CA1055863A

CA1055863A - Laundering pre-spotter and method of production

Info

Publication number: CA1055863A
Application number: CA238,585A
Authority: CA
Inventors: John H. Barrett (Jr.); Brian P. Flynn
Original assignee: Purex Corp
Current assignee: Purex Corp
Priority date: 1974-11-08
Filing date: 1975-10-29
Publication date: 1979-06-05
Also published as: AU502125B2; GB1528366A; US3953353A; JPS5170388A; FR2290491A1; AU8619275A

Abstract

A B S T R A C T
A solid product for rub-on application to stains and soil deposits on fabric preparatory to laundering, comprising blended water soluble non-ionic detergent and stable laundry enzyme uniformly dispersed therein, and the method of manufacturing the product.

Description

1~)55~3i63 The p~esent invention rel~tes to a solid product for rub-on application to staills and soll deposits on ~abric preparatory to launderlng, and a method of manufacturing the product.
Laundry prespotters have long been known and used to treat fabric stains which resist the usual washing pro-cesses. The advent and increasing use of hydrophobic synthetic fibers in place of cotton has created a need for ~mproved stain treatments to combat the affinity of such f~bers for greasy soils as well as other wash resistant soils. The application of permanent press finishes to cot-ton and cotton blends also has accentuated the need or e~fective prespotters designcd or romoval o a multipli-city of grease and food based stains.
The present invention therefore provides a detergent article in stick form for rub-on application to stains and soil deposits on fabrics preparatory to laundering, the article comprising a water soluble solid product which com-prises a mixture of non-ionic detergentsJ the solid product having ASTM penetrometer hardness between about ~.5 and 10.5 measured using a standard needle with 50 gram load.
The present invention further provides a process of manufacturing the detergent article of the preceding para-graph that includes heating the product mixture composition -for conversion to fluid state, pumping the heated mixture -through a cooling zone from which the mixture passes to a filling head, dispensing the mixture from said head into containers wherein the mixture is further cooled and solidified, and recirculating residual fluid from the ' .
. . .

dispensing head through a heating zone and returning the heated mixture -to the supply chamber.
Prior art prespotters in the form of liquids, powclers, aerosols ancl s-ticks are known.
Liquids containing specific chemical reagents acting to decolorize or remove certain stains by means of chemical reaction on the stain are known (e.g. the familiar two solution '~ink eradicator"), as are solid sticks containing specific chemicals or solvents to react with or clissolve specific stains. None of these stain removers are effec-tive against a wide spectrum of stains.
Liquid laundry detergents have been recommended for direct application to heavily soiled areas. Laundry bar soaps and dry powdered detergents have been similarly recomrnended for applicat.ion to moistened soiled Eabrics.
Dry products, some containing enzyrnes, have been marketed for use with water to form a pre-soak solution in which heavily stained articles are immersed for a time prior to ~$~5~

.

~0558~ii3 laundering. Each of the foregoing suffer rom the disadvan-tage o~ inconvenience in use, need for dilution with water with accompanying loss of effectiveness, tendency to spill, tendency to contact the skin, danger of accidental ingestion or failure to affect a broad spectrum of stains.
Aerosol prespotters, some containing enzymes, are known, but these suffer the disadvantages common to aerosols such as~ flammability, inhalation danger, depletion of atmospheric ozonQ, and the problem of safe disposal of empty containers.
Liquid prespotters, some containing enzymes, are known but these share with the other liquids mentioned above inconvenience in use, tendency to spill, ana danger of accidental ingestion.
The present invention providas, for rub-on appli-cation to stains and soil deposits on fabrics preparatory to laundering, the solid product consisting essentially of water soluble nonionic detergent and stable laundry enzyme uniformly dispersed therein.
Prefera~ly, the prespotter i5 provided in solid form of nonionic detercfent and enzvme composition which is free of all of the above cited disadvantages associated with prior art compositions; which is particularily well suited for use on all fabrics - both traditional and modern, both sturdy and delicate; which applies direc-tly on a stain a maximum concentration of effective soil removing agents, and which is effective on a broad spectrum of soils. Accord-ingly, we have provided a prespotter which can be molded in the form of a stick with structural rigidity suficient to permit forceful application to a soiled fabric r enough ..

