~ ~ a~
I I~ ~ I I ~ a) ~ ~ ~J
~ ~ ~ r~
o o~ ~ . o ~ ~ o O ~ I O u~ O ~r ~ ~D
,~ n o ~, Co . U~ o aJ ~
O ~ ~ ~ ~1 ~I Ln ~ r7 o CO I o ~
a~~r o o o o o o U~
E~ er a In U O ~O O O
d~ ~ D ~ O
~ ~ .
m o a U(~ E~ E
~ ~ ~ QJ a) al ~ o v C) ,1 ~ Y
~1) ~ V E~
~, ~ x x x x z ~ a ~ o U~ o .
..
In the above table, PVC latex A was an aqueous latex of 50 weight parts vinyl chloride, 48 parts ethyl acrylate, and 2 parts acrylic acid prepared in an aqueous medium in the presence of -5 sodium persulfate, tetrasodium pyrophosphate, sodium alpha olefin sulfonate, and caustic. Its pH was 7.5 and Tg 37C. PVC latex B was also an aqueous latex of 63 weight parts vinyl chloride, 35 parts n-butyl acrylate, 1 part acrylic acid, and 1 part N-methylol acrylamide ~48%), prepared in an aqueous medium in the presence of sodium persulfate, tetrasodium pyrophosphate, sodium alpha olefin sulfonate, and hydroxyl amine sulfate. Its pH was 5.0 and its Tg was 37C. X-linker A was a modified melamine-formaldehyde resin, more specifically, hexamethoxymethyl melamine, i.e., Cymel 373, available from American Cyanamid.
X-linker B was a water-dispersible phenol-formaldehyde resin, i.e., Durez 14798, available from Occidental Petroleum Company. X-linker C was a non-ionic aqueous dispersion of a solid Bisphenol A epoxy resin, i.e., CMD 35201, available from Celanese Plastics and Specialties Company. X-linker D was an aqueous acrylate resin of 55 weight parts ethyl acrylate, 30 parts methyl methacrylate, and 15 parts N-methylol acrylamide, available from The BFGoodrich Cornpany as Carboset 533H resin. Ammonium chloride served as an acid catalyst for the modiEied melamine-Eormaldehyde resin or the x-linker A, whereas the amine catalyst, tridimethyl aminoethyl phenol, served as a catalyst for the emulsified epoxy resin or x-linker C.
, , ' . ' ....... . . .
~ 3 The data in Table III shows that the latexes by themselves without crosslinkers, as in samples #28 and #29, have very poor tensile strength after oil immersion for 96 hours in lOW-40 oil at 177C of filter paper samples impregnated therewith.
. .
Claims (17)
1. An oil filter comprising a filter substrate impregnated with a cured binder, said substrate being resistant to hot oil at 177°C. when immersed therein for 96 hours, said binder comprising a water-based latex selected from the group consisting of insoluble homopolymers of vinyl halide or vinylidene halide and insoluble copolymers of vinyl halide and/or vinyl-idene halide with one or more of copolymerizable mono-mers having a latex solids concentration of about 5 to 70% by weight, 1 to 30 weight parts per 100 weight parts of latex solids of cross-linking resin, and 1 to 30% by weight of said cross-linking resin of a catalyst for promoting the cross-linking of said latex; said copolymers contain at least 20% by weight of latex solids of a polymerized vinyl halide; said substrate is selected from filter paper and nonwoven fibers; and said cross-linking resin is selected from epoxy resins, melamine-formaldehyde resins, melamine resins, phenol-formaldehyde resins, polyacrylate resins, and mixtures thereof.
2. Oil filter of claim 1 wherein vinyl halide is vinyl chloride and said copolymers are polymers of vinyl chloride copolymerized with one or more of copolymerizable monomers selected from the group con-sisting of vinylidene chloride; alpha,beta-olefinically unsaturated carboxylic acids containing 3 to 5 carbon atoms; monounsaturated dicarboxylic acids containing 4 to 8 carbon atoms; esters of .alpha.,.beta.-olefinically unsaturated monocarboxylic and dicarboxylic acids containing 4 to 20 carbon atoms; acrylamides and meth-acrylamides and their N-alkylol derivatives containing 1 to 20 carbon atoms selected from the group consist-ing of hydroxyalkyl diacetone acrylamides and meth-acrylamides, hydroxyalkyl acrylamides and methacryl-amides, N-alkyol acrylamides and methacrylamides, and mixtures thereof; vinyl ethers containing 4 to 22 carbon atoms; vinyl ketones containing 3 to 12 carbon atoms; vinyl esters of carboxylic acids con-taining 4 to 22 carbon atoms; alpha olefins containing 2 to 12 carbon atoms; styrene and styrene derivatives;
and mixtures thereof.
and mixtures thereof.
