US3723381A

US3723381A - Poly(vinyl acetate-dialkyl maleate acrylic acid) textile sizes

Info

Publication number: US3723381A
Application number: US00098915A
Authority: US
Inventors: J Fantl; C Williams; A Corey; D Donermeyer
Original assignee: Monsanto Co
Current assignee: Monsanto Co
Priority date: 1970-12-16
Filing date: 1970-12-16
Publication date: 1973-03-27
Anticipated expiration: 1990-03-27
Also published as: DE2162285A1; US3832321A; GB1335586A; US3716547A; US3817892A; US3854990A

Abstract

DISCLOSED HEREIN ARE POLY(VINYL ACETATE-DIALKYL MALEATEACRYLIC ACID) TEXTILE SIZES AND TEXTILES SIZED THEREWITH.

Description

United States Patent 3,723,381 POLY(VINYL ACETATE-DIALKYL MALEATE ACRYLIC ACID) TEXTILE SIZES Albert E. Corey, East Longmeadow, Donald D. Donermeyer and Joel Fantl, Springfield, and Charles R. Williams, Longmeadow, Mass., assignors to Monsanto Company, St. Louis, M0. N0 Drawing. Filed Dec. 16, 1970, Ser. No. 98,915 Int. Cl. C081? 45/30 US. Cl. 260-333 UA 6 Claims ABSTRACT OF THE DISCLOSURE Disclosed herein are poly(vinyl acetate-dialkyl maleateacrylic acid) textile sizes and textiles sized therewith.

BACKGROUND OF THE INVENTION (1) Field of the invention The present invention relates to textile sizes. More particularly, it relates to poly(vinyl acetate-dialkyl maleateacrylic acid) textile sizes wherein the dialkyl maleate is selected from the group consisting of dimethyl maleate and diethyl maleate and to textiles sized with these materials.

(2) The prior art Polymeric substances are well known in the prior art for use as textile sizes. In conventional loom operations yarn is sized with an aqueous solution of a water soluble material such as a copolymer of vinyl acetate and carboxylic acid, woven into cloth on a conventional loom with a mechanical shuttle and then the size is removed in a water bath. While these sizes have been adequate in the past, recent developments in the textile industry have created an increasing demand for textile sizes with improved tensile strength, elongation, toughness, solubility characteristics, etc.

One such development in recent years is the water jet loom. The water jet loom employs a jet of water in place of a mechanical shuttle in order to weave the yarn into a fabric. A water jet loom provides a faster weaving operation and less mechanical abrasion of the yarn. The result is an increase in production and improved quality in the woven fabric.

The size used in water jet weaving operations is customarily applied from aqueous solution. Once it is applied to the yarn and dried, the size must be sufliciently water resistant so as to remain on the yarn during the weaving operation. Moreover, in order to be efiicient and eifective, the size must retain its adhesion and film properties such as high tensile strength when wet by the water jets in the weaving process without becoming soft and slimy. Finally, the size must be soluble in mild aqueous alkali solutions or organic solvents so that it can be removed from the woven fabric. The foregoing properties are the result of a critical inter-relationship between chemical composition and molecular weight of the polymeric material which is used as the textile size.

The sizes of the prior art which are customarily used in conventional loom weaving operations are found to lack the necessary physical properties which arerequired for use with water jet looms.

Thus, there exists in the art a need for improved textile sizes which can be used to size yarns which are to be woven on conventional or Water jet looms and then removed using either an aqueous alkali solution or an organic solvent.

SUMMARY OF THE INVENTION The above-mentioned need in the prior art is fulfilled by the present invention which provides poly(vinyl acetatefor use as yarn warp sizes for use on conventional or water jet looms.

THE PREFERRED EMBODIMENTS The sizes of the present invention are prepared from latices obtained by interpolymerizing vinyl acetate, 21 dialkyl maleate selected from the group consisting of dimethyl maleate and diethyl maleate and acrylic acid. The polymerization charge comprises from 83 to by weight of vinyl acetate, from 2 to 10% by weight of dialkyl maleate and from 3 to 7% by weight of acrylic acid based on the total weight of the monomers. More preferably, the polymerization charge comprises from 87.5 to 91% by weight of vinyl acetate, from 5 to 7.5% by weight of dialkyl maleate and from 4 to 6% by weight of acrylic acid based on the total weight of the monomers.

The monomers are polymerized using latex polymerization methods at a temperature in the range of from 40 to 60 C. and preferably at a temperature in the range of from 40 to 45 C. At temperatures below about 40 C. the polymerization rate is too slow and the reaction mass tends to coagulate. At polymerization temperatures above 60 C. the product is of low molecular weight and lacks the tensile strength and elongation required in sizes for use on water jet looms.

The interpolymerization is carried out using a surfactant which comprises a phosphate ester of an alkyl phenolethylene oxide condensate wherein the alkyl group contains from 7 to 11 carbon atoms. Especially preferred are the phosphate esters of tertiary octyl phenol-ethylene oxide condensates (hereinafter referred to as PEOP-EO) and the phosphate esters of nonyl phenol-ethylene oxide condensates (:PENPEO). These preferred surfactants are available commercially as Triton XQS (Rohm & Haas Company) and GAFAC RE-870 (General Aniline & Film Company), respectively. The amount of the phosphate ester of an alkyl phenol-ethylene oxide condensate used will be in the range of from 1.0 to 4.0% by weight based on the total weight of the latex.

Preferably, the interpolymerization of the monomers is carried out using an anionic co-surfactant in combination with the phosphate esters of an alkyl phenol-ethylene oxide condensate. The use of the co-surfactants reduces the amount of coagulum in the resulting latex and provides a better product. The preferred co-surfactants used in the present invention include alkyl sulfonates such as sodium dodecyl; benzene sulfonate; fatty alcohol sulfates such as sodium lauryl sulfate; dialkyl sulfosuccinates, sodium dihexyl sulfosuccinate; etc.

The amount of cosurfactant used in the range of 0.1 to 0.3% by weight and more preferably 0.15 to 0.25% by weight based on the total weight of the latex.

The polymerization processes are initiated by a two component redox free radical initiator system. Suitable oxidizing components for the system are the inorganic peracid salts such as ammonium, potassium and sodium persulfates, perborates, and hydrogen peroxide. Preferred, however, are the oil soluble organic hydroperoxides such as t-butyl hydroperoxide, cuxnene hydroperoxide, p-menthane hydroperoxide, etc., and esters of the t-butyl perbenzoate type. The useful reducing components include compounds like the sulfites, bisulfites, hydrosulfites and thiosulfites; ethyl and other alkyl sulfites; the sulfoxylates,

such as sodium formaldehyde sulfoxylate; and the like.

4 Especially preferred are initiator systems based on t-butyl butyl hydroperoxide polymerization initiator is dissolved hydroperoxide and sodium formaldehyde sulfoxylate; and in the monomeric mixture and eight percent (8%) of the redox combinations such as mixtures of hydrogen permonomeric change (charge B) is then dispersed in the oxide and an iron salt, hydrogen peroxide and zinc formcharge A. The remainin 92% of the monomers (charge aldehyde sulfoxylate or other similar reducing agent; hy- B) is added to the reaction vessel by a conventional dedrogen peroxide and a titanous salt; potassium persulfate layed addition technique over a period of 2 /2 hours. Durand sodium bisulfate and a bromate mixed with a bisuling this time the temperature of the reaction batch is f maintained in the range of from 41 to 45 C. while main- The use of equimolar amounts of initiator system comtaining mild agitation. ponents is generally preferred although the amount of The resulting latex has a total solids of 35.7%, a pH of each component as well as the total amount of catalyst 4.9 and a Brookfield viscosity of 23 centipoises. The poly used depends on the type of component used as well as on (vinyl acetate-dimethyl maelate-acrylic acid) resin has a other polymerization conditions and may range between specific viscosity of 2.51 when measured as a 1% solution .02 and 0.2% by weight of the total polymerization sysin dimethyl sulfoxide at 25 C. Other properties of this tern, the preferred range being 0.02 to 0.06% for the latex are tabulated in Table I below.

oxidizing component and 0.04 to 0.1 for the reducing Examples 2 to 10 component.