~05586;3 softness to permit substantial quantities to become trans-ferred to the soiled fabric as a consequence of being rubbed against the fabric, sufficient plastlcity to prevent crack-ing orcrumbling in use, and yet able to withstand prolonged storage at elevated temperatures up to about 125F.
No single nonionic detergent is known which em~
bodies all of the desired features. Those which are solid at room temperatures are either too hard and brittle, or are : :
not sufficiently resistant to high temperatures often en~
countered in warehouse storage.
We have discovered that suitable physical charac-teristics may be obtained with certain substantially anhy-drou~ mixtures o m~terials yielding solid masses having a combination of hardness and plasticity such that the ASTM
Penetrometer hardness, using a standard needle with a 50 gram load, is between 4.5 and 10.5 mm and preferably between 6.5 and 8.5 mm; together with a melting point of 125F to 140F and preferably between 128~F to 134F when measured by the method of Class II materials of the Pharmacopeia of the United States, Revision XVIII. The expression "essen- ?
tially anhydrous" is used ln the product description and definition in recognition that the p.roduct may not be strict-ly anhydrous because of minor accummulations of moisture in the mixture ingredients during storage or as received from ~5 the suppliers. The product moisture content wi.ll not be ~
substantial and usually below a maximum of 2%. We have found these substantially anhydrous mixtures to be effective vehicles for applying enzymes to stains while affording ex-~ .
cellent long term storage stability with respect to enzyme ., , ~ .
potency.

" ,.

~05~3 .~
A presently preferred product is composed o an intimate mixture of.
A. 5-40% waxy solid, preferably water soluble nonionic which imparts body and harness, B. 10-6G% solid nonionic detergents having effective sur-factant and stain removing properties, C. 10-75~ uid nonionics serving to plasticize ~he mix-ture and which preerably also act as ~ffective surfactants, and D. .01-10% laundry enzyme.
Examples of these typical compositions as to their A, B, and C components are: ~
,$ 1) A: 20% Carbowax~ 000 ~Union Carbide's polyethylene glycol 4000 with mol. wt. 3000-3700) B: 30% Pluronic F-68 (BASF Wyandotte's polyethylene oxide polypropylene propylene glycol containing about 80% ethylene oxide on a hydrophobe of about 1750 mol. wt.) C: 50% Igepal C0-630 (GAF's polyethoxylated nonyl phenol containing an average of 9.5 moles of ethylene oxide).

2) A: 20% Carbowax 6000 (Union Carbide's polyethylene glycol 6000 with mol. wt. of 6000-7500) B: 30% Plurafac A-38 (BASF Wyandotte's polyethoxylated ~atty alcohol, believed to contain about 12 moles ethylene oxide) C: 50% Igepal CO-630

3) A: 10%~Carbowax 6000 B: 25~ T-Det N-30 (Thompson-Hayward Chemical's poly-ethoxylated nonyl phenol containing an average of ~ ~r~.de ~ri~ 5 ~05~363 - -"
30 moles of ethylene oxide) "~J/~ C: 65~ Igepal C0-630

4) A: 20% Carbow x 6000 B: 30% Neodol 25-12 (Shell Chemical's pol~ethoxylated ~ .
C12-C15 primary linear alcohol with 12 moles of ethylene oxide) and 30~ Pluroni.c EA-7135 ~BASF .
Wyandotte's polyethoxylated fat:ty alcohol believed to contain about 100 moles of ethylene oxide).
C: 20~ Igepal C0-630 :

5) A: 25~ Carbowax 6000 B: 50% Neodol 25-12 C: 25~ Neodol 23-6.5 (Shell Chemical's polyethoxylated C12-C13 primary linear alcohols wlth an average of