3. Oil filter of claim 2 wherein amount of said cross-linking resin is in the range of about 5 to 20% by weight based on the weight of latex solids and wherein amount of said catalyst is in the range of 5 to 20% by weight based on the weight of the cross-linking resin.
4. Oil filter of claim 3 wherein said latex is selected from copolymers of 40 to 70% vinyl chloride, 30 to 60% lower alkyl acrylate and one or more mono-mers selected from-acrylic acid and N-alkylol acryl-amide, based on the total weight of all monomers used to make the latex.
5. Oil filter of claim 4 wherein amount of acrylic acid is 0.5 to 3% and amount of N-alkylol acrylamide is 0.5 to 2%, said lower alkyl acrylate containing 1 to 8 carbon atoms in the alkyl group and said N-alkylol acrylamide containing 1 to 4 carbon atoms in the alkylol group.
6. Oil filter of claim 5 wherein said N-alkylol acrylamide is N-methylol acrylamide, said cross-linking resin is emulsified epoxy resin, and said filter sub-strate requires a single cure of the binder during its preparation.
7. Filter substrate of claim 3 wherein said catalyst is selected from ammonium chloride, tridi-methyl aminoethyl phenol, and mixtures thereof.
8. Oil filter of claim 2 wherein said catalyst is selected from ammonium chloride, tridimethyl amino-ethyl phenol, and mixtures thereof.
9. Oil filter substrate comprising a substrate impregnated with a cured binder, said substrate being resistant to hot oil at 177°C. when immersed therein for 96 hours, said binder comprising a water-based latex selected from the group consisting of water insoluble homopolymers of vinyl halide or vinylidene halide and water insoluble copolymers of vinyl halide and/or vinylidene halide with one or more of copoly-merizable monomers having a latex solids concentration of about 5 to 70% by weight, a cross-linking resin, and 1 to 30 weight parts per 100 weight parts of latex solids of a catalyst for promoting the cross-linking of said latex, said copolymers contain at least 20%
by weight of latex solids of a polymerized vinyl halide, said substrate is selected from filter paper and non-woven fibers; and said cross-linking resin is selected from epoxy resins, melamine-formaldehyde resins, melamine resins, phenol-formaldehyde resins, polyacryl-ate resins, and mixtures thereof.
by weight of latex solids of a polymerized vinyl halide, said substrate is selected from filter paper and non-woven fibers; and said cross-linking resin is selected from epoxy resins, melamine-formaldehyde resins, melamine resins, phenol-formaldehyde resins, polyacryl-ate resins, and mixtures thereof.
10. Filter substrate of claim 9 wherein amount of said cross-linking resin is in the range of about 5 to 20% by weight, based on the weight of latex solids, and wherein amount of said catalyst is in the range of 5 to 20% by weight, based on the weight of the cross-linking resin.
11. Filter substrate of claim 10 wherein said latex is selected from copolymers of 40 to 70% vinyl chloride, 30 to 60% lower alkyl acrylate and one or more monomers selected from acrylic acid and N-alkylol acrylamide, based on the total weight of all monomers used to make the latex.
12. Filter substrate of claim 11 wherein amount of acrylic acid is 0.5 to 3% and amount of N-alkylol acrylamide is 0.5 to 2%, said lower alkyl acrylate containing 1 to 8 carbon atoms in the alkyl group and said N-alkylol acrylamide containing 1 to 4 carbon atoms in the alkylol group.
13. Filter substrate of claim 12 wherein said N-alkylol acrylamide is N-methylol acrylamide, said cross-linking resin is emulsified epoxy resin, and said filter substrate requires a single cure of the binder during its preparation.
