DE2401221A1 - ANTISTATIC TEXTILE AND FLOORING PRODUCT - Google Patents

Description

The invention relates to antistatic textile and floor covering products with improved resistance to cleaning and less tendency to migrate; it concerns in particular an antistatic carpet that has a "layer of fiber, an underlying primary backing, an applied to it." Latex pre-coating, an anti-static conductive coating and © has a polymer base (reinforcement)

Usual floor coverings, especially carpet structures, can Generate and transmit considerable electrostatic charges, mesa electrostatic charges occur when people are in the Contact with the wearing dielectric layer, e.g. the fiber layer of the carpet, occurs on this fiber layer move. The charge itself is created by the movement of dielectric shoe components that interact with the dielectric The protective layer are in contact · These charges are then transferred to the shoe wearer. When the carrier is then grounded, the enriched charge is discharged through the part of the person's body that is in contact with the earth.

409830/0789

person to be very uncomfortable. Bas described above Problem can be eliminated if the electrostatic charges are distributed within the flooring structure and subsequently can be derived into the environment.

Antistatic coating materials and carpet structures are already known. For example, US Pat. No. 2,302,00J describes that enriched electrostatic charges can be distributed over a multiplicity of electrically conductive fibers which are arranged within the fiber layer. In U.S. Patent schx'ift 3,510,386 describes a! Peppichstruktur which is disposed an anti-static layer _comprises% directly below the Abnutzungoschicht (sliding layer), in this case the batt primary backing. It is stated therein that the antistatic layer can alternatively be arranged directly below the primary element, so that the antistatic coating compound overlooks the ends of the fibers and makes contact with them. which form the pile that is in contact with it. It also states that the antistatic coating must penetrate essentially into the backing and into part of the pile fibers in order to be effective ,, and their effective lifespan. A secondary problem that arises is the risk of fire due to the flammability of the carpet structure as a result of the migration of the antistatic coating material upwards through the textile structure, which leads to a stiffening of the pile, which then stands up for the attack of the flame, as well as the The fact that the migration leads to a loss of effectiveness and durability of the product when such a treated carpet is washed «

In contrast to this, in the textile and floor covering products according to the invention, electrostatic charges become quickly and

409830/0789

thoroughly distributed without the need for specific electrically conductive fibers. The structures according to the invention, dissipate electrostatic charges.

The antistatic coating composition of the invention is Introduced between two polymer bases or reinforcements, in contrast to the vast majority of the known ones antistatic coating compositions suitable for a such "sandwich-like arrangement" and insulation between polymeric substrates or reinforcements are neither compatible nor are effective. Because of this! ^ Compatibility, in particular in carpets that had been treated with these known antistatic coating compositions, previously the most polymeric underlays or reinforcement layers and in particular the IT natural latex underlay that is commonly used Not used. In contrast, the -is according to the invention used antistatic cover with natural latex underlay or reinforcement layers, adhesives and most other polymeric coating compounds.

The following description relates to the most preferred embodiment of the invention, i.e. a carpet structure, however, it is clear to those skilled in the art that it is not limited thereto. Under the term used here "Flooring" also means linoleum-petroleum product flooring, vinyl and asbestos panels and tile flooring, polyurethane and polyolefin floor coverings and the like, to which the present invention also relates.

The present invention seeks to provide an improved antistatic Specify textile and floor covering product with a higher resistance to cleaning and a lower tendency for the antistatic coating material to migrate. target It is also of the invention to provide an antistatic floor covering product with an antistatic coating that is distributed between two polymeric layers, which in turn underneath the wear layer of the flooring product

409830/0789

are arranged. The aim of the invention is also to provide a new antistatic {deppich structure.

Further objects, features and advantages of the invention are given the following description.

The invention generally relates to an antistatic textile and floor covering product, which is characterized is that it has

(1) a wear layer _$ β * Β. cine fiber textile layer,

(2) a latex slip layer located underneath this wear layer ,

O) a precoat layer located beneath this Layer of an antistatic coating composition, which consists essentially of a mixture of

(a) an organic antistatic agent,

(b) a wetting agent from the group of the ionic and non-ionic humectants and

(c) an electrolyte when that humectant is a non-ionic humectant, and

(4-) a polymeric backing layer (reinforcement layer), which covers the antistatic layer, which in turn lies between the precoat layer and the polymeric backing layer is arranged.

The antistatic which is the subject of the present invention Floor covering and textile structure is shown in the only figure of the accompanying drawing on the basis of a carpet, a preferred embodiment of the invention, explained in more detail. The floor covering, i.e. the carpet, 2 has a usual wear layer (Running layer), e.g. a fiber layer, 4 on,

409830/0789

which can be blown, tufted, knitted, flocked or of some other structure, as is customary in carpets. This fiber layer can consist of any of the usual textile fibers or mixtures or mixtures thereof, such as those used for the production of carpets, for example from wool, polyamides (e.g. ITylon 66 and Hylon 6), cotton, polyolefins (especially polypropylene), acrylic, modacrylic fibers, Polyesters and the like The fiber layer 4 is woven into or looped through (tufted) or in some other way attached to a backing layer 5, in the form of a woven cotton or jute fabric, although other fibers and other types of construction can be used for the reinforcement «The basic carpet structure can be any carpet product, for example one of the well-known tufted, Brussels, Wilton, Axminster, chenille, Velvet, flocked, knitted carpets and the like - or pile layer 4 with its primary backing 5 'to which the fiber-forming pile is attached or by we When it is looped through and the like, coated with a latex precoat layer 3 consisting of. any of the usual latices, this layer then being provided with an antistatic coating 6 which forms a uniform, continuous layer thereon. 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 to produce this antistatic coating should be sufficient to substantially cover the precoat layer 3. Normally, about 0.34 (0.01 to 20 oz./yd). To about 680 g / m, preferably 68-340 g / m ² (2.0 to 10.0 oz./yd· ²⁾ of the anti-static Coating applied.

The one used for the preparation of the antistatic coating layer 6 The antistatic coating compound ideally consists of a mixture of a textile antistatic agent and 10 up to 50 parts by weight of a humectant. It can also about 0.1 to about 1 part by weight of a non-ionic

409830/0789

or a cationic wetting agent can be used to distribute the antistatic coating composition support. Preferably about 0.1 to about 1 part by weight of an electrolyte also ground the coating composition incorporated, especially if a non-ionic or a weakly ionic humectant, i.e. a ' one with a relatively low dissociation constant is used. The one used to make the antistatic Coating 6 used antistatic coating composition is preferably in the form of an aqueous solution or Dispersion applied, although others if desired Solvents or liquid dispersing media can be used can, and in the case of aqueous solutions or dispersions, volatile, water-soluble solvents, e.g. lower aliphatic ^ alcohols with 1 to 4 · carbon atoms, acetone and the like, may be added to facilitate drying of the antistatic layer after application thereof.

Examples of Satisfactory Latex Precoating Layers 3 * which can be applied to the underside of the primary substrate 5 are filled or unfilled coatings made of acrylic latices, Vinyl acetate latices, styrene / butadiene latices (preferably carboxylated latices), natural latex, vinyl chloride / vinylidene chloride copolymers and the like. With plasticizing monomers such as butyl acrylate, and ethylene / vinyl chloride copolymers and the like. Satisfactory adhesive coatings include all of the above, in general however, styrene / butadiene latices are preferred.

After the antistatic coating 6 has been applied to the precoat layer 3 , a polymeric backing layer (reinforcement layer) 8 is applied to the carpet and forms an essential element of the carpet structure of the invention. This polymeric backing layer is preferably applied in the form of an aqueous dispersion (latex) and it preferably consists of a known natural rubber latex or

409830/0789

from a compounded carboxylated butadiene / styrene rubber latex, which is commonly used as latex underlays for carpets; is used, although other polymeric coatings ₉ ZeB, those made of polystyrene, vinylidene chloride * polyacrylates, butadiene / styrene rubbers and the like can be used here as well as for the pre-absorbent layer 3 Examples of known compounded natural rubber which are commercially available are as follows: Lotol GX-3I8O (a product of Firraa US Rubber Company), compounded, carboxylated styrene / butadiene G-UHaiilatices, such as Lot; el GX-IO76 (a product of Γ Irma US Rubber Company).

Although the exact requirement for the antistatic property The tone of the inventive product is not yet complete gG are clarified, it is believed that the two polymeric übercraügo 3 and 8 have the function of anti-static coating 6 sticking to the right place without glitching To hinder the distribution of the electrical charge · The electrostatic charges accumulated in the pile 4 are protected by the antistatic layer 6 within the entire? Distributed