The solids contents of the latices can be varied over a The following Examples 2 to 10 are set forth to illuswide range. The preferred latices having a solids content trate variations in the latex polymerization reaction conin the range of from 15 to 65% by weight and more pref- 2O ditions of the present invention. In each case the general erably from 35 to 55% by weight, based on the total procedures of Example 1 are followed except for the weight of the latex. noted changes. The resulting latices have solids contents During the polymerization reaction a conventional base in the range of from 35 to 42% by weight and Brookfield such as ammonium hydroxide or sodium hydroxide is used viscosities in the range of from 10 to 50 cps. at C.

to buffer the latex to a pH in the range of 4.0 to 6.0. 25 These examples are tabulated in the following Table I.

TABLE I [Summary of Examples 1 to 10] Example 1 2 3 4 5 6 7 8 9 10 Charge A: 57' 87 70 Charge B:

Total monomer 40.0 0 40.0 35 40 35 40 Percent vinyl acetate 90.5 80. 85 91 90.5 90.5 89.5 90.5 00.5 Percent dialkyl maleate 5.0 10.0 5 0 5.0 5.0 6.0 5.0 5.0 Percent acrylic acid 4. 5 3. 35 3 35 4. 5 4. 5 5.5 4. 5 4. 5 Percent; total coagulu 0.68 0.02 0 16 0.15 .18 0.07 0 04 Polymer proper t1cs Specific viscosity 2.51 1.38 1.64 2.85 2. 92 6.05 2.78 2.58 Tensile/percent elongation: Dry 05% RH..- 3,100/233 5,130/110 2, 350/380 2, 000/283 2,150/320 3,320/370 3,560/423 3, 040/330 Wet 1,770 442 2, 030/310 1, 530/430 2, 310/541 720/500 2,000/574 1,440/470 Dry 80% R.H 2, 340/370 The following examples are set forth in illustration of In the foregoing Table I, percent total coagulum refers the present invention and should not be construed as a to all coagulum produced, both filterable and remaining limitation thereof. Unless otherwise indicated, all parts as fouling on the impeller and walls of the reactor. This and percentages given are by weight and polymerization value is measured by recovering the coagulum by filtratemperatures are maintained in the range of from 41 to tion and by scraping from the equipment, drying it, weigh- 45 C ing it, and calculating its percent weight based on the cal- PART A PREPARATION OF LATICES culated SOlldS. Values in excess of 0.75 indicate that ob ectionable kettle fouling would occur in commercial Example 1 scale batches which would cause serious problems in prod A latex is prepared in conventional latex polymerizauct i l F F handlmg and equlpment clean'up' tion equipment while maintaining a nitrogen atomsphere f "scoslty meilsuremellts are made on 1% 50111 and mild agitation using the following charge: tlons 1n d1methl 1 sulfoxlde at Tensile (p.s.1.) and elongation are measured accord- Charge- Parts ing to ASTM Method D-88267 after conditioning at (A); and 80% relative humidity. The wet values are obtained on 4 mil films which are immersed in water for five Water 62.03 (5 t PEOPEO 1.58 th 1 1 t th 1k 1 I t Ammonium hydroxide 0.20 xamp e uses 1e y ma ea c as e 1a y ma ea c 65 component while all of the other examples use dimethyl Sodlum formaldehyde sulfoxylate maleate. Examples 1, 4, 5 and 7 to 9 use a phosphate ester (B): of an octyl phenol-ethylene oxide condensate (PEOPEO) while the other examples use a phosphate ester of a nonyl g i gg a ggfiz g g if phenol-ethylene oxide condensate (PENPEO). Example Vinyl acetate (VOAC) 3167 70 1 uses a single surfactant while Examples 2 to 10 use a Acrylic acid L58 combination of a major amount of PEOPEO or PENPEO with a minor amount of sodium dihexyl sulfosuccinate The PEOPEO surfactant, ammonium hydroxide buffer (SD,S) which is available commercially as Aerosol M.A. solution, sodium formaldehyde sulfoxylate and the Water from American Cyanamid. Note in Examples 2 to 10 that are charged to a glass lined reaction vessel. The tertiary 7 when. a combination of surfactants is used, the percent total coagulum is significantly lower than in Example 1 wherein a single surfactant is used.

Examples 1 to 4 and 7 to 10 are prepared using ammonium hydroxide as the butter agent while Examples 5 and 6 use sodium hydroxide. The high wet tensile strength of the polymers prepared in Examples 1 to 5 and 7 to 10 using ammonium hydroxide, indicate their suitability for use as a size in a water jet Weaving process.

The polymeric products of Examples 2 and 3 contain only 3.35% acrylic acid monomer. These polymers have good water resistance, tensile and elongation making these polymers very suitable for use in water jet weaving processes using organic solvent desizing methods.

In order to be suitable for use as sizes in the water jet weaving process the polymeric size must have a good tensile strength, toughness and adhesion to the yanr under Wet conditions. The specific viscosities of the polymers of the present invention are good indices as to wet tensile strength and toughness when considered in the context of the type and amount of comonomers present in the polymer. The preferred polymers of the present invention have a specific viscosity in the range of from 1.2 to 12.0 and more preferably in the range of from 1.3 to 10.0.

r The correlation between specific viscosity of the polymers of the present invention and wet tensile strength are shown in the following Table II wherein five series of polymers are prepared using the general procedures of Examples 2 to 10 above. Variations in the amount of catalyst and polymerization temperatures lead to variations in the specific viscosity of the resulting polymers. These polymers are then tested for wet tensile strength and the results are tabulated in the following Table II.

1 Polymers are prepared using the following percent by weight monomeric charges: A=vinyl acetate/dimethyl maleate/acrylic acid 91.65/5.0/ 3.35; B=vinyl acetate/dimethyl maleate/acrylic acid 90. 5/5/4.5; C= vinyl acetate/dimethyl maleate/acrylic acid 90/5/5; D =vmyl acetate] diethyl maleate/acrylic acid 90.5/5/5A; E =vinyl acetate/dibutyl maleate/ acrylic acid 91.65/5/3.35.

2 Tensile values for 0-1 and (3-2 are determined at 80% RH.

The data in the foregoing Table II illustrate that in a given series, using the prescribed dimethyl maleate and diethyl maleate monomers of the present invention, the greater the specific viscosity the greater is the wet tensile strength. On the other hand, Series E prepared using dibutyl maleate has very low wet tensile strength as compared to comparable polymers having approximately the same specific viscosity. In this regard attention is directed to a comparison between Series E and Series A-3, A-4, B-1 and B-2.

Examples 11 to 13 The following Examples 11 to 13 are set forth as control examples to illustrate the effect of polymerization temperature on the physical properties of the resulting latex. In each example the general charge and procedure of Example -1 0 is repeated while the polymerization temperature is varied. The specific viscosity of the resulting polymer is then measured. The results are tabulated in Table III below.

TABLE III [Summary of Examples 11 to 13] Polymerization Specific Example Temp, C. viscosity 1 Run coagulated.

The data in the foregoing Table III indicates that, with the framework of the present invention polymerization temperatures below 40 C. lead to coagulation while increasing temperatures a'bove 45 ,C. lead to polymers with decreasing specific viscosities. However, for any given polymer system within the framework of the present invention, optimum specific viscosity is obtained when the polymerization reaction is in the range of from 40 to 60 C. and more preferably from 40 to 50 C.

The following Examples 14 to 19 are set forth to further illustrate the criticalities of the present invention.

Example 14 The general charge and procedure of Example 3 is repeated here except that fumaric acid is substituted for the acrylic acid used in Example 3. The reactants are mixed and heated. N0 significant polymerization reaction has taken place even after 24 hours.

Example 15 In this example 88% by weight of vinyl acetate, 5% by weight of dimethyl maleate and 7% by weight of monomethyl maleate are interpolymerized according to the general procedure of Example 10.

The monomethyl maleate monomer is being used in place of the acrylic acid used in Example 10. The resulting polymer is found to have a specific viscosity of 1.8, tensile strength of 1880 p.s.i. dry and 1060 p.s.i. wet and elongation of 200% dry and 500% wet. The low wet tensile of this polymer coupled with poor wet adhesion to acetate fibers and film insolubility in aqueous alkali, makes it unacceptable for use as a size in a water jet weaving process.

Example 17 In this example dibutyl maleate is used in place of the dimethyl maleate and diethyl maleate used in Examples 1 to 10 above. The general polymerization procedures used in Example 1 are followed here using 91.65% by weight of vinyl acetate, 5.0% by weight of dibutyl maleate and 3.35% by weight of acrylic acid. The resulting polymer has a specific viscosity of 1.79, tensile strength of 2050 p.s.i. dry and 680 p.s.i. wet and elongation of 230% dry and 240% wet. The low wet tensile strength of this polymer makes it unacceptable for use as a size in a water jet weaving process.

Example 18 In this example methyl methacrylate is used in place of the dimethyl maleate used in Examples 1 to 8 and 10 above. The general polymerization methods of Example 7 4 are used here using a monomer charge of 89% by weight of vinyl acetate, 5% by weight of methyl methacrylate and 6% by weight of acrylic acid. The reaction mixture coagulated and no polymer was obtained for testing.

Example 19 In this example acrylonitrile is used in place of the dimethyl maleate used in Examples 1 to 8 and 10 above. The general polymerization methods of Example 4 are followed using a monomer charge of 90% by weight of vinyl acetate, 5% by weight of acrylic acid.

After four hours reaction time only 6.5% of the monomers have been converted into polymer.

Example 20 This example illustrates the criticality of using a surfactant which is a phosphate ester of an alkyl phenolethylene oxide condensate. Example 4 is repeated here except that octyl phenol-ethylene oxide condensate is used as the surfactant in place of the phosphate ester of octyl phenol-ethylene oxide condensate used in Example 4. The octyl phenol-ethylene oxide condensate used in this example is a well-known surfactant which is available commercially as Triton X-405 from Rohm and Haas. After three hours reaciton time the batch was completely coagulated.

Example 21 Example 20 is repeated here except using a surfactant which is a phosphate ester of an aliphatic alcohol-ethylene oxide condensate. After three hours reaction time the batch was completely coagulated.

PART B.TESTING OF THE LATICES OF EX- AMPLES 1 TO 5 AND 7 TO 10 AS TEXTILE SIZES The latices prepared in Examples 1 to 10 are tested in order to determine their suitability as yarn sizes in both conventional and water jet weaving processes. The sizes are prepared by dissolving the latex in a basic solution such as ammonium hydroxide or sodium hydroxide solution. Other basic solutions may be used to dissolve the latices as for example, solutions of alkali and alkaline earth metal hydroxides as well as aqueous solutions of methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, n-propyl amine, n-butyl amine, morpholine, etc.

The key properties considered in these tests are listed below:

Solubility.All of the latices in question are soluble in aqueous bases such as aqueous ammonium hyroxide to provide sizing solutions.

Sizing solutions.-Prepared from the latices of Examples 1 to 5 and 7 to 10 have Brookfield viscosities in the range of from 1 to 300 centipoises at 4 to 5% solids allowing ease of application to the yarn.

Wet tensile strength.Films prepared from the latices of the present invention have wet tensile strength in excess of 1000 p.s.i. and the necessary toughness and film integrity required in water jet sizes.

Percent elongation-These values further indicates that the latices in question have the necessary film toughness required in water jet sizes.

Adhesion.The latices of Examples 1 to 5 and 7 to 10 have been tested and found to have good adhesion to the following yarns-filaments, acetate, polyester, rayon, texturized polyester, nylon; spun polyester, cotton, rayon and wool; acetate, nylon and blends thereof.

Resolubility in mild alkali.Dried films of the latices in question are readily soluble in tetrasodium pyrophosphate-surfactant solutions which indicates that the size is easily removed from the woven fabric. The size is also soluble in chlorinated solvents used in desizing operations.

Size efiiciency.Is a measure of the amount of size add-on required in a given operation. The add-on is the amount of size that must be applied to the yarn in order to permit it to be woven on a water jet loom. In general, the less size add-on required, the more efficient the size. Sizes prepared from the latices of the present invention have excellent efficiency as is indicated by the following Examples 22 to 24.

Example 22 A latex composition is prepared as in Example 10 above using monomeric charge of 90.5% by weight of vinyl acetate, 5% by weight of dimethyl maleate and 4.5% by weight of acrylic acid. The resulting latex, wherein the polymer component has a specific viscosity of 2.7, is dissolved in aqueous ammonium hydroxide to give a 5.0% solids solution having a pH of 9.0.

This sizing solution at F. is applied to a denier, 41 monofilament, low twist bright acetate yarn on a commercial eleven can slasher at a rate of 90 yards per minute for a size add-on of 2.1%. Drying can temperatures on the slasher are /200/200/215/220/220/230/ 220/2l0/80/l30 F. respectively. The split is very easy, and no ends break out at start-up.

The sized warp is entered into a Nissan Prince water jet loom, where at 400 picks per minute the weaving operation runs at very high efficiency, 98%) with no second quality fabric produced. The woven fabric has a dry appearance in contrast to warps woven with lower M.W. (specific viscosity of 0.7) materials which become wet and slimy. Successive warps shows the same excelent performance. This fabric was desized in a conventional process by scouring in tetrasodium pyrophosphate wetting agent baths. The size is also removable in a chlorinated solvent scouring process.

Example 23 Example 22 is repeated here using a latex with a specific viscosity of 2.73. This latex is dissolved with aqueous ammonium hydroxide to give a 4.5% solids solution having a pH of 9.2. The size is applied to a 75 denier 20 monofilament low twist (75/20/LT) bright acetate yarn on a seven can slasher. The slasher is run at 25 yards per minute at a size add-on of 1.9% using drying can temperatures of 150/ 170/ 210/ 160/ 15 0/ cold, respectively. The warp splits very easily and weaves at very high etficiency to give good quality fabric which is desized as in Example 22.

Example 24 This example is set forth to illustrate the exceptional efficiency of the sizes prepared according to the processes of the present invention. Example 22 is repeated here using a latex with a specific viscosity of 2.73. This latex is dissolved with aqueous ammonium hydroxide to give a 4.5% solids solution having a pH of 9.2. The size is applied to a 150 denier, 40 monofilament, 0.8 twist (150/40/0.8) bright acetate yarn on a seven can slasher at 55 yards per minute at a size add-on of 1.6%. Drying can temperatures are 190/210/210/210/190/cool. The warp splits very easy, and no ends break out during the sizing operation. The warp weaves at very high efliciency to give good quality fabric which is desired as in Example 22. The add-on rate (1.6%) used in this example is unsually low when compared to the sizes of the prior art which must be used in much larger amounts.

Sizes which are obtained from polymers prepared by the processes of the present invention are compared to commercially available textile sizes. The results of these comparisons is set forth below. In these tests the toughness value is the product of tensile times elongation.

Various sizes in the form of ammonium salts are ap plied to acetate and polyester filaments under water jet conditions. The size is tested for wet tensile, wet elongation, wet toughness and wet adhesion. The results are tabulated in the following Table IV.

application the size remains on the resulting fabric as a loom finish. Sizes used in this application must be very TABLE IV [Tests on Water jet size on acetate and polyester filament] Adhesion I Specific Tensile Percent Toughness Size Composition 1 viscosity (p.s.i.) elongation (X10 Acetate Polyester A VA/DMM/AA 90.5/5/4.5 2 36 2,150 540 116 Excellent Good.

VA/DBM/AA 91.65/5/3.35 1 79 700 250 17. 5 P

A CA 96/4 0. 7 750 200 VA/MMM 93/7 1.4 700 400 28 VA/MIBM 79/21 1. 9 60 540 3. 2 VA/MA 47/53 0 0 AA/AE 480 200 9. 6

Values are in weight percent. VA=vinyi acetate; DMM=dirnethyl maleate; DBM =dibutyl maleate; MMM=monomethyl maleate; MIBM=monoisobutyl maieate; AA=acrylic acid; CA=crotonic acid; MA=maleic anhydrlde; AE=acryllc ester.

1 Qualitative adhesion tests are run under wet conditions on fiber imbedded into size.

Size A is obtained from a latex that is prepared according to the processes of the present invention. Sizes C to G are commercially available sizes which are representative of the prior art. Note that Size A has good to excellent adhesion and is at least five times (5 X) tougher than the sizes of the prior art.

CONVENTIONAL SIZE ON ACETATE, RAYON AND TEXTURIZED POLYESTER Various sizes in the form of sodium salts are applied to filament acetate, rayon filament and texturized polyester. The sizes are then tested under conditions of 65% RH. for tensile, elongation, toughness and adhesion. The results are tabulated in the following Table V.

TABLE V [Conventional size on acetate, rayon and texturized polyester] Percent Adhesion 9 Tensile elonga- Tough- (p.s.i.) tion ness Acetate Rayon Polyester 3, 060 370 1, 580 300 12 2, 000 200 18 2, 250 160 14 1, 400 400 16 500 500 30 5, 300 60 26 High 1,800 30 5 9 d0.

1 Compositions A to F are the same as in Table IV above except that A has a specific viscosity of 2.94; G is a commercial gelatin size; H is an equimolar styrene-maleic anhydn'de copolymer.

3 Numerical values are pounds required to break %X% lnch lapjoints.

Size A, which is obtained from a latex prepared according to the processes of the present invention, exhibits greater toughness and better adhesion than the sizes of the prior art.

LOOM FINISH ACETATE AND NYLON SIZES Various sizes in the form of ammonium salts are applied to acetate and nylon filament yarns. In the acetate resistant to water spotting. The sizes are then tested under conditions of RH. for tensile, elongation, toughness and adhesion. The results are tabulated in the follow- 1 Compositions A to E same as in Table IV above except thnt A has a specific viscosity oi 2.66. The polyvinyl alcohol used is a partially hydrolyzed low molecular weight polymer which cannot be used as a loom finish because of its water sensitivity.

2 Tested as in Table V.

Once again, Size A, which is representative of the sizes of the present invention, shows superior toughness. The adhesion of this size to acetate and nylon further indicate its utility as a textile size.

SPUN SIZES FOR AQUEOUS REMOVABLE AND SOLVENT REMOVABLE APPLICATIONS In certain applications it is desirable to size yarns such as cotton, rayon, wool, polyester and blends thereof and then remove the size from the resulting fabric using either aqueous alkali or an organic solvent. In the following tests various sizes are applied to polyester and then tested under conditions of RH. for tensile, elongation, toughness, adhesion and solubility. The test results are tabulated in the following Table VII.

TABLE VII [Spun sizes for aqueous removable and solvent removable applications] Solubility 3 Tensile Percent Toughness Adhesion Size (p.s.i.) elongation (X10 (p.s.i.) Aqueous Organic A 3,500 360 126 180 Yes Yes B 1,000 400 40 Yes Yes C 1,600 200 30 es Yes. D 2,000 200 40 80 Yes N0. E 660 620 40 100 Yes N0 PVOH-PH--- 4,800 420 190 Yes No PVOH-FH-.. 6.600 320 210 40 Yes No OMC/binder 2,800 60 17 70 Yes No Starch/binder..-" 2,700 30 8 60 Yes No esion tests are run on a 5 5 square inch polyester to wood board bond.

I The aqueous solution contains a tetrasodiurn pyrophosphate-wetting agent combination. The organic solvent used is trichloroethylene.

Size A which is representative of the sizes of the present invention exhibits excellent toughness and adhesion. Moreover, this material is removable in conventional aqueous desizing operations as well as in organic solvent desizing operations. This latter feature is especially important where water shortages or water pollution problems exist.

Another feature of the present invention is the fact that the polymeric material may be dissolved in organic solvents to form a size. This feature is especially desirable in certain applications wherein solvent size removal techniques are also employed. In such applications the polymer solids are recovered from the latex, using conventional means. The polymer solids are then dissolved in an organic solvent to form the textile size and the size in the form of an organic solvent solution is applied. Size removal may be accomplished using aqueous alkali or organic solvent methods.

Preferred organic solvents used in preparing the sizes are alcohols, ketones, esters and aromatic solvents. Especially preferred are chlorinated aliphatic hydrocarbons such as methylene chloride, methylene bromide, chloroform, bromoform, ethylene dichloride, ethylene dibromide, ethylidene chloride, ethylidene bromide, s-tetrachloroethane, hexachloroethane, s dichloroethylene, 1, 1,1 trichloroethane, 1,1,2 trichloroethane, trichloroethylene, trimethylene bromide, trichlorobromoethane, trichloromethane, 1,2,3 trichloropropane, 1,1,2 trichloropropane, trifluoro 1,2 tribromoethane, trifiuoro- 1,1,2-tribromoethane, trifluoro 1,1,2 trichloroethane, 2,2 dichloro 1 bromoethane, 1,3-dichloro 2 methyl propane, 1,2 dichloro 2 methyl propane, 1,1- diiodoethane and the like. Chlorinated aliphatic liquid hydrocarbons are preferred in the practice of this invention because of their generally lower cost, greater availability and the ease with which these solvents may be handled.

From the foregoing, it should be obvious that many variations are possible in the present invention without departing from the spirit and scope thereof.

What is claimed is:

1. A composition for sizing textile yarns comprising a solution of a latex interpolymer of from 83 to by weight of vinyl acetate, from 2 to 10% by weight of a dialkyl maleate selected from the group consisting of dimethyl maleate and diethyl maleate and from 3 to 7% by weight of acrylic acid based on the total weight of the monomers in a chlorinated aliphatic hydrocarbon solvent.

2. A composition as in claim 1 wherein the amount of vinyl acetate is in the range of from 87.5 to 91%, the amount of dialkyl maleate is in the range of from 5 to 7.5% By weight and the amount of acrylic acid is in the range of from 4 to 5% by weight.

3. -A composition as in claim 1 wherein the dialkyl maleate is dimethyl maleate.

4. A composition as in claim 1 wherein the interpolymer has a specific viscosity when measured as a 1% solution in dimethylsulfoxide at 25 C. in the range of from 1.2 to 12.

5. A composition as in claim 1 wherein the interpolymer has a specific viscosity in the range of from 1.2 to 12 when measured as a 1% solution in dimethylsulfoxide at 25 C., and the sizing solution has a Broo'kfield viscosity in the range from 1 to 300 cps.

6. A composition as in claim 5 wherein the organic solvent is selected from the group consisting of methylene chloride, chloroform, ethylene dichloride, 1,1,1-trichloroethane, and 1,1,2-trichloroethane.

References Cited UNITED STATES PATENTS 2,686,137 8/1954 Rossin et al 1l7138.8 R 2,853,471 9/1958 Beadell 260-296 MP 3,231,534 1/1966 Blades et a1. 26029.6 TA 3,449,282 6/ 1969 Lasher et al. 26029.6 TA

WILLIAM H. SHORT, Primary Examiner L. M. PHYNES, Assistant Examiner US. Cl. X.R.

117-13833 R, 139.5 A, 161 UZ, UT, C; 26029.6 TA, 78.5 B, UA, E