14. Oil filter of claim 1, 2 or 3, wherein said cross-linking resin is selected from emulsified epoxy resins, lower alkoxy lower alkyl melamine resins, and polyacrylate resins containing pendant unsaturation.
15. Filter substrate of claim 9, 10 or 11, wherein said binder includes a cross-linking resin selected from emulsified exposy resins, lower alkoxy lower alkyl melamine resins and polyacrylate resins containing pendant unsaturation.
16. Oil filter of claim 1, 2 or 3, wherein said binder is selected from copolymers of 40 to 70%
vinyl chloride, 30 to 60% lower alkyl acrylate of 1 to 8 carbon atoms and one or more monomers selected from 0.5 to 3% acrylic acid and 0.5 to 2% N-alkylol acrylamide, of 1 to 4 carbon atoms, based on the total weight of all monomers used to make the latex;
wherein said filter substrate is selected from filter paper and nonwoven fabric containing 5 to 50% by weight of latex solids; wherein said cross-linking resin is emulsified expoxy resin; said filter sub-strate requiring a single cure of the binder during its preparation and is able to withstand a hot oil immersion test.
vinyl chloride, 30 to 60% lower alkyl acrylate of 1 to 8 carbon atoms and one or more monomers selected from 0.5 to 3% acrylic acid and 0.5 to 2% N-alkylol acrylamide, of 1 to 4 carbon atoms, based on the total weight of all monomers used to make the latex;
wherein said filter substrate is selected from filter paper and nonwoven fabric containing 5 to 50% by weight of latex solids; wherein said cross-linking resin is emulsified expoxy resin; said filter sub-strate requiring a single cure of the binder during its preparation and is able to withstand a hot oil immersion test.
17. Filter substrate of claim 9 or 10, wherein said binder is selected from copolymers of 40 to 70%
vinyl chloride, 30 to 60% lower alkyl arcylate of 1 to 8 carbon atoms and one or more monomers selected from 0.5 to 3% acrylic acid and 0.5 to 2% N-alkylol acrylamide, of 1 to 4 carbon atoms, based on the total weight of all monomers used to make the latex;
wherein said filter substrate is selected from filter paper and nonwoven fabric containing 5 to 50% by weight of latex solids; wherein said cross-linking resin is emulsified epoxy resin; said filter sub-strate requiring a single cure of the binder during its preparation and is able to withstand a hot oil immersion test.
vinyl chloride, 30 to 60% lower alkyl arcylate of 1 to 8 carbon atoms and one or more monomers selected from 0.5 to 3% acrylic acid and 0.5 to 2% N-alkylol acrylamide, of 1 to 4 carbon atoms, based on the total weight of all monomers used to make the latex;
wherein said filter substrate is selected from filter paper and nonwoven fabric containing 5 to 50% by weight of latex solids; wherein said cross-linking resin is emulsified epoxy resin; said filter sub-strate requiring a single cure of the binder during its preparation and is able to withstand a hot oil immersion test.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US665,478 | 1976-03-10 | ||
US06/665,478 US4623462A (en) | 1984-10-29 | 1984-10-29 | Oil filters using water-based latex binders |
Publications (1)
Publication Number | Publication Date |
---|---|
CA1279795C true CA1279795C (en) | 1991-02-05 |
Family
ID=24670269
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CA000493253A Expired - Fee Related CA1279795C (en) | 1984-10-29 | 1985-10-18 | Oil filters using water-based latex binders |
Country Status (10)
Country | Link |
---|---|
US (1) | US4623462A (en) |
EP (1) | EP0181540A3 (en) |
JP (1) | JPS61111116A (en) |
KR (1) | KR860003045A (en) |
CN (1) | CN85107940A (en) |
AU (1) | AU4831285A (en) |
BR (1) | BR8505311A (en) |
CA (1) | CA1279795C (en) |
ES (1) | ES8701509A1 (en) |
FI (1) | FI854213L (en) |
Families Citing this family (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AU594495B2 (en) * | 1986-09-02 | 1990-03-08 | Fumakilla Limited | Heat fumigation apparatus |
US4999239A (en) * | 1989-03-20 | 1991-03-12 | Air Products And Chemicals, Inc. | Ethylene-vinyl chloride copolymer emulsions containing tetramethylol glycoluril for use as binder compositions |
US5334648A (en) * | 1991-10-30 | 1994-08-02 | The B. F. Goodrich Company | Emulsion polymers for use as a urea formaldehyde resin modifier |
US5244695A (en) * | 1992-03-17 | 1993-09-14 | Air Products And Chemicals, Inc. | Aqueous binder saturants used in a process for making nonwoven filters |
JP3256330B2 (en) * | 1993-05-28 | 2002-02-12 | 三井化学株式会社 | Water-resistant surface coating agent and coated paper using the same |
IT1287629B1 (en) | 1996-03-06 | 1998-08-06 | Universal Filter Spa | PROCESS FOR MANUFACTURE OF FILTER MEDIA, MEDIA SO MANUFACTURED, AND FILTERS USING SAID MEDIA |
US5795649A (en) * | 1996-06-03 | 1998-08-18 | Ici Americas Inc. | Release film and method of making thereof |
IT1283450B1 (en) * | 1996-07-18 | 1998-04-21 | Fad Fabriano Autoadesivi S P A | FILTERING MEDIA IN THE FORM OF A PAPER SHEET FOR FILTERS OF FLUIDS IN GENERAL |
AU6375300A (en) * | 1999-07-30 | 2001-02-19 | Donaldson Company Inc. | Cellulose based filter media and cartridge apparatus |
US6599638B1 (en) * | 1999-09-10 | 2003-07-29 | Dow Reichhold Specialty Latex Llc | Colloidally stabilized emulsions |
US6390305B1 (en) | 2000-05-19 | 2002-05-21 | Air Products Polymers, L.P. | Saturant binder systems for high performance air and oil filters |
DE10310882A1 (en) * | 2003-03-11 | 2004-09-23 | Basf Ag | Use of aqueous binders in the manufacture of filter materials |
US20060090436A1 (en) * | 2004-10-29 | 2006-05-04 | Georgia-Pacific Resins, Inc. | Filter media saturating resole resin |
JP4264108B2 (en) * | 2007-01-11 | 2009-05-13 | 横浜ゴム株式会社 | Curable resin composition |
DE102009006584B4 (en) * | 2009-01-29 | 2011-06-01 | Neenah Gessner Gmbh | Single or multi-layer filter material, filter element of such a material and method for its production |
WO2015168462A1 (en) * | 2014-04-30 | 2015-11-05 | K&N Engineering, Inc. | Filter oil formulation |
CN107974206A (en) * | 2017-12-18 | 2018-05-01 | 安徽新立滤清器有限公司 | A kind of filter high viscosity binding agent |
Family Cites Families (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
BE550356A (en) * | 1955-08-17 | |||
US3224592A (en) * | 1963-09-04 | 1965-12-21 | Robert L Burns | Oil filter for an internal-combustion engine |
BE654181A (en) * | 1963-10-10 | |||
US3520416A (en) * | 1968-02-12 | 1970-07-14 | Pall Corp | Liquid and gas-permeable microporous materials and process for making the same |
US3788878A (en) * | 1972-07-14 | 1974-01-29 | Goodrich Co B F | Impregnating nonwovens with an alkyl acrylate polymer-carboxylic polymer latex |
NL7308406A (en) * | 1973-06-18 | 1974-12-20 | ||
SU486762A1 (en) * | 1973-12-26 | 1975-10-05 | Всесоюзный Научно-Исследовательский Институт Молочной Промышленности | Method for preparing filtered milk material |
JPS51105406A (en) * | 1975-02-12 | 1976-09-18 | Mitsubishi Paper Mills Ltd | Senishiito * b * noseizoho |
GB1522280A (en) * | 1976-06-01 | 1978-08-23 | Hollingsworth & Vose Co | Filter medium and method of making same |
GB1599483A (en) * | 1977-02-17 | 1981-10-07 | Exxon Research Engineering Co | Wax separation process |
JPS57113810A (en) * | 1980-12-29 | 1982-07-15 | Japan Exlan Co Ltd | Dewatering filter and dewatering method for water-containing oil |
US4333971A (en) * | 1981-06-05 | 1982-06-08 | Monsanto Company | Substrate treating compositions |
-
1984
- 1984-10-29 US US06/665,478 patent/US4623462A/en not_active Expired - Fee Related
-
1985
- 1985-10-04 AU AU48312/85A patent/AU4831285A/en not_active Abandoned
- 1985-10-18 CA CA000493253A patent/CA1279795C/en not_active Expired - Fee Related
- 1985-10-24 BR BR8505311A patent/BR8505311A/en unknown
- 1985-10-24 EP EP85113554A patent/EP0181540A3/en not_active Withdrawn
- 1985-10-25 ES ES548230A patent/ES8701509A1/en not_active Expired
- 1985-10-28 FI FI854213A patent/FI854213L/en not_active Application Discontinuation
- 1985-10-28 JP JP60239627A patent/JPS61111116A/en active Pending
- 1985-10-28 CN CN198585107940A patent/CN85107940A/en active Pending
- 1985-10-29 KR KR1019850007996A patent/KR860003045A/en not_active Application Discontinuation
Also Published As
Publication number | Publication date |
---|---|
ES548230A0 (en) | 1986-12-01 |
AU4831285A (en) | 1986-05-08 |
KR860003045A (en) | 1986-05-19 |
CN85107940A (en) | 1986-05-10 |
ES8701509A1 (en) | 1986-12-01 |
EP0181540A3 (en) | 1988-09-21 |
JPS61111116A (en) | 1986-05-29 |
FI854213L (en) | 1986-04-30 |
US4623462A (en) | 1986-11-18 |
BR8505311A (en) | 1986-08-05 |
EP0181540A2 (en) | 1986-05-21 |
FI854213A0 (en) | 1985-10-28 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CA1279795C (en) | Oil filters using water-based latex binders | |
US5498658A (en) | Formaldehyde-free latex for use as a binder or coating | |
US5536766A (en) | Formaldehyde-free binding, impregnating or coating compositions for fibrous sheet materials | |
US3996181A (en) | Aqueous composition containing acrylic or butadiene polymers | |
US3694393A (en) | Method of producing paper,and paper obtained | |
US4455342A (en) | Acrylic resin dispersions | |
US4002801A (en) | Heat sealable articles treated with vinyl halide polymer latices | |
US4524093A (en) | Fabric coating composition with low formaldehyde evolution | |
US5244695A (en) | Aqueous binder saturants used in a process for making nonwoven filters | |
EP0192710B1 (en) | Acrylic emulsion copolymers | |
US4374894A (en) | Polyolefin nonwovens with high wet strength retention bonded with vinyl chloride copolymers | |
EP0261378B1 (en) | Heat resistant binders | |
EP0312008B1 (en) | Heat resistant acrylic binders for nonwovens | |
US4942086A (en) | Two-stage heat resistant binders for nonwovens | |
JP2002212372A (en) | Reduced formaldehyde nonwoven fabric binder containing polymerized unit of n-methylolacrylamide | |
CA1279744C (en) | Formaldehyde-free latex and fabrics made therewith | |
US7247586B2 (en) | Vinyl acetate/ethylene and vinyl chloride polymer blends as binders for nonwoven products | |
US4962141A (en) | Ethylene-vinyl chloride copolymer emulsions containing tetramethylol glycoluril for use as binder compositions | |
CA1297217C (en) | Ethylene vinyl acetate compositions for dielectric sealing applications | |
US5011712A (en) | Formaldehyde-free heat resistant binders for nonwovens | |
EP0017364A1 (en) | Radiation-curable allyl benzoylbenzoate copolymers, their use, products thereof, and methods of making these products | |
EP0439314A2 (en) | Process for the manufacture of wood composition boards, prepress sealer compositions and use thereof | |
US5087487A (en) | Non-thermoplastic binder for use in processing textile articles | |
US3068121A (en) | Pressure sensitive adhesive tape and paper backing element impregnated with an acrylic ester copolymer and a water-dispersible aldehyde resin | |
US4999239A (en) | Ethylene-vinyl chloride copolymer emulsions containing tetramethylol glycoluril for use as binder compositions |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
MKLA | Lapsed |