6.5 moles of ethylene oxide) The above examples provide a solid composition ~.
having nearly optimum strength, plasticity, hardness and resistance to high storage temperatures while.providing high concentrations of effective surfactants. We have found that useful solid compositions can be achieved without using any waxy component (A) by combining from 40 to 90% o a solid nonionic de~ergent ~B) with from 10 to 60% o a liquid non-ionic (C). Examples of suah compositions are:
6) B: 40% Pluronic F-68 :
C: 60~ Igepal CO-630 ;;

7) B: 50% Pluronic EA-7135 C: 50% Carbowax 400 (Union Carbide's polyethylene glycol ~
400 with a mol. wt. o~ 380-420.) .;
The compositions of examples 6 and 7 melt about 120F, in contrast to examples 1-5 which melt at about 130F.
The last two examples are therefore, less resistant to high ~:-~ rr~ r~ 6 ~0~5~63 storage temperatures and correspondingly less desirable.
We have further found that useful solid composi-tions can be achieved without use of solid nonionic deter-gent (B) by combining from 40 to 70% of a waxy component (A) 5 with from 30 to 60% of a liquid nonionic detergent (C). An example of such a composition is:
' ~ 8) A: 60% Carbowax 4000 C: 40~ IgepalrC0-630 The composition of example 8 has desirable physi'cal characteristics, but imparts to treated stains less active surfactant than any of the more preferred compositions 1-5.
Dry powdered, granulated or prilled enzymes may be incorpoxated in any of the above compositions to produce a final composition containing Erom about 0.01% to 10.0% of enzyme. An example of such a composition is:
9) A: 10% Carbowax 6000 B: 25~ T-Det N-30 C: 64.5~ Igepal C0-630 D: 0.5~ Esperase P.4.0 (Novo's prilled proteolytic enzyme--see below under "Enzymes") The composition o~ e~ample 9 has all o~ the a~ore-mentioned desirable attributes and in addition is highly effective in removing protein bound soils such as grass stains, as well as a wide spectrum of common stains such as grease, oil, lipstick, ball point pen ink, mascara, gravy, etc.
The above-named ingredients have substan~ially the following melting temperatures:
- A: 100 to 200F
B: 85 to 165F

Tr~e ~r~ 7 ~558~i3 ,`

C: -40 to 80F
SUITABLE RAW MATERIAI S
A. Waxes: ~he following materials are suitable for use as the solid component A . These materials are all waxy in nature with melting points abvve about 100F and preferably above 120F and may be differentiated from the solid nonionic detergents described below in that they con- ~:
tain either hydrophobic or hydrophilic molecul~s, but not both. Suitable naturally occurring materials include vege-table waxes such as carnauba wax, candelilla wax, Japan wax, ~-Ocuricury wax, sugarcane wax, palm wax, raffia wax, esparto wax, and Douglas fir bark wax; animal waxes such as beeswax, Chinese wax, shellac, and spermaceti; mineral waxes such as Montan wax, ozocerite and ceresin wax~ and petroleum waxes .
such as re~ined paraf~in and mlcrocrystalline waxes.
Further suitable waxy materials are the synthetic waxes such as cetyl alcohol, stearyl alcohol or high molecu- :
lar weight alcohols having 20 or more carbons; higher mole-. cular weight saturated fatty acids with at least 12 carbons.
More pre~erred by virtue of being water soluble or at least . .
water dispersable are such synthetic waxes as esters of polyhydric alcohols including glycerol mono-, di-, and.tri-stearates, ethylene glycol palmitate, ethylene glycol stear- .
ate, ethylene glycol dilaurate, ethylene glycol dimyristate, . ; ~.
ethylene glycol dipalmitate, ethylene glycol disteàrate, .~: :
propylene glycol palmitate/ propylene glycol stearate, pro~
pylene glycol dilaurate, propylene glycol dipalmitate, pro~
pylene glycol distearate, methoxy polyethlene glycols with . molecular weights from 1900 to 5,000, polyethylene glycols :
with molecular weights from 1300 to 20,000, and the like.

