US3341451A

US3341451A - Textile processing agents

Info

Publication number: US3341451A
Application number: US436264A
Authority: US
Inventors: Dziuba Wladyslaw Adam; Palmer Gordon
Original assignee: Courtaulds PLC
Current assignee: Akzo Nobel UK PLC
Priority date: 1964-03-06
Filing date: 1965-03-01
Publication date: 1967-09-12
Anticipated expiration: 1984-09-12
Also published as: GB1101360A; FR1436657A; SE316447B

Description

United States Patent 3,341,451 TEXTILE PROCESSING AGENTS Wladyslaw Adam Dziuba and Gordon Palmer, Coventry, England, assignors to Courtaulds Limited, London, England, a British company No Drawing. Filed Mar. 1, 1965, Ser. No. 436,264 Claims priority, application Great Britain, Mar. 6, 1964, 9,493/ 64 4 Claims. (Cl. 252- 85) The invention is concerned with textile processing agents used in the processing of natural and artificial fibres, filaments and the like, hereinafter included in the term fibres. The processing agents are particularly applicable to artificial fibres.

There are many different types of fibres, for example, regenerated cellulose, cellulose acetate, polyamide, polyester, polyolefin, and polyacrylonitrile including modacrylic fibres, which diifer in the ease with which they may be processed. Thus, each fibre has characteristic frictional and electrical properties. It is common practice to apply a processing agent suited to a particular fibre during its manufacture, in order to reduce the friction between the fibre and the parts of textile machines With which it comes into contact, and to minimise the build up of static electricity. It is obviously advantageous if a particular processing agent may be employed for the lubrication of a variety of types of artificial fibres. The invention provides a processing agent which may advantageously be used on a variety of fibres. Furthermore, processing agents according to the invention may have outstanding anti-static properties compared with conventional processing agents.

In its widest aspect a textile processing agent according to the invention incorporates a potassium'alkyl phosphate. Preferably the alkyl radical has, on average, from 6 to 10 carbon atoms. In the preferred form of processing agent, the potassium alkyl phosphate is dispersed in an inert, neutral, non-volatile, organic liquid, for example, a mineral oil or an ester, and the processing agent is preferably rendered homogeneous with a blending agent. The term processing agent used throughout this specification means compositions which are applied to fibres for the purpose of improving the ease with which they may be processed. Normally the compositions are liquidsand are preferably so when filamentary materials are treated. The compositions may also be solids, for example, waxes which are commonly applied to staple fibres where slower speeds are employed. The processing agents may be aqueous or non-aqueous. The non-aqueous form is preferred as this type of processing agent may combine I lubricating properties with anti-static properties. The nonaqueous processing agents may be applied as emulsions in water or in undiluted form. In another form, the processing agents may contain both water and a non-aqueous liquid or liquids and be rendered homogeneous by suitable compounds.

The potassium alkyl phosphate, should, as stated above, preferably contain, on average, from 6 to 10 carbon atoms in the alkyl radical although certain amounts of alkyl radicals outside this range may be present. The

preferred range of from 6 to 10 carbon atoms is determined by the properties desired in the product. With less than six carbon atoms in the alkyl radical the molecules are believed to migrate into the fibres and so decrease the effeclriveness of the processing agent, the lubricity is also decreased. With over ten carbon atoms the antistatic properties deteriorate and the compatibility with aqueous components of the processing agents decreases although lubricity is improved. For applications where one particular property is required in the process ing agent at the expense of other properties, potassium alkyl phosphates outside the preferred range may be quite suitable.

The phosphates may be prepared from mixtures of alcohols or from substantially pure alcohols. For reasons of economy, mixtures of alcohols are preferred, such, for example, as a mixture of aliphatic alcohols containing predominantly from 7 to 9 carbon atoms per molecule; a suitable product is sold by Imperial Chemical Industries Limited under the trade name of Alphanol 79. If a substantially pure alcohol is used, we have found that 2 ethyl hexanol, octanol and nonanol are satisfactory.

The preparation of the potassium alkyl phosphate may be performed, in preference, by reacting phosphorus pentoxide with the chosen alcohol or blend of alcohols in a solvent medium. Advantageously the solvent may be a component of the processing agent to be made. This, of course, avoids a purification step by removal of the solvent. Though not essential, it is preferred that the primary reaction between the phosphorus pentoxide and the alcohol should be performed with excess of the former to avoid the presence of any low molecular weight alcohol after reaction, subsequently the excess phosphorus pentoxide should be reacted with a higher alcohol (or some other fatty derivative containing a hydroxyl group, such as a glycerol fatty acid monoester or a glycol fatty ether or ester), an excess of which can be tolerated and may be desirable. The product is an alkyl phosphate ester which may be neutralised with a solution of potassium hydroxide. It is desirable that the potassium hydroxide solution used should be highly concentrated, having a concentration of at least 40 percent by weight. However, where the blended processing agent contains an appreciable quantity of water, a dilute potassium hydroxide solution may be used to neutralise the alkyl phosphate ester. In suitable circumstances, the potassium hydroxide may be added in solid form. It will be appreciated that the reaction between phosphorus pentoxide and an alcohol or alcohols leads to the production of a mixture containing, largely, monoand dialkyl acid phosphates. The term phosphate as used in this specification includes both monoand dialkyl phosphates and mixtures of these compounds.

As stated above, the potassium alkyl phosphate will normally be used dispersed in an inert, substantially neutral, non-volatile, organic liquid (hereinafter referred to as organic liquid) with the product rendered homogeneous with a blending agent. By the term inert as applied to the organic liquid it is meant that the liquid should not react to an appreciable extent with the potassium alkyl phosphate. The term should not, however, be construed as necessarily extending to other ingredients of the processing agent which may be added to the organic liquid during preparation of the product. By the term non-volatile we mean that the liquid should have a loW vapour pressure at ambient temperatures and should not boil at a temperature below about C., preferably the liquid boils at a much higher temperature.

Besides acting as a vehicle for the alkyl phosphate salt, the organic liquid usefully increases the anti frictional properties of the processing agent. The organic liquid may comprise a mixture of compounds, for example, a mineral oil or a single substance, such as a monoester, for example, butyl stearate, which should preferably contain more than 12 carbon atoms per molecule. Alternatively the oil may be a mixture of a mineral oil with a monoester. It may be desirable to compound the organic liquid from a mineral oil with the addition of lubricity additives, such as dioleyl citrate, pentaerythritol di-, tri-, or tetra-oleate, oxidised arachis oil, vegetable oils, for example palm kernel oil, and naturally occurring or syn- 3 thetic glycerides. The best lubricity additives are those which are capable of associating with metals.

As stated above, the processing agents containing liquids may be rendered homogeneous by the addition of a blending agent. Obviously this should preferably be done without requiring the use of excessive amounts (such as ,over 90 percent by weight in the lubricant) of the blending agent. It will be appreciated that the potassium alkyl phosphate is an antistatic agent, an agent which increases the conductivity of the processing agent and fibres to which it is applied, and the blending agent is present to enable the phosphate to form a homogeneous dispersion within the organic liquid so that the processing agent may be readily and uniformly applicable to textile fibres. The best blended processing agents have many desirable properties of which the following are important; they should reduce friction, they should impart a high electrical conductivity to fibres, and they should :be easily removable from textile materials. Processing agents are, of course, normally removed from the fibrous materials to which they are applied before thematerials are sold. Removal can conveniently be by scouring. Other desirable properties are that they should be colourless, non toxic,

stable and cheap and that they should not detrimentally affect the fibres to which they are applied.

We have found that the blending agents described in the specification of our copending United States patent application No. 399,399 are particularly useful as the blending agents in the processing agents of the present invention. The blending agent of the said copending application comprises a mixture of compounds having the (R O)P=O O(RO)n-H where the groups R are hydrocarbon radicals having, on average, between 6 and 18 carbon atoms, the groups R are and n is an integer of at least 1. 12 need not of course be the same integer throughout the mixture. Preferably the average value of n is between 1 and 2. Such blending agents may be prepared by reacting an alcohol, having an average of between 6 and 18 carbon atoms per molecule of alcohol, with phosphorus pentoxide and reacting the phosphates produced with at least one mole, per acid group of the phosphates, of an alkylene oxide containing from 2 to 4 carbon atoms.

Alternative blending agents are polyethylene glycol derivatives of alcohols which have between 8 and 18 carbon atoms per molecule of alcohol. These may be made by reaction between ethylene oxide and an alcohol or mixture of alcohols in the proportion of from 2 to moles of ethylene oxide to 1 mole of the alcohols. The alcohols should preferably have straight chain molecules and be liquids; they may be saturated or unsaturated. The product, that is the polyethylene glycol derivative of the alcohol, is preferably water soluble as blending agents which are water soluble or nearly so act as emulsifiers. Suitable blending agents of this type are prepared by reacting oleyl alcohol with 5 moles of ethylene oxide, or lauryl alcohol with 2 moles of ethylene oxide, or alcohols of intermediate chain length with intermediate amounts of ethylene oxide. These ratio of alcohol to ethylene oxide give the preferred balance of hydrophobic and hydrophilic properties.

The relative proportions of the ingredients of the textile processing agents may be varied widely. In processing agents having the potassium alkyl phosphate dispersed in an organic liquid with the addition of a blending agent, we prefer that in parts by weight of the formulated processing agent there should be between 5 and 25 parts of the potassium alkyl phosphate, between 5 and 25 parts of the blending agent and between 50 and 90 parts of organic liquid. However, the amount of the organic liquid used is particularly open to variation and there may be less than 50 parts of the liquid used although this is undesirable for economic reasons. The relative proportions of the ingredients will also vary, of course, with the properties of the specific ingredients in any particular mixture. Normally, however, it is expected that the same order of weights of potassium alkyl phosphate and blending agent will be employed in a particular processing agent blend.

It will be appreciated that in the processing agent of the present invention, it is the potassium alkyl phosphates which contribute most to increasing the electrical conductivity. There may, however, be other compounds added to the processing agent which help to increase the electrical conductivity or other desirable properties. Alkyl phenols, for example, octyl phenols, may usefully be incorporated in the processing agent.

We have found that the viscosity of the processing agents which are liquid having lubricating properties may advantageu-osly be between 70 and 300 Redwood seconds (1 mm. capillary diameter).

Processing agents according to the invention are illustrated by the following examples, in which parts and percentages are by weight:

EXAMPLE 1 An alkyl phosphate ester was made from the following ingredients:

The phosphorus pentoxide and the Alphanol were reacted together in the white oil and then the oleyl alcohol was added to be sure that there was no phosphorus pentoxide left unreacted.

30 parts of the alkyl phosphate prepared as above were mixed with 15 parts of coconut fatty alcohols di-propylene glycol phosphate (the blending agent) in 10 parts of white mineral oil of 65 seconds Redwood viscosity at 20 C, 5.6 parts of a 50 percent w./w. aqueous solution of potassium hydroxide, and 40 parts of n-butyl stearate. The blending agent was prepared as described in the specification of our said copending United States patent application number 399,399 by reacting 11 parts of phosphorus pentoxide and 52 parts of coconut fatty alcohols together in 56 parts of the mineral oil and then reacting 90 parts of the product with 16 parts of propylene oxide, the excess of which was removed by evaporation under nitrogen.

The processing agent had a viscosity of 121 Redwood seconds. On treating a matt nylon 6 filament yarn, when the agent was applied during spinning in the form of an aqueous emulsion, it was found that the treated fibres had a conductivity of 700 10- mhos/cm./ 1000 denier. The yarn used (40 denier, 10 filaments, 0.3 t.p.i.) had a yarn/metal coefficient of friction of 0.5-0.75 on a Bucket and Pollit testing machine when 1 percent w./w. of the processing agent was applied to the yarn-When the above yarn was heated to C. for 5 minutes there was only very slight discolouration.

With cellulose triacetate yarn (200 denier, 38 filament) when the processing agent was applied as 100 percent oil during spinning, the conductivity averaged over 850 mhos/cm./ 1000 denier and the friction coefiicient was 0.36 when 2 percent of processing agent was applied to the yarn.

EXAMPLE 2 An alkyl phosphate was prepared in the same manner as in Example 1 with the exception that Empilan KB2 replaced the oleyl alcohol. Empilan KB2 is the trade name of a product consisting largely of lauryl alcohol reacted with 2 moles of ethylene oxide and is sold by Marchan Products Ltd.

The processing agent was blended as follows:

Parts Alkyl phosphate as prepared above 30 Blending agent (oleyl di-propylene glycol phosphate) in White oil 10 Potassium hydroxide (50 percent aqueous solution) 5.4 Butyl stearate 40 The blending agent was prepared in a manner similar to that described in Example 1 by reacting 45 parts of commercial grade oleyl alcohol with 7 parts of phosphorus pentoxide in 43 parts of mineral oil and then reacting the phosphate produced with 15 parts of propylene oxide, the excess of which was removed by evaporation under nitrogen.

The processing agent was found to have good selfemulsifying properties and was similar in friction-reducing and antistatic properties to the processing agent prepared as in Example 1.

10 parts of which were used in the preparation of the blending agent.

As in the previous examples, the processing agent had excellent properties and was used successfully when spinning a variety of fibres.

EXAMPLE 4 30 parts of the alkyl phosphate ester prepared as described in Example 1 were mixed with 15 parts of an ethoxylated cetyl alcohol (made by reacting about 3.5 moles of ethylene oxide with 1 mole of alcohols, predominantly cetyl alcohol) about 5.5 parts of a 50 percent aqueous solution of potassium hydroxide (the pH of the product being adjusted to between 7.5 and 8.5), 15 parts of palm kernel oil and 35 parts of butyl stearate.

The blended processing agent had a viscosity of 152 Redwood seconds. It possessed good emulsification and lubrication properties and gave a conductivity of about 1000 10 mhos/cm./ 1000 denier on application to nylon 6 yarn as a 15 percent aqueous emulsion.

What we claim is:

1. A homogeneous textile processing agent compris ing from 5 to 25 percent by weight of a potassium alkyl phosphate in which the alkylradical has, on the average, from 6 to 10 carbon atoms per molecule; from 50 to percent by weight of an organic liquid selected from the group consisting of a mineral oil, a liquid monoester of an alkanol and a fatty acid containing at least 12 atoms per molecule, a vegetable oil and mixtures of at least two thereof; and from 5 to 25 percent by weight of a blending agent selected from the group consisting of (1) a substantially equimolecular mixture of compounds having the formulae:

( (R0)g-P=O O--(R-O)..H wherein the groups R are hydrocarbon radicals having, on the average, from 6 to 18 carbon atoms, the groups R are and n is an integer of at least 1; (2), a polyethylene glycol derivative of reaction between an alcohol having, on the average, from 8 to 18 carbon atoms per molecule and from 2 to 5 moles, per mol of alcohol, of ethylene oxide, and mixtures of (1) and (2).

2. A homogeneous textile processing agent according to claim 1 wherein the blending agent is the substantially equimolecular mixture of compounds and n is between 1 and 2.

3. A homogeneous textile processing agent according to claim 1 wherein the blending agent contains a polyethylene glycol derivative of reaction between ethylene oxide and an alcohol having straight chain molecules.

4. A homogeneous textile processing agent according to claim 3 wherein the alcohol is oleyl alcohol.

References Cited UNITED STATES PATENTS 1,914,331 6/1933 Nuesslein et a1. 2528.8 2,069,303 2/1937 Dreyfus et al 252-86 2,256,112 9/1941 Dickey 252-8.8 X 2,676,975 4/1954 Fortress et al. 252-8.6 2,803,565 8/1957 Sugar 252-83 X 2,842,462 7/1958 Haas et a1 2528.9X

LEON D. ROSDOL, Primary Examiner. SAMUEL H. BLECH, Examiner. J. T. FEDIGAN, Assistant Examiner.

Claims

1. A HOMOGENEOUS TEXTILE PROCESSING AGENT COMPRISING FROM 5 TO 25 PERCENT BY WEIGHT OF A POTASSIUM ALKYL PHOSPHATE IN WHICH THE ALKYL RADICAL HAS, ON THE AVERAGE, FROM 6 TO 10 CARBON ATOMS PER MOLECULE; FROM 50 TO 90 PERCENT BY WEIGHT OF AN ORGANIC LIQUID SELECTED FROM THE GROUP CONSISTING OF A MINERAL OIL, A LIQUID MONOESTER OF AN ALKANOL AND A FATTY ACID CONTAINING AT LEAST 12 ATOMS PER MOLECULE, A VEGETABLE OIL AND MIXTURE OF AT LEAST TWO THEREOF; AND FROM 5 TO 25 PERCENT BY WEIGHT OF A BLENDING AGENT SELECTED FROM THE GROUP CONSISTING OF (1) A SUBSTANTIALLY EQUIMOLECULAR MIXTURE OF COMPOUNDS HAVING THE FORMULAE: