US3823056A

US3823056A - Antistatic floor covering and textile structure

Info

Publication number: US3823056A
Application number: US00323807A
Authority: US
Inventors: W Cooney
Original assignee: GAF Corp
Current assignee: ISP Investments LLC
Priority date: 1973-01-15
Filing date: 1973-01-15
Publication date: 1974-07-09
Anticipated expiration: 1991-07-09
Also published as: BE809748A; JPS5047422A; FR2324790A1; FR2324790B1; DE2401221A1

Abstract

ANTISTATIC FLOOR COVERING AND TEXTILE PRODUCTS OF ENHANCED DURABILITY TO CLEANING AND REDUCED MIGRATION TENDDENCY ARE PRODUCED BY APPLYING BETWEEN TWO POLYMERIC

COVERING LAYERS DISPOSED BENEATH THE TEXTILE OR FLOOR COVERING WEAR LAYER AN ANTISTATIC COMPOSITION CONSISTING ESSENTIALLY OF A MIXTURE OF (A) AN ORGANIC ANTISTATIC AGENT, (B) A HUMECTANT WHICH MAY BE EITHER A NONIONIC HUMECTANT, SUCH AS GLYCERIN, OR AN IONIC HUMECTANT SUCH AS CALCIUM CHLORIDE, AND (C) WHEN SAD HUMECTANT IS NONIONIC HUMECTANT, AN ELECTROLYTE SUCH AS CALCIUM CHLORIDE OR SODIUM CHLORIDE AND APPLYING A POLYMERIC BACKING COATING OR SODIUM CHLORIDE STATIC LAYER, WHEREBY THE ANTISTATIC LAYER IS DISPOSED BETWEEN THE TWO POLYMERIC COVERING LAYERS.

Description

3 1974 w. .J. COONEY 3,823,056

ANTISTATIC FLOOR COVERING AND TEXTILE STRUCTURE Filed Jan. 15, 1973 4 FIBROUS FILE 2 m Wm/mummmuuwmwm Z ZZ'ZQZI XQ 6 ANTISTATIO L Y R IO SECONDARY BACKING A E 8 POLYMERIC LAYER (OPTIONAL) BACKING LAYER United States Patent O 3,823,056 ANTISTATIC FLOOR COVERING AND TEXTILE STRUCTURE William J. Cooney, Hixson, Tenn., assignor to GAF Corporation, New York, NY. Filed Jan. 15, 1973, Ser. No. 323,807 Int. Cl. B32b 3/16 US. Cl. 161-67 17 Claims ABSTRACT OF THE DISCLOSURE Antistatic floor covering and textile products of enhanced durability to cleaning and reduced migration tendency are produced by applying between two polymeric covering layers disposed beneath the textile or floor covering wear layer an antistatic composition consisting essentially of a mixture of (a) an organic antistatic agent,

(b) a humectant which may be either a nonionic humectant, such as glycerin, or an ionic humectant such as calcium chloride, and

(c) when said humectant is a nonionic humectant, an electrolyte such as calcium chloride or sodium chloride and applying a polymeric backing coating over the antistatic layer, whereby the antistatic layer is disposed between the two polymeric covering layers.

BACKGROUND OF THE INVENTION This invention is directed to antistatic textile products and floor coverings of textile and non-textile compositions. Most specifically the invention relates to an antistatic carpet structure which has a fibrous layer, a primary backing thereunder, a latex pre-coat layer thereover, an antistatic-conductive coating, and a polymeric backing.

Conventional floor coverings, especially carpet structures, are capable of generating and transferring substantial charges of static electricity. These charges of static electricity are created when persons in contact with the dielectric wear layer, such as the fibrous layer of the carpet move over said fibrous layer. The charge per se is created by the movement of dielectric shoe components which are in contact with the dielectric wear layer. These charges are then transferred to the wearer of the shoe. When the wearer subsequently becomes grounded, the accumulated charge discharges through that part of the individuals body which is in contact with the ground. This discharge procedure can result in severe discomfort to the individual. The above described problem can be eliminated if the charges of static electricity can be dispersed throughout the floor covering structure, and subsequently dissipated into the surrounding environment.

The prior art discloses antistatic compositions and carpet structures. For example, US. Pat. 2,302,003, Cadwell et al., teaches that accumulated charges may be dispersed via a plurality of conducting fibers which are positioned throughout the fibrous layer.

US. Pat. 3,510,386, Goins et a1, teaches a carpet structure that must have an antistatic layer disposed directly beneath the wear layer, in that case, the fibrous pile primary backing. The patent teaches that it is mandatory that the antistatic layer be disposed directly beneath the primary backing so that the antistatic composition is operative to coat and contact the ends of the fibers, forming the pile in contact therewith. The patent teaches that "ice the antistatic composition must substantially penetrate the backing and part of the pile fibers in order to be effective."

This presents problems in application, types of textile structures to which the antistatic composition may be applied and in its efiective life span. An ancillary problem is also the fire hazard attendant to the flammability of the carpet structure due to migration of the antistatic composition up through the textile structure thus causing a stiffening of the pile with resultant stand-up to the flame; and the fact that said migration causes a loss in the effectiveness and durability of the product when such a treated carpet is washed.

In contrast thereto, the floor covering and textile struc ture of this invention disperses quickly and thoroughly, charges of static electricity without the need of specific conducting fibers. The structure of this invention bleeds off charges of static electricity.

The antistatic composition of this invention is incorporated between two polymeric backings in contrast to the vast majority of the prior art antistatic compositions which are not compatible nor effective for such a sandwiching and isolation between polymeric backings. Because of this incompatibility, carpets specifically, which are treated with these prior art antistatic compositions could not utilize most polymeric backings, and particularly the commonly used natural latex backing. In contrast, the antistatic coating of this composition as utilized herein is compatible with natural latex backings, adhesives and most other polymeric coating compounds.

The following description is directed to the most preferred embodiment of the instant invention, viz, carpet structure, however, it is to be understood that the term floor covering as used herein is intended to include linoleum petroleum product floorings, vinyl and asbestos sheet and tile floor covering, polyurethane and polyolefin floorings and the like and the invention is directed thereto as well.

SUMMARY OF THE INVENTION It is an object of this invention to provide for an antistatic textile and floor covering product of enhanced durability to cleaning and having a low degree of migration tendency of the antistatic composition.

It is another object of the invention to provide for an antistatic flooring product having an antistatic composition interspersed between two polymeric layers, which in turn are disposed beneath the Wear layer of said flooring product.

It is yet another object of the invention to provide for an antistatic carpet structure.

Other objects and advantages will become more apparent as the description proceeds.

Broadly speaking, the invention includes the provision of an antistatic textile and floor covering product comprising (1) a Wear layer, such as a fibrous textile layer,

(2) a latex pre-coat layer disposed beneath said wear layer,

(3) an antistatic coating composition layer disposed beneath said pre-coat layer, said antistatic layer consisting essentially of a mixture of (a) an organic antistatic agent, (b) a humectant selected from the group of ionic and monionic humectants, and

(c) when such humectant is a nonionic humectant, an

electrolyte, and

(4) a polymeric backing layer covering said antistatic layer, said antistatic layer in turn, being disposed between said pre-coat layer and said polymeric backing layer.

DETAILED DESCRIPTION The subject antistatic floor covering and textile structure is illustrated as a carpet in the single figure of the accompanying drawing. The structure, of the floor covering, such as a carpet 2 has a conventional wear layer, such as a fibrous layer 4 which can be woven, tufted, knitted, flocked or other structure usual in carpets. This fibrous layer can be composed of any of the usual textile fibers or blends or mixtures thereof employed in carpet manufacture, such as wool, polyamides (e.g. nylon 66 and nylon 6), cotton, polyolefins (particularly polypropylene), acrylics, modacrylics, polyesters, etc. The fibrous layer 4 is woven in, tufted through, or in some other manner affixed to a backing layer 5, usually a woven fabric of cotton or jute, although other fibers and types of construction can be employed for the backing thereof. The basic carpet structure may be any carpet manufacture, such as the well known tufted, Brussels, Wilton, Axminster, chenille, velvet, flocked, knit etc. In accordance with the present invention the underside of the fibrous or pile layer 4 with its primary backing to which the fiber forming pile is afirxed or through which it is tufted, etc. is coated with a pre-coat latex layer 3, comprised of any of the conventional latices, this layer 3 is then coated with an antistatic coating 6 which provides a uniform continuous layer thereover. The antistatic coating 6 is effective without being in contact with the backing and the ends of the fibers forming the pile. The amount of material applied as such antistatic coating should be sufficient to substantially over the pre-coat layer 3. Normally from .01 to 20 ounces per square yard and preferably from 2.0 to 10.0 ounces per square yard of the antistatic coating is applied.

The antistatic coating composition employed for the antistatic coating layer 6 ideally comprises a mixture of a textile antistatic agent and to 50 parts by weight of humectant. There may also be employed from 0.1 to about 1 part by weight of a nonionic or cationic type wetting agent to assist the dispersing of the antistatic composition. It is also preferable to incorporate in the coating composition from about 0.1 to about 1 part by weight of an electrolyte particularly if the humectant employed is nonionic in character or is only weakly ionic, i.e. has a relatively low dissociation constant. The antistatic coating 6 is preferably applied in the form of an aqueous solution or dispersion, although other solvents or liquid dispersing mediums may be employed if desired and in the case of aqueous solutions or dispersions, volatile water-soluble solvents, such as lower aliphatic alcohols of 1 to 4 carbon atoms, acetone and the like, may be included to facilitate drying of the antistatic layer following its application.

Examples of satisfactory pre-coat latex layers 3 which may be applied to the underside of the primary backing 5 include filled or unfilled coatings of acrylic latexes, vinyl acetate latexes, styrene-butadiene latexes (preferably carboxylated), natural latex, vinyl chloride and vinylidene chloride interpolymers and the like with plasticizing monomers, such as butyl acrylate and including ethylenevinyl chloride copolymers and the like. Satisfactory adhesive coats include all of the above, but in general styrene-butadiene latexes are preferred.

After the antistatic coating 6 has been applied to the pre-coat layer 3, a polymeric backing layer 8 is then applied to the carpet and forms an essential element of the carpet structure of this application. This polymeric backing layer is preferably applied in the form of an aqueous dispersion (latex) and is preferably a known compound natural rubber latex or compounded carboxylated butadiene-styrene rubber-latex, commonly employed as latex backing for carpetings, although other polymeric coatings, such as polystyrene, vinylidene chloride, polyacrylates, butadiene-styrene rubbers and the like may be employed both herein and as the pre-coat layer 3. As examples of known natural compounded rubber latices which are commercially available may be mentioned: Lotol GX-3180, U.S. Rubber Company, compounded carboxylated styrene-butadiene rubber latices such as Lotol GX-1076, U.S. Rubber Company.

While the exact reasons for the antistatic properties of the carpet structure of the present invention are not fully understood, it appears that the two polymeric coatings 3 and 8 serve the function of holding the antistatic coating layer 6 in place yet without interferring with electric charge dissipation. Charges of static electricity built up in the pile 4 are dispersed throughout the entire carpet area by antistatic layer 6 and subsequently bled off into the ground or atmosphere. In order to assist bleeding such charges to the ground, the polymeric coating 3 and 8 may have incorporated therein a material such as as carbon black or any agent which will lower the dielectric properties of the polymeric layers.

A number of preferred compositions for the antistatic coating layer 6 of the carpet structure of the present invention are disclosed in US. Pat. 3,519,561 of Andrew J. Kelly and Robert C. Britt entitled Antistatic Composition and Process. Particularly preferred are those antistatic compositions disclosed in said patent in which potassium formate is employed as humectant since it has been found that not only is potassium formate particularly effective as a humectant in such coating compositions, but compositions containing the same are compatible with the latex backing and specifically overcomes premature coagulation or gelling of latex backing based on natural compounded rubber, thus not interfering with good bonding of the latex coated with the carpet backing. On the other hand, the antistatic coatings containing calcium chloride are incompatible with certain known latex coatings which have been used as carpet bac kings in that they cause premature coagulation or gelling of the latex with resultant poor adhesion of the latex to the carpet backing so that in the case of loosely woven or tufted carpets the latex does not function satisfactorily to hold the tufts in place.

While antistatic layers based on the antistatic compositions of the above mentioned patent are particularly preferred, it will be understood that one may employ any antistatic layer based on any known antistatic material suitable for textiles which will disperse charges of static electricity. Such agents are normally nitrogen containing or carboxylic containing organic antistatic agents and as examples thereof may be mentioned the following compounds:

Bukester R1499lauric acid polyethylene glycol ester.

Amine oxides or quaternar ammonium salts of vinyl pyrrolidone dirnethylamino-ethylmethacrylate copolymers.

Vinyl pyrrolidone acrylamine copolymerssuch as a copolymer of vinyl pyrrolidone and 25% acrylamide.

Zelec DP--lauryl alcohol phosphate.

Catanac SN-stearylamidopropyl dimethyl-p-hydroxyethyl ammonium nitrate.

Ethoquad C/l2polyoxyethylated quaternary ammonium salt.

Phosphonamide sulfonate of an alcohol ethoxylate, i.e., a product of the formula whereinR represents the hydrocarbon residue of an 5 alkanol (such as Alfol 1412) and n represents an integer of 8 to 20.

Partial esters of the copolymer of vinyl methyl ether and maleic anhydride with nonionic surface active agentsdescribed in French Pat. No. 1,360,209.

Esters .of phosphoric acid and ethoxylated aliphatic alcohol such as the phosphate esters of lauryl alcohol condensed with 4 moles of ethylene oxide or of dodecyl alcohol condensed with about 2 moles of ethylene oxide Polyglycol 4000 Sucrose octa-acetate Polyethoxy amides of stearic and oleic acid Methyl diethanolamine ethoxylate Ethoxylated 2,3,7,9-tetramethyl-5-decyne-4,7-diol Polyoxyethylenemono-oleate Lauryl trimethyl ammonium chloride Undecylimidazolone Lauryl dimethylbenzyl ammonium chloride Polyoxyethyl stearyl ammonium chloride Oleic-monoisoproparol amide Vinyl acetate/styrene/ acrylic acid polymers Ethoxylated diamines Long chain amine oxides Hydroxybutyramides Quaternized polymers of vinylpyridine Quaternized copolymers of vinylpyridine and vinylpyrrolidone Phosphate esters of the type described in US. Pats. 3,004,056 and 3,004,057 and Belgian Pat. 641,097.

The phosphate esters of the type referred to in said patents may be prepared by reacting one mole of P with 2 to 4.5 moles of a nonionic surface active agent having the molecular configuration of a condensation product of at least one mole of ethylene oxide with one mole of a compound containing at least 6 carbon atoms and a reactive hydrogen atom under substantially anhydrous conditions and at a temperature below about 110 C. The process does not require the use of an excess of the hydroxylic organic compound (in this instance the defined nonionic surface active agent), in order to bring the P 0 into solution. Substantially no tertiary phosphate ester is formed and little or no P 0 remains in the composition. Depending upon the particular ratio of P 0 to the nonionic surface active agent employed, and the nature of such nonionic, the product may in some instances contain some unreacted nonionic surface active agent which for certain uses is actually advantageous.

For similar reasons, the proportions of secondary phosphate ester:primary esterzfree nonionic in the products thereof will in general fall within the range of about 20 to 45% secondary ester:30-80% primary ester:040% nonionic, by weight.

Lighter colored or substantially colorless products are obtained when the phosphation reaction is carried out in the presence of a small or catalytic amount of a phosphorus-containing compound selected from the group consisting of hypophosphorous acid, salts of hypophosphorous acid, phosphorous acid, and salts and esters of phosphorous acid. The process comprises reacting one mole of P 0 with 2 to 4.5 moles of a nonionic surface active agent having the molecular configuration of a condensation product of at least one mole of ethylene oxide with one mole of a compound containing at least 6 carbon atoms and a reactive hydrogen atom, under substantially anhydrous conditions and at a temperature below about 110 C. in the presence of a small amount of one or a 6 mixture of the aforementioned hypophosphorous or phosphorous acid compounds.

By the use of such compounds in the described phosphation reaction, it has been found that an unexpected and substantial improvement in the (absence of) color of the products and the resistance of such products to discoloration in storage is obtained. Products resulting from the use thereof generally have VCS (varnish color scale, Gardner scale, standards of 1933) values of at least one less than products of the same process carried out in the absence of the hypophosphorous or phosphorous acid compound. Products having a VCS color of about 1 or less are thus made possible, as compared with VCS colors of from about 2 to 7 or more for products produced without the aid of the present invention. Further, the products have been found to resist discolorations or darkening even after storage for three to six months.

The nonionic surface active agents employed as reactants are well known in the art and are disclosed along with suitable methods for their preparation in numerous patents and other publications. In general, they may be obtained by condensing a polyglycol ether containing the required number of alkenoxy groups or an alkylene oxide such as propylene oxide, butylene oxide, or preferably ethylene oxide, with an organic compound containing at least 6 carbon atoms and a reactive hydrogen atom. As such compounds containing a reactive hydrogen atom there may be mentioned alcohols, phenols, thiols, primary and secondary amines, and carboxylic and sulfonie acids, and their amides. The amount of alkylene oxide or equivalent condensed with the reactive chain, will depend primarily upon the particular compound with which it is condensed. As a convenient rule of thumb, an amount of alkylene oxide or equivalent should be employed which Will result in a condensation product containing about 20 to by weight of combined alkylene oxide. However, the optimum amount of alkylene oxide for attainment of the desired by hydrophobic hydrophilic balance may be readily determined in any particular case by preliminary test and routine experimentation.

In general, the nonionic surface active agents, having the molecular configuration of a condensation product of at least one mole of an alkylene oxide, preferably ethylene oxide, with one mole of a compound containing at least 6 carbon atoms and a reactive hydrogen atom are preferably polyoxyalkylene derivatives of alkylated and polyalkylated phenols, multi-branched chain primary aliphatic alcohols having the molecular configuration of an alcohol produced by the 0x0 process from a polyolefin of at least 7 carbon atoms, and straight chain aliphatic alcohols of at least 10 carbon atoms. Examples of these derivatives and other suitable nonionic surface active agents which may be phosphated in accordance with the present invention are included below. In this list, E.O." means ethylene oxide and the number preceding same refers to the number of moles thereof reactedwith one mole of the given reactive hydrogen-containing compound.

Nonylphenol+9-ll E.O. Nonylphenol+2 E.O. Dinonylphenol+7 E.O. Dodecylphenol+18 E.O. Castor oil+20 E.O. Tall oil+18 E.O.

Oleyl alcohol+20 E.O. Lauryl alcohol+4 E.O. Lauryl alcohol+15 E.O.

Hexadecyl alcohol-{-12 E.O. Hexadecyl alcohol+20 E.O. Octadecyl alcohol-F20 E.O. Oxo tridecyl alcohol:

(From tetrapropylene)+7 E.O. (From tetrapropylene) 10 E.O. (From tetrapropylene) +15 E.O.

erally, about 0.01 to 7 Dodecyl mercaptan+9 E.O. Soya bean oil amine+10 E.O. Rosin amine-F32 E.O. Coconut fatty acid amine+7 E.O. Cocoa fatty acid+ 10 E0. Dodecylbenzene sulfonamide+l E.O. Decyl sulfonamide+6 E.O. Oleic acid+ E.O. Polypropylene glycol (30 oxypropylene units),+ B0.

In carrying out the phosphation reaction the P 0 is preferably added gradually, with vigorous agitation to the nonionic surface active agent in liquid form. If the latter agent is a solid at room temperature, it should be heated to above its melting point. Addition of the nonionic surface active agent to the P 0 is inadvisable since this has been found to result in the formation of tar and the like and to prevent the reaction from proceeding to completion. The reaction is exothermic and in some cases cooling is necessary to prevent the temperature from going above 110 C. since this tends to produce discolored and darkened products. The reaction proceeds continuously during addition of the P 0 and solution thereof in the nonionic surface active agent, and is substantially 90% complete or more by the time all of the P 0 has been added. The few particles of solid P 0 remaining in the reaction medium may be removed at this point if time is of the essence, but it is preferred in the interests of economy to allow the reaction to proceed for an additional period of time which may range from /2 to 5 hours or more at ambient temperatures up to about 110 C. until all of the P 0 has dissolved indicating complete reaction between the reactants involved. Vigorous agitation during the reaction is highly desirable to facilitate and expedite completion of the reaction.

It is an advantageous feature that the P 0 may be employed in dry, solid form as a granular powder or other finely divided or particulate form, for reaction with the above defined nonionic surface active agents. However, if desired, the P 0 may first be dispersed in an inert organic diluent such as benzene, xylene, ether, pentane, or low and high boiling hydrocarbon fractions.

After completion of the reaction, the reaction mixture may be cooled and discharged. If carried out under rigid anhydrous conditions the product should consist of a mixture of the primary and secondary phosphate esters of the nonionic surface active agent combined, depending upon the proportions of reactants, in some instances with a small proportion of unreacted nonionic surface active agent. Any small amount of water present in the reaction mixture will result protanto in the formation of some phosphoric acid in the product. The degree of esterification in the product may be determined by potentiometric titration or by titration with alkali to methyl orange and then to phenolphthalein.

The products may be supplied in free unneutralized form, or in the form of the partially or completely neutralized salts containing as cations alkali metals, alkaline earth metals, metals, ammonium and organic amines. It is to be understood that such salts are to be regarded as the equivalent of the present products in heir free form. As examples of suitable cations, there may be mentioned sodium, potassium, lithium, calcium, strontium, barium, magnesium, iron, tin, cadmium, aluminum, antimony, chromium, manganese, mercury, nickel, silver, zinc, ammonium and aliphatic, alicyclic, aromatic and heterocyclic organic amines such as the mono-, diand tri-methylamines, ethylamines, propylamines, laurylamines, stearylamines, ethanolamines, propanolamines, butanolamines, hexanolamines, cyclohexylamines, phenylamines, pyridylamines, morpholinylamines, and the like.

Where desired, the above products may be modified by the addition to the reaction medium of a small amount of hypophosphorous or phosphorous acid compound. Genand prefe ably bout 8 of such compound, based on the weight of the nonionic surface active agent being phosphated is sufiicient to provide the desired improvements with respect to prevention of color degradation of the products and improvement in resistance of the products to color degradation in storage. Hypophosphorous acid and its alkali metal salts, e.g. sodium and potassium salts are generally preferred although any metal, alkaline earth metal, ammonium or amine salt of hypophosphorous acid or phosphorous acid may be employed, in addition to phosphorous acid per se. When hypophosphorous acid is employed, it is preferred to use a 30 to 50% aqueous solution thereof although aqueous solutions of this acid and other of the water soluble hypophosphorous and phosphorous acid compounds may be employed in the form of aqueous solutions ranging in concentration from less than 5 up to or more. It should be borne in mind that the reaction should be carried out under substantially anhydrous conditions and accordingly the water introduced in such solutions should be held to a minimum.

The salts of hypophosphorous acid and phosphorous acid employed herein may be in their hydrated or dehydrated form. As examples of such salts, there may be mentioned aluminum, cadmium, sodium, potassium, lithium, calcium, strontium, barium, magnesium, ammonium, mono-, diand tri-methylamine, -ethylamine, -propylamine, -ethanolamine, and -propanolamine, pyridinyl, and morpholinyl phosphites and hypophosphites.

Esters of phosphorous acid may also be employed. These esters may be described as mono-, di-, and tri-alkyl, -aryl, and -cycloalkyl phosphites. It will be understood that mixed esters are included. As some specific examples of such esters in which the esterifying group generally contains from about 1 to 20 carbon atoms, there may be mentioned ethyl phosphite, lauryl phosphite, Oxo tridecyl phosphite (the esterifying alcohol having the molecular configuration of an alcohol produced from tetrapropylene or triisobutylene by the 0x0 process), stearyl phosphite, phenyl phosphite, cyclohexyl phosphite, the corresponding diand tri-snbstituted phosphites, ethyl phenyl phosphite, ethyl diphenyl phosphite, lauryl cyclohexyl phosphite, dipropyl phenyl phosphite, and the like.

The hypophosphorous or phosphorous acid compound is preferably admixed with the non-ionic surface active agent prior to its addition to the nonionic surface active agent. It will accordingly be understood that the hypophosphorous or phosphorous acid compound or mixture thereof may be added at the start of the reaction or continuously or intermittently as the reaction proceeds.

The examples in the following table are only illustrative. In each of these examples, the nonionic surface active agent is first charged to a reactor equipped with an agitator. If the charge is solid at room temperature, it is heated to melt the same. The additive referred to in the table is then added to and dissolved in the nonionic surface active agent with vigorous agitation. The solid granular P 0 is then charged to the reactor with vigorous agitation over a period ranging from about 5 minutes to about 1 hour and usually about 15 minutes. After the initial exothermic reaction subsides, the reaction mixture is heated to C. and held at this temperature for about 5 hours after which the mixture is cooled and discharged. A sample of the reaction mixture is titrated with alkali to methyl orange and then to phenolphthalein as a control on the esterification. The VCS color readings are measured in the prescribed manner. A reading of one is the lowest color reading measurable by this method, the highest being 18. Products prepared with the use of the additives referred to in the table sustained no change in color after 3 to 6 months storage.

Preferred are the monoesters t of am the diesters and the mix- TABLE A NoniOIliO P305 VCS Example Nonionlc agent parts parts Parts Additive where employed color 1 Nonylphonol 2 E.O. CnH1oCaH (OCrH )zOH 2,888 284 Control 2 2- ..do 2,288 284 3.4 Hypophosphorous acid (50%)-.. 1 3- Nonylphenol 4 E O C H C H (OC H )4OH 2,855 213 ControL- 4. 2,855 213 4.2 Hypophosphorous acid (50%)--. 5- Nonylphenol 6 CoHnCuHKOCzHQsOH. 484: 47. 3 COIltl'Ol 4 6- do 484 47. 3 1.0. Hypophosphorous acid (50% 1 do 484 47.3 0.5..- Sodium hypophosphlte 1 do 484 47.3 2.0 Triphenyl phosphite 2 Nonylphenol 10 E.O. CoHmCsH (OCzH4)1o0H 1,821 108 Control 4 o. 1,821 108 7.0.... Hypophosphorous acid (30%)..- Nonylphenol 100 E.(). CgHmCoHKOCzHDmuO 605 11- 9 001111101 2 do (Z105 152.2"? Hypophosphorous acid (50%)--. 1 13 D on 1 henol 7E.O. C H C H 00 H) OH 27 on to 14- fidoi f. f.. .i 1 5 2 7 (1:.0. 1... Hypophosphorous acid (30%)... 15-- Dodec l henol 6E.O. C H CH 00 H 011.... 5 on to 16-- "din 1 f i ff ..2a.fi 1,106562 g.0 t 1 Hypophosphorous acid (50%)-.. 1.- .O trld ll hl 3E.O.CH OCH 0 onro 1%-- do ecy a c0 0 u M 1.2 166 23.7 1 Hypophxophorous acid (50%) g 19 do 23 7} Phosphorous acid- 2 20 L or 1 lcohol 4E.0. C H OCH OEL- 21- 141%: ..i "2f 724 71 1.8 Hypophosphorous acid 50%)--- i 1 From tetrapropylene by the 0x0 process.

A suitable quaternary ammonium compound, may be represented by the following structural formula:

wherein R=(CHY) CH and n=6 to 26; R" and R=(CHY) CH and n=0 to 6. The alkyl moiety may be branched or straight chain, y being hydrogen or an alkyl group as defined above. R" and R need not be the same.

The quaternary ammonium compounds may be made in ways known in the art, such as for example by dissolving in isopropyl alcohol one mole of dimethyl stearyl amine; then from a separatory funnel add thereto /2 mole of diethyl sulfate keeping temperature below 50 C.; after the last of the diethyl sulfate is added and the exotherm is stopped, reflux for one hour and cool. Evaporate the alcohol.

Preferred quaternary ammonium compounds include: compounds where R and R" are lower alkyl particularly preferred is wherein R and R" are methyl. R may be C saturated or unsaturated, i.e., cocoa, stearic, oleic and the like.

The quaternized copolymers referred to may be those that are compounds which are first copolymerized and thereafter quaternized or those wherein the monomers are first quaternized and then copolymerized. Procedures known in the art for carrying out the above processes may be employed.

The quaternary copolymers employed are those which have Unit I and either Units II or HI, or all three Units.

II III wherein n represents 40-90 mole percent, m is 10-60 mole percent, p is from 1060 mole percent and n+m or p or n+m+p==100; R is H or CH R is OH (|JH-CH2 or C H where x=218; R is CH or C H R is CH C2H5:

X is Cl, Br, I, S0 HSO CH SO and M is a monomeric unit resulting from the heteropolymerization employing a mono vinyl monomer different from and co polymerizable with n. M may be 5 to 40 where p is 0 to 50; the latter occurring where n, m and p are all employed.

As indicated from the above formula, such quaternary copolymers are prepared by the copolymerization of an N-vinyl lactam, such as N-vinyl pyrrolidone and di-lower alkylaminoalkyl (or hydroxy alkyl) acrylate or methac-,

rylate, and optionally a further mono vinyl different from and copolymerizable with n. The monomers are copolymerized in accordance with the present invention so that based upon mole percent, the vinyl pyrrolidone units are present in an amount of 40-90 mole percent, the units derived from the di-loweralkylaminoalkyl (or hydroxy alkyl) acrylate or methacrylate constitute from 10 to 60 mole percent, and the units derived from said further copolymerizable vinyl monomer also constitute from 10 to 60 mole percent.

Suitable heterocyclic N-vinyl lactams have the formula:

wherein R represents an alkylene bridge group of 2 to 4 carbon atoms necessary to complete a 5, 6 or 7-membered heterocyclic ring system, and R represents either hydrogen or a lower alkyl group, and n is an integer of at least 3.

All of the specific polymeric materials characterized by the foregoing general formula are commercially available and are called polymeric N-vinyl lactams. They are obtained by polymerizing organic 5, 6 or 7 membered ring compounds containing in their rings the --NHCO- group, such as, for example,

N vinyl-2-pyrrolidone, N-vinyl-2-piperidone, N-vinyl-Z-caprlactam, N-vinyl-3-methyl-2-pyrrolidone, N-viny1-3-methyl-2-piperidone, or N-vinyl-3-methyl-2-caprolactam, N-vinyl-4-methyl-2-pyrrolidone, N-vinyl-4-methyl-2-piperidone or N-vinyl-4-methyl-2-caprolactam, N-vinyl-S-methyI-Z-pyrrolidone, N-vinyl-S-methyl-2-piperidone, N-vinyl-3-ethyl-2-pyrrolidone,

N-vinyl-4,5-dimethyl-2-pyrrolidone, N-vinyl-S,5-dimethyl-2-pyrrolidone, N-vinyl-3 ,3,5-trimethyI-Z-pyrrolidone, N-vinyl-S-methyl-5-ethyl-2-pyrrolidone, N-vinyl-3 ,4,5-trimethyl-3-ethyl-2-pyrrolidone, N-vinyl-6-methyl-2-piperidone, N-vinyl-6-methyl-2-piperidone, N-vinyl-3 ,5 -dimethyl-2-piperidone, N-vinyl-4,4-dimethyl-2-piperidone, N-vinyl-7-methyl-Z-caprolactam, N-vinyl-7-ethyl-2-caprolactam, N-vinyl-3,S-dimethyl-Z-caprolactam, N-vinyl-4,6-dimethyl-2-caprolactam and N-vinyl-3,S,7-trirnethyl-2-caprolactam.

Of these several compounds, N-vinyl-Z-pyrrolidone is most preferred as it is readily available and provides products having excellent properties.

Exemplary di-loweralkylaminoalkyl (or hydroxy alkyl) acrylates or methacrylates suitably employed include such materials as:

dimethylaminomethyl acrylate dimethylaminomethyl methacrylate diethylaminomethyl acrylate diethylaminomethyl methacrylate dimethylaminoethyl acrylate dimethylaminoethyl methacrylate dimethylamino-Z-hydroxy propyl acrylate dimethylamino-Z-hydroxy propyl methacrylate diethylamino-2-hydroxy ethyl acrylate diethylamino-Z-hydroxy ethyl methacrylate dimethylaminobutyl acrylate dimethylaminobutyl methacrylate dimethylaminoamyl methacrylate diethylaminoamyl methacrylate dimethylaminohexyl acrylate diethylaminohexyl methacrylate dimethylaminooctyl acrylate diethylaminooctyl methacrylate diethylaminooctyl acrylate diethylaminooctyl methacrylate dimethylaminodecyl methacrylate dimethylaminododecyl methacrylate diethylaminolauryl acrylate diethylaminolauryl methacrylate dimethylaminostearyl acrylate dimethylaminostearyl methacrylate diethylaminostearyl acrylate diethylaminostearyl methacrylate etc., the non-hydroxy alkyl units being preferred.

The mono vinyl or vinylidene monomer represented by M in the above structural formula can comprise any conventional vinyl monomer copolymerizable with N-vinyl pyrrolidone. Thus, for example, suitable conventional vinyl monomers include the alkyl vinyl ethers, e.g., methyl vinyl ether, ethyl vinyl ether, octyl vinyl ether, etc.; acrylic and methacrylic acid and esters thereof, e.g., methacrylate, methyl methacrylate, etc.; vinyl aromatic monomers, e.g., styrene, a-methyl styrene, etc.; vinyl acetate; vinyl alcohol; vinylidene chloride; acrylonitrile and substituted derivatives thereof; methacrylonitrile and substituted derivatives thereof; acrylamide and methacrylamide and N- substituted derivatives thereof; vinyl chloride, crotonic acid and esters thereof; etc. Again, it is noted that such copolymerizable vinyl monomer can comprise any conventional vinyl monomer copolymerizable with N-vinyl pyrrolidone and where a terpolymer is formed, copolymerizable with both units n and m, and being different from both.

Accordingly, preferred quaternized copolymers employed in the present invention can be characterized as having a repeating structural unit derived from (A) 40-90 mole percent of vinyl lactam;

acrylate or methacrylate of a di-loweralkylaminohydroxylalkyl acrylate or methacrylate; or

(C) 10-60 mole percent of a vinyl monomer different from and copolymerizable with A and B.

Such copolymers are conveniently prepared by subjecting a solution of vinyl lactam and the amino acrylate or amino methacrylate monomer with or without an optional copolymerizable vinyl monomer to conditions conducive to vinyl polymerization through the double bond. Thus, for example, polymerization may suitably be initiated by the action of free radicals, the polymerization proceeding exothermically once initiated. Suitable free radical catalysts conveniently employed and suitably utilized in accordance with the production of the copolymers include organic and inorganic peroxides, e.g., hydrogen peroxide, t-butyl peroxide, etc., aliphatic azo compounds, e.g., azobisisobutyronitrile as well as other free radical forming catalysts well known in the polymerization art.

The polymerization is preferably carried out in solution at temperatures varying from about 50 C. to 100 C. or more; however, to avoid run away conditions and to obtain a copolymer of a desirable molecular weight it is sometimes preferred to carry out the copolymerization at a temperature of from about to about C. The copolymerization reaction is preferably carried out in the absence of free-oxygen, conveniently under a blanket of an inert gas, such as, nitrogen, argon or the like, or at atmospheric pressure.

As indicated previously the copolymers are in the form of their quaternary salts. Accordingly, after completion of the polymerization reaction the polymer is submitted to a treatment conducive to quaternization of the tertiary amino group, utilizing a conventional quaternizing agent. Thus, noting the above structural formula for the copolymers, suitable quaternizing agents include, such as, dialkyl sulfates, e.g., dimethyl sulfate, diethyl sulfate, etc.; alkyl sulfonic acid, e.g., methyl sulfonic acid, ethyl sulfonic acid, etc.; benzyl halides, e.g., benzyl chloride, benzyl bromide, benzyl iodide, etc.; alkyl halide, etc. Accordingly, any conventional quaternizing agent can be advantageously employed in the production of the quaternary N-vinyl pyrrolidone copolymers used in the compositions of the present invention.

The molecular weight of the quaternized copolymers should be between 800 and 5,000.

Operative group IA, IIA and HE metal sulfonates and sulfates may be represented by the following generic formulae:

1. Alkylaryl Sulfonates (i.e. Naccanol 402B) 2. Alkylbenzene Sulfonates 3. Linear Sulfonates R is CH (CH n is 0-200 H R-o o crn-oH,-o

5. Sulfonated Esters n is 1-1000 13 14 r as glycerol, urea, ethylene glycol, sorbitol, ethoxylated R is e- 7 ni 2-1 sorbitol, lauric acid esters and mixtures of the same.

It will be apparent that where a deliquescent salt is Ms H4 employed as the humectant, it may also function as an A 5 electrolyte. However, where glycerine or other nonionic humectants are employed, they should be combined with R13 H 11 is an electrolyte. Also in the case of deliquescent salts, such as sodium and potassium formate which have a relatively Alkyl Naphthalene Sulfonates Nekal BA'75) low dissociation constant, it is preferable to incorporate a 7. Igepon As 10 small amount of a salt of a strong base and strong acid 0 having a high dissociation constant, such as sodium chlo- J ride, potassium chloride or calcium chloride. Salts which 8 I e on T5 are not sufficiently deliquescent such as sodium chloride, g p sodium sulfate, potassium nitrate, so that they do not 0 function wholly satisfactorily as both humectant and elec- R-i J N CH1 CH;S oaNa trolyte, can be employed in combination with a nonionic (R and are alkyl or aromatic groups) humectant, such as glycerine or urea or in combination with a more highly deliquescent salt, such as potassium 15 to be undel'sto9d that y one of the above 9 formate or calcium chloride. Thus in the composition of pollen'ts may be used 111 Place of the alkoxylated ternary the present invention, the humectant and electrolyte may amme however humectant whefe F the be either a single compound or a mixture of compounds. electrolyte) must still be employed in COIljllIlCtlOfl theredesired a further backing, such as a jute backing, Wlthillustrated as 10 in the drawings, may be applied over Partlcularly prefefred antlstatlc layers based the latex coating, but is not an essential element of the oxylated tertiary amines represented by the following gencarpet Structure f this invention eral formula: The details of the present invention will be apparent (OHR'-CHR-0)..H from consideration of the following specific examples and RN claims, in which all parts, proportions and percentages are by weight unless specified otherwise.

(OHR'GHR'O)..H E AMPL wherein R represents analiphatic hydrocarbon radical of X ES from about 8 to about 22 carbon atoms, each R represents In these examples the antistatic composition was prehydrogen or methyl and n represents an average integer pared by adding the base and organic acid to water to of at least 1, preferably 1 to about 30, although higher form the humectant in situ. The alkoxylated amine emalkoxylated derivatives, i.e., the products obtained by ployed was stearyl amine which had been ethoxylated with condensing 1 molar proportion of a primary aliphatic 20 moles of ethylene oxide per mole of amine. The thus (saturated or unsaturated) amine with up to 50 molar prepared antistatic composition may, if desired, be modiproportions of an alkylene oxide, usually ethylene oxide, fied by thickening with any known thickener, such as may be employed if desired. Such alkoxylated amines are sodium polyacrylate, methyl cellulose or the like. A pH well known in the art and are prepared by condensing 40 adjustment up to about 7-13 may also be desirable in the primary saturated or unsaturated aliphatic amine of certain instances were reduced susceptibility to migration from 8 to 22 carbon atoms, with an alkylene oxide, usually and enhanced flame retardency are desired. A wetting ethylene oxide, although propylene oxide and butylene agent where employed, may be tridecyl alcohol which had oxide may be employed if desired, until glycol groups of been ethoxylated with 6 moles of ethylene oxide per mole desired chain length are obtained. Such products have been of alcohol. disclosed, for example in US. Pats. 1,970,578, 2,174,762, In all cases the antistatic coating was applied to the 2,510,284 and 2,593,466. underside of the latex pre-coat layer, the latter having been As a humectant in the composition of the present invenapplied to the back of a tufted carpet having a primary tion there may be used various deliquescent salts of metals loosely wooven jute backing, and the type of fibers cmof the Groups I and H, Periodic Table, particularly of the ployed in the tufted pile are given in Table I as well as alkali metal and alkaline earth metals. Specific deliquethe amount of antistatic composition applied to the scent salts which I prefer to employ as humectant, include underside of the pre-coat layer. After application of the alkali metal salts of lower aliphatic carboxylic acids, the antistatic coating the carpet was dried to remove such as sodium formate, potassium formate, lithium excess moisture. A latex coating was then applied over formate, cesium formate, sodium and potassium acetate, the antistatic coating. potassium butyrate and mineral acid salts like calcium The testing procerure used in these examples was the chloride. There may also be used such organic humectants AATC 134-1969 Test.

' TABLE I Humectant Parts Coating Basic wet- Elec- DH wt. in Example com- Organic Parts ting tro- Parts adjustment Carpet ozs. per number poun arts acid Parts amine agent lyte Parts water acid or base pH fiber sq. yard 1 NaOH 40 Formic. 56 20 2 NaCl 2 6.5 Acrylic 5 2.. NaOH 40 .-do 66 20 2 NaCl 2 6.5 Polyester 6 3 NaOH 40 20 2 NaCl 2 6.5 Po1ypropy1ene-. 6 4. NaOH 40 20 2 NaCl 2 9 Nylon 5 5. NaOH 40 20 2 NaCl 2 6.5 5 6 R011 56 20 2 NalC 2 9 4 7 KOH 56 20 2 NaCl 2 6.5 5 3.... NaOH 10 1 K01 1 6.5 5 9. NaOH 10 1 KCl 1 6.5 4 10 KOH 20 1 N801 2 6.5 6 11 E011 20 1 NaCl 2 6.5 4, 12 KOH 25 1 NaCl 3 6.5 5 1a KOH 25 1 NaCo a 6.5 5 14... KOH 25 2 NaOl 2 5 5 15 KOH 25 2 NaCl 2 5 5.5 5 i 5 Poiypropulene 5 Untreated control.

TABLE IL-STATIC RESULTS ACORDIN G TO AA'lC 134-1969 Before cleaning, After steam cleaning, Control-No treatment,

volts volts volts TABLE IV.-STATIC RESULTS ACCORDING TO AATC 134-1969 Before cleaning After steam cleaning Chrome Neo- Chrome Neo- Chrome Neo- Chrome Chrome Ex. leather lite leather lite leather lite leather Neollte leather Neolito +100 -100 +450 +500 +10-1l, 000 45, 000 2, 000 1, 300 1,500 l, 400 -250 250 +400 +600 2, 000 1, 300 1, 500 -1, 400 ---100 l00 500 500 300 200 800 -400 1, 300 -1, 400 1, 100 1, 200 100 +200 1,000 -1, 100 500 800 500 -800 -l, 700 1, 300 1, 500 1,100 400 600 -1, 300 -1, 200 l, 200 1, 300 300 500 1, 300 -1, 200 7, 000 1, 000 200 300 -1, 700 -900 1, 500 1, 100 800 1,000 -1, 700 -1, 800 1, 600 1, 900 600 700 1, 200 -1, 200 800 900 200 800 -1, 800 1, 300 1, 500 1, 200 400 1, 200 700 --1, 100 900 1, 200 600 400 81 --1, 100 1, 200 800 950 800 600 800 1, 200 900 1, 100 850 -7, 000 4, 200 11, 000 5, 200 17, -5, 400 9,000 0, 200

EXAMPLES 18-3 3 EXAMPLES -49 In these examples the samples treated were nylon and wool tufted carpet structures. In all cases the antistatic coating was applied in the same manner as in the preceding examples.

In these examples the humectant was not formed in situ, but instead was added directly to the antistatic composition. In Examples 41-44 the calcium chloride functioned as both a humectant and electrolyte.

The composition of the antistatic coating, as well as the test results and other pertinent information for these examples are given in Table V.

TABLE III Humectant Parts Coating ting Elecwt. in Example Basic Organic Parts agent tro- Parts pH adjustment Carpet ozs. per number compound Parts acid Parts amine wetlyte Parts water acid or base pH fiber sq. yard NaOH 20 2 NaCl 2 NaOH 60 20 2 NaCl 2 KOH 46 20 2 NaCl 2 KOH 46 20 2 N 301 2 NaOH 23 10 1 KCl 1 NaOH 23 10 1 KCl 1 KOH 60 20 2 NaCl 1 KOH 60 20 2 NaCl 1 KOH 74 25 2 NaCl 3 KOH 74 25 2 NaCl 3 KOH 56 25 3 NaCl 2. 5 KOH 56 25 3 NaCl 2. 5 29% NH4OH 60 20 2 NaCl 2 29% NH OH 46 20 2 NaCl 2 29% NH|OH 121 Propiom 74 20 2 NaCl 2 1 Untreated control.

TABLE V Parts Coating pH adjustwt. in Example Parts ting Electro- Parts ment acid Carpet ozs. per number Humeetant Parts amine agent lyte Parts water or base pH fiber sq. yard 35 Sorbitol ester 10 20 1 NaCl... 1 Acetic 5 Cl 20 20 2 do 5 20 20 5 2o 20 5 30 2o 5 30 20 5 30 20 5 40 20 5 40 2o 5 40 20 2 5 10 10 1 CaClz. 10 5 30 a 10 1 NaCl-.. 1 5 30 4 10 u 5 1 Ethoxylated sorbitol launlc acid ester.

2 Humectant was electrolyte.

1 N -octyl, N -ethyl morpholinium ethosulfate. 4 Quaternary diethyl sultate imidazollne.

I Untreated control.

TABLE VI.STATIC RESULTS ACCO RDIN G T AATC 134-1969 Before cleaning After steam cleaning Chrome Chrome Example leather Neolite leather Neollte EXAMPLES 50-78 by the reaction of a basic component as in Examples 1- 18. The procedure for these examples was as follows:

10 to minutes. The dried fabric was then conditioned for at least 6 hours at a temperature of 70:5 F., and to relative humidity. The coated material was then tested on an Atlab Tester, as developed by the Atlas Chemical Co., Wilmington, Del. The test procedure consists essentially of a means of controlled rubbing of a strip of fabric across a pair of static-generating (Teflon) bars and across a stainless steel bar which transfers the friction generated charge to an electrostatic voltmeter for measurement. This testing was conducted at 77 F.- -2 F., and at a constant relative humidity of 35 to 40%.

The composition of the antistatic coating, as well as the test results and other pertinent information for these examples, are given in Table VII.

EXAMPLES 79-1 11 In these examples the samples treated were conventionally woven and nonwoven fabrics of the type and fibers shown in Table VII. In all cases the antistatic coating was applied in the same manner to the back of the precoat latex and the textile sample dried to remove excess moisture. A polymeric backing was then applied to the fabric and cured at a temperature of from 200- 325 F. for from 10-30 minutes. The coated material was then tested on an Atlab Tester in the manner de- TABLE VII Hmneetant Elec- Parts troamine lyte NaOl NaCl 20 NaCl 20 NaCl 20 NaCl 20 NaOl Basic compound Organic Example Parts acid number 121 Formic 121 Acetic q as mammuxq a a; ooeczmoevhmfiw a agg ag pH adjust- Parts ment acid or Parts water base 210 Acetic Percent Charge coating build-up pH Nylon textile weight o Upholstery .do

150 do 200 Acetic 2 0 d l Untreated.

The samples were cut and coated first with a latex backing and then with the antistatic coating. In these examples, the coating weight was based on the weight of the fabric in question. A polymeric backing was then applied to the fabric and dried at a temperature of from about 200 to 325 F. for a period of time of from about H moo H scribed above in connection with Examples 77-78. In these examples the humectant was not formed in situ, but instead was added directly to the antistatic composition.

The composition of the antistatic coating as well as test results and other pertinent data for these examples are given in Table VIII.

TABLE VIII Wet- ting EleepH Percent Charge Amine agent tro- Parts adjustment coating build-up Ex. No; Humeetant Parts parts parts lyte Parts water acid pH Textile weight in kv.

10 10 1 NaCl 1 Acetic 5.5-6.5 Tafiete 2 1 10 10 1 NaCl 1 70 do 5.5-6.5 .....(10 5 0 10 10 1 NaCl 1 70 ..do 5.5-6.5 do 10 0 10 10 1 NaCl 1 70 ...do 5.5-6.5 Nylon rayon filled 2 1 upholstery.

10 10 1 NaCl 1 70 do 5 5 10 10 1 NaCl 1 10 0 20 20 0 CaClz 5 2 1 20 20 Y 0 CaCla 5 5 0 20 20 0 CaCh 5 10 0 20 20 0 CaCl: 5 2 1 20 20 0 02.012 5 5 0 See footnotes at end of table.

in kv.

TABLE VIIIContinued Wet- ting ElecpH Percent Charge Amine agent tro- Parts adjustment coating build-up Humcctant Parts parts parts lyte Parts water acid pH Textile weight in kv.

20 20 68.013 75 Acetic 6. 0-6.5 Upholstery 0 2O 01 0 100 do 5.5-6.5 Taffeta.-. 3 O 20 20 01 (i) 0 5 .5 d0 5 0 2O 20 01 0 .5 ..d0... 10 0 20 20 01 0 5.5-6.5 Upholstery- 3 0 20 20 01 t) 0 5.5-6. d 5 0 20 20 01 (5) 0 5.5-6. 10 0 30 20 01 0 5. 0-5. 3 0 30 20 01 0 5. 0-5. 5 0 30 20 01 (a) 0 5. 0-5. 10 0 30 20 01 (5) 0 5. 0-5. 3 0 30 20 01 (is) 0 5. 0-5. 5 0 30 20 01 (i) 0 5.0-5. 10 0 4O 20 01 (a) 0 5.0-5. 3 0 40 20 01 (s) 0 5. O-5. 5 0 40 20 01 (s) 0 5.0-5. 0 l0 0 40 20 01 (5) 0 5. 0-5. 3 0 40 20 01 (i) 0 5. 0-5 5 0 40 20 01 (5) 0 5. 0-5.5 d0 10 0 30 1 10 1 NaCl 1 5 0-5 5 TafietL 2 5 0-1 30 10 1 NaCl 1 do 5. 05.5 Nylon ray 5 0-1 upholstery. 30 1 10 1 NaCl 1 110 .do 5. 0-5. 5 Nylon rayon non-w0ven. 5 .5

1 N-octyl, N-ethyl morpholinium ethyl sulfate. I Condensate 0f tridecyl alcohol with 6 moles of ethylene oxide. 3 Etlioxylated sorbitol lauric acid ester.

EXAMPLES 1 12-1211 4 Nylon-unless otherwise specified. 6 Humectaiit was electrolyte.

a) an organic antistatic agent,

In these examples the sample floor covering was treated a humfictfmt Selected from the group of lomc in accordance with the components as given in Table and nomomc humcctantsifim IX. The antistatic coating was applied in sandwich Whfin Such cctant is a nonionic humecform to the underside of the flooring product in accordtant, an electrolyte, and ance with the procedure as outlined earlier. Electrostatic p lymeri a king layer covering said antistatic test results are given in Table X. layer, said antistatic layer being disposed between TABLE IX Basic Eleccompo- Organic tro- Parts pH adjust- Ozs. per nent Parts acid Parts Conductor parts on soiids bases Parts lyte Parts water ment pH sq. yard KOH 56 Formic--- 46 Naccanol-40 lb 20 NaCl 2 180 KOH 8.5 4 KOH 5 do 46 Nansa HS- 20 NaCl 2 180 KOH 8.5 4 KOH 56 do 46 Sodium lauryl sulfate" 20 NaCl 2 180 KOH 8.5 4 KOH 56 do 46 Alipal 4 20 NaCl 2 180 KOH 3.5 4 KOH 56 ...do 46 Gaitex 288 20 NaCl 2 180 KOH 8.5 4 K011 56 do 4s NekalBA-75 20 NaCl 2 180 KOH 8.5 4 KOH so do 4e IgeponAP-78 20 NaCl 2 180 KOH 8.5 4 KOH 56 do 46 Igepon T-33- 2o NaCl 2 180 KOH 8.5 4 KOH 56 -.do 46 Aerosol OT 20 NaCl 2 180 KOH 8.5 4 121 KOH 56 do 46 Triethanol amine lauryl sulfate..- 20 NaCl 2 180 KOH 8.5 4

1 See tests Table X.

TABLE X said pre-coat layer and said polymeric backing layer. e A' 1969 readings in electrostatic l 2. An antistatic product as defined in claim 1 wherein After Steam cleaning said Wear layer is a fibrous textile material. Ch Ch 0m 3. An antistatic product as defined in claim 2 wherein 1'01'116 l Example number leather Neolite leather Neolite 531d 011s q layer 13 of the P yP 4. An antistatic product as defined in claim 3, wherein +i,20o 90o +l,700 -1,00o fib +1'500 1,000 44,600 sai rous textile layer is a tufted carpet structure hav- H.200 +1,80 4,500 ing pile fibers tufted through a woven backing. +1, 100 -1,400 +1,500 1,200 +1'500 400 4.17200 400 55 5. An antistatic product as defined in claim 4, wherein +1, 900 -1,700 +2, 000 l,900 +1300 2000 +1 770 100 said organic antistatic agent is an alkoxylated tertiary +1,e0 -1,s0o +1, 500 -2,0oo amine. +1. 6. An antistatic product as defined in claim 3, wherein It is obvious that numerous changes and modifications can be made in the above described details without departing from the spirit and nature of the invention. Therefore, it is to be understood that any such changes and modifications are included within the scope of the invention and that the invention is not to be limited except as set forth in the appended claims.

I claim:

1. An antistatic textile and floor covering product comprising l) a wear layer,

(2) a latex pre-coat layer disposed on at least one surface of said layer,

(3) an antistatic coating composition layer disposed on said pre-coat layer, said antistatic layer consisting essentially of a mixture of said antistatic coating composition is applied at a concentration of from about 2.0 to 10 oz. per sq. yd.

7. An anistatic product as defined in claim 6, wherein said organic antistatic agent is an alkoxylated tertiary amine.

8. An antistatic product as defined in claim 3 wherein said fibrous pile is secured to a primary backing layer.

9. An antistatic product as defined in claim 2, wherein said organic antistatic agent is an alkoxylated tertiary amine.

10. An antistatic product as defined in claim 1 wherein said floor covering is selected from the group consisting of vinyl homopolymeric and copolymeric sheet and tile products, asbestos-composition sheet and tile products, polyurethane and polyolefin flooring products and linoleum-petroleum products.

11. An antistatic product as defined in claim 1, wherein said antistatic coating composition is applied at a concentration of from about 0:1 to 20 oz. per sq. yd.

12. An antistatic product as defined in claim 11, wherein said organic antistatic agent is an alkoxylated tertiary amine.

13. \An antistatic product as de'fined in claim 1, wherein said organic antistatic agent is an aJ-koxylated tertiary amine.

14. An antistatic product as defined in claim 1, wherein said organic antistatic agent is a quaternary ammonium compound.

15. An antistatic product as defined in claim 1, wherein said humectant is an ethoxylated sorbitol lauric acid ester.

22 16. An antistatic product as defined in claim 1, wherein said organic antistatic agent includes as amine, N- octyi-iN-ethyl morpholinium ethylsulfate.

17. \An antistatic product as delfiued in claim 1, wherein said organic antistatic agent is a phosphate ester.

References Cited UNITED STATES PATENTS 8,510,686 5/[1970 Goins 15 1-66 MARION E. MCCAM-ISH, Primary Examiner US. Cl. X.R.