,, : .
. .

lQ~51!3~;~

Especially preferred are the polyethylene glycols with average molecular weights from about 3,000 to about 8,000.
~Carbowax 4000 and Carbowax 6000, Union Carbide Co.~.
B. Nonionic Detergents: Those suitable for use as the solid component B include all homologues of the classes described below whose melting point is about 80~F
and preferably above 100F. Those nonionic detergents suitable for use as liquid component C include all homologues of the classes described below with melting points below 80F and preferably below about 60F.
The term "nonionic detergent" as used herein may be defined to include all surface active ayents possessing~
within their molecule both a hydrophilic group and hydro-phobic group and which do not ionize in aqueous solution.
Nonionic detergents are usually, but not necessarily, com-posed of the condensation products of ethylene oxide and propylene oxide with hydrophobic organic molecules and con-tain an average of 6 to 100 moles of alkylene oxide per mole of hydrophobe.
Suitable nonionic detergents are the polyoxy-alkylene alkylphenols where in the hydrophobic group con-tains a phenolic nucleus have a substituent alkyl group of at least 4 but preferably 8 to 12 carbon atoms and the hy-drophilic portion is comprised of at least 3 but preferably 6 to 100 moles of ethylene oxide or propylene oxide per ~:~
mole of alkylphenol. Exemplary of this type are ethoxylated nonylph~nols with an average. ethylene oxide content of 9.5 moles per mole of nonylphenol ~Igepal C0-630 GAF) suitable for use as the liquid component C and those with an average ethylene oxide content of 30 moles per mole of nonylphenol 'g ,. , . , , ,. . ,.,, . ,, . :.
, , ~S~63 (Igepal C0-880 GAF) suitable for use as the solid component B.
Also suitable nonionic dete:rgents are the poly-oxyalkylene alcohols wherein the hydrophobic group is de-rived from natural or synthetic primary or secondary straight chain fatty alcohols having about 8 to 22 carbon atoms and :~
the hydrophilic group is composed of at least 3 but prefer-ably 5 to 100 moles of ethylene oxide or propylene oxide.
Exemplary of this type of nonionic surfactant are secondary alcohol ethyoxylates having 11 to 15 carbons in the secondary alcohol hydrophobe. Those with an average ethylene oxide content of 12 moles- of ethylene.oxide, (Tergi-tol 15~S-12 Union Carbide) are.suitable for use as thq solid "B" component while those containing 9 moles of ethylene oxide (Tergitol 15-S-9 Union Carbide) can be used as the liquid C componant.
Othe.r suitable nonionic detergents are the poly- ~
alkylene esters of the higher organic acids usually having ~ .-

- 8 or more carbon atoms in the acid hydrophobe, and 10 or more moles of ethylene oxide as the hydrophilic group. ` .
Naturally occurriny fatty acids o~ either animal or vegeta-ble origin may be used, as well as tall-oil fatty acids or rosin acids. Synthetically derived fatty acids are also suitable as hydrophobes. Exemplary of this class are a polyoxyethylene stearate having 50 moles of ethylene oxide per mole of stearic acid (Myrj 53, Atlas Chemical Ind.), suitable for use as solid component B ; and a polyoxy-ethylene condensate of naturally occurring coconut fatty acids having 5 moles of ethylene oxide per mole of coconut fatty acids (Ethofat C/15, Armak Co.), suitable for use as 11~5~ 3 liquid component C.
Still other suitable nonionic detergents are the polyalkylene alkylamines whose hydrophobic group is from a primary, secondary, or tertiary amine and whose ethylene oxide content is sufficiently high to impart both water solubility and nonionic chaxacteristics in neutral and alka-line environments. Useful hydrophobic groups include the amines of fatty acids with 8 or more carbons or naturally occurring mixtures thereof, n-alkyl-l, 3-propanediamine where the alkyl group is derived from ~atty acids of 8 or more carbons, t-aliphatic alkylamines with 12 or more-car-bons, and dehydroabietylamines. Exemplary of this type of nonionic detergent are polyoxyethylene t-aliphatic amine~
wherein the aliphatic amine has ~rom 12 to 14 carbons and the hydrophilic group an average of 15 moles of ethylene oxide per mole of amine (Priminox R-15, Rohm & Haas Co.), suitable for use as liquia component C ; or wherein the ali-phatic group contains from 18 to 22 carbons and there is an average of 25 moles of ethylene oxide per mole of amine (Priminox T-25, Rohm & Haas Co.), suitable for use as the solid component B.
Further suitable nonionic detergents are the polyalkylene alkylamides having a hydrophobic group derived from an amide of a fatty acid or ester, including napthenic ~5 esters and monoesters of dicarboxylic acids. EIydrophobic , groups such as sulfonamides, imides, carbamnates, urea, guanidine and imidazoline are similarly usefulO Examples of this class are the polyoxyethylene amide of hydrogenated .tallow fatty acids having 60 moles of ethylene oxide per 30 . mole of hydrophobe (Ethomid HT-60, Armak Co.), suitable for .' ' ' .
iQ
.

~ ~5~63 use as the solid component B and the polyoxyethylene amide of oleic acid having 5 moles of ethylene oxide per mole of hydrophobe (Ethomid 0/15, Armak Co.), suitable for use as the liquid component C .
A further class of suitable nonionic detergents are the fatty acid esters of various polyols. These include the fatty acid esters of alkylene glycvls, glycerols, poly-glycerols, hexitols and sugars and their polyoxyethylene condensates. Exemplary of these nonionics are the polyoxy- . ~
ethylene sorbitan monostearate containing 20 moles of ethy ~:
lene oxide per mole of hydrophobe (Tween 60, Atlas Chemical Div. I.C.I America) suitable Eor use as the liquid component C and polyoxyeth~lene sorbitan tristearate containing 20 moles o ethylene oxide per mole of hydrophobe (~ween .
65, Atlas Chemical Div. I.C.I America), suitable for use as the solid component B . :
An additional group of suitable nonionic deter-gents are the polyalkylene oxide block copolymers made by condensing alkylene oxides with a hydrophobic base itself obtained by condensing alkylene oxides with a reactive ox ganic molecule~ The ~ydrophobic base usually has a molecu-lar weight of 500 to 2000 and the polyoxyalkylene hydrophilic portion may constitute from about 10~ to about 95% of the total copolymer. The hydrophilic bases for these block copolymers are formed by the addition of one alkylene oxide to a mono or polyfunctional organic molecule having one or more reactivë hydrogen atoms or hydroxyl groups, followed by the addition of more of the same alkylene oxide, a dif-ferent alkylene oxide, or a fixed or varied ratio of two or more mixed alkylene oxides. Suitable starting no or .
10rK . 12 .

1~55l5 63 polyfunctional organic compounds include aliphatic and aro-matic alcohols, acids, mercaptanes, amines, amides, glycols, glycerols and sugars. Alkylene oxides which may be used in ~ -the condensation to form ~he hydrophobe include propylene, butylene, styrene, cyclohexane, amylene. The hydrophilic polymer chain is usually polyoxye~hylene but may also con-tain higher oxyalkylenes such as oxypropylene and oxybuty-lene. Exemplary of this group of nonionic detergents are polyoxyethylene polyoxypropylene glycols based on a hydro-phobic polymer made by condensing propylene oxide with pro-pylene glycol and having an average molecular weight of about 1750 and having an added hydrophilic group o poly-oxyethylene. Such a polyol wherein the hydrophilic group comprises about 30% of the whole by weight (Pluronic ~63, BASF Wyandotte Co.), is suitable for use as liquid component C and that wherein the hydrophilic group comprises about 80% of the whole by weight ;(Pluronic F-68, BSAF Wyandotte Co.) is suitable for use as the solid component 'B .
Further suitable miscellaneous types of nonionic deterg~nts which may find use as either liquid component C
or solid compenent B include fatty alkanolamides such as the monoethanolamides, diethanolamides and isopropanolamides wherein the acyl radical has about 10 to 14 carbons; amine oxides wherein at least one substituent on the nitrogen is of an alliphatic, aromatic, heterocyclic or alicyclic radi-cal containing 6 or more carbons; sulfoxides; phosphine oxides; acetylenic glycols; and polyoxyethylene acetylenic glycols.
C. Other Nonionic Liquids: In addition to those nonionic detergents cited above which are suitable for use - ,.

, ~I:lS5~6~
as liquid component C by xeason of having a melting point below 80F and preferably below about 60F, we find other nonionic liquids are useful as liquid component C by virtue of serving as a plasticiser despite the lack of significant detergent function. We find the suitable plasticisers may be selected ~rom the mono-, di-, and polyhydric alcohols, their alkyl or aryl ethers, their alkyl esters, or their alkoxy derivitives which are liquid above about 80F. ~ `
For example, ethylene glycol, glycerine, l-hexanol, glyceryl triacetate or propylene glycol monomethyl ether may be used.
D. Enzymes: The enzymes suitable for use-in this stick prespotter are generally well described by McCarty q in U. S. Pat. #~,519,570. Applicable for our purposes are the hydrolase enzymes referred to in column 4 o~ the McCarty patent. Since McCarty, an improved physical orm of enzyme has become commercially availabIe and is now preferred over the dry powders he describes.
The presently preferred physical form of enzyme is known as "prilled enzymes". Prilled enzymes may consist of any o~ the above described commercially produced con-centrated dry powdered laundry enzymes which have been rendered dust free and free flowing by having been encapsu-lated in spherical particles of an inert substance, usually a high melting water soluble wax such as one of those de-scribed abo~e as suitable for use as the solid componentA , or a high melting nonionic detergent such as one of those described above as suitable for use as solid component B . Especially preferred for manufacture of prilled enzymes intended for incorporation in detergent products are the highly ethoxylated fatty alcohols containing about 50 moles }4 .

~()s~

of ethylene oxide per mole of alcohol. Commercially avail-able prilled en~ymes are spherical particles usually between 100 and 100~ microns in diameter. A prilled enzyme product preferred for use in the compositions of this invention is Esperase P 4.0 manufactured by Novo Industri A/S of Copenhagen, Denmark. The primary enzyme component of Esperase P ~.O is described by the manufacturer as being a subtilisin(EC number 3.4.4.16C, Dixon ~ Webb, ENZYhlES, second edition, 1964) iden-tical to that contained in Alcalase. ~
When Esperase P 4.~ is incorporated in the com- ;
positions of this invention by the methods herein described, its encapsulating agent melts, dissolves in and disperses throughout the molten mixture, thus releasing the finely divided powdered active enzyme which in turn, with mechanical agitation, becomes uniformly dispersed throughout.
IV. PROCESS OF MANUFACTURE
: .
We have discovered a process of manufacture by which the ingredients of our invention can be mixed and cast - ;
into a stick form that is homogenous in composition and free of crater-like surface depressions, while retaining the de-sired hardness, strength, plasticity and resistance to ele-vated storage temperatures.
The process is generally applicable to any of the contemplated compositions of our inventions with suit-able adjustments in melting and casting temperatures to accommodate variations in melting range of the waxy compo-nent ~A) and the solidification temperature of the final mass.
The present invention therefore further provides a process of manufacture of the product that includes heat-ing the product mixture composition for conversion to fluid 5~363 state, pumping the heated mixture through a cooling zone from which the mixture passes to a filling head, dispensing the mixture from said head into containers wher2in'the mix-ture is further cooled and solidified, and recirculating residual fluid from the dispensing head through a heating zone and returning the heated mixture to the supply chamber.
The preferred process involves the melting to-gether of the major components A, B and C, the addition of enzyme at a temperature below that which would cause de-naturation and loss o~ anzyme activi~y, supercooling theresultant melt and'immediately casting into a dispensing container and cooling to form a solid stick within the dis-pensing container.
In the process of manu~acturing the product, any combination of components A, B, and C as hereinabove de- ~ ' scribed and defined may be premixed with the anzyma ~ after the mixture has been heated and uniformly blended at a temperature below any temperature injurious to the enzyme.
The premix is introduced to what may be referred to as a supply chamber in which the blend with dispersed enzyme is maintained at a temperature sufficient'to assure pumpable ~luidity of the mixture, e.g. about 140F, by indirect heat txansfer as by cixculating hot water through a closed coil or a jacket about the chamber. The mixture is continuously ~5 stirred or agitated to maintain consistency of the composi-tion.
From the supply'chamber the mixture is pumped through cooling zone in the form of a coil immersed in lower temperature water to cool the pumped stream to a re-duced tempexature, e.g. of about 116F but which is variable ' 16 5~ E;.3 ~ :
in accordance with permissible changes in the compositionof the product. From the cooling coil the mixture passes under pump pressure through a recirculating filling head, e.g. of the piston type, from which the cooled,mixture is delivered into tubes which, for the purposes of forming pre-spotter sticks,'may be open'top cylinders being ad~anced in single file on a conveyor. As the i-ilLed tubes advance, ~;
beyond the ~illing head, they are cooled by circulation of, ambient or refrigerated air blown from a fan. When the top '' of each stick content has solidified, the tube may be capped '~
and allow~d to cool for an additional period until the mix~
ture is solidified throughout~ ~ ~ , ; ;
From the dispensing head the residual nuxture is recirculated to the supply chamber'through a heating zone in the form of an externally heated coil which elevates the temperature of the mixture to that maintained in the supply ~' chamber.
The process may be further detailed in reference ' to the specific composition of Example 9 given above. The mixture is prepared in the described manner by heating and agitating the mixture at a temperature of 150 ~ 10F.
Following uniform dispersion of the enzyme in the mixturer "
the latter is transferred to and held in the supply chamber at a tempexature of about 140-150F. The molten mixture is pumped through the cooling zone coil and cooled to a temper-ature of 114 t 1F. Immediately after the cooled mixture exits the cooling stage, it passes through the dispensing head into the ultimate dispensing containers. The filled containers are air cooled to a temperature of 80 -~ 10F.
For cylindrical containers of about 2.5 oz. contents and 1'7' , ~)S5~3 : :~
about 3 1/2 " height and 1 1/2 " diamete:r a cooling period of around 15 minutes in 80F air is adequate.

, .

Claims

The embodiments of the invention in which an exclusive property or privilege is claimed are defined as follows:

1. A detergent article in stick form for rub-on application to stains and soil deposits on fabrics preparatory to laundering, the article comprising a water soluble solid product which comprises a mixture of non-ionic detergents, the solid product having ASTM penetrom-eter hardness between about 4.5 and 10.5 measured using a standard needle with 50 gram load.

2. The article of claim 1 which is essentially an-hydrous and soap-free.

3. The article of claim 1 wherein said stick is cylindrical.

4. The article of claim 1 having a melting point between about 125°F and 140°F.

5. The article of claim 1 in which said nonionic detergent includes a blend of normally solid and normally liquid nonionic detergents.

6. The article of claim 5 in which the melting temperature ranges of said normally solid and liquid detergents are respectively about 80°F to 165°F, and -40°F
to 80°F.

7. The article of claim 5 in which said blend in-cludes a higher melting -temperature normally solid hard-ening wax having a melting temperature of about 100°F to 200°F.

8. The article of claim 7 further including a stable laundry enzyme uniformly dispersed therein and in which the weight percentages of said detergents and enzyme in said article are:
normally solid detergent 10 to 60%
normally liquid detergent 10 to 75%
wax 50 to 40%
enzyme 0.01 to 10%

9. The article of claim 7 or 8 in which said product is essentially anhydrous and soap-free.

10. The process of manufacturing the article defined in claim 1 that includes heating the product mixture com-position for conversion to fluid state, pumping the heated mixture through a cooling zone from which the mixture passes to a filling head, dispensing the mixture from said head into containers wherein the mixture is further cooled and solidified, and recirculating residual fluid from the dispensing head through a heating zone and returning the heated mixture to the supply chamber.

11. The process of claim 10 in which the mixture contains a relatively high temperature melting wax, a non-ionic detergent normally in solid form, and a normally liquid nonionic component and wherein the temperature of the circulated mixture is maintained above the solidifica-tion temperature of the wax.

12. The process of claim 11 in which the melting temperature ranges of the normally solid and liquid deter-gents and the wax component are respectively 80°F to 165°F, and -40°F to 80°F, and 100°F to 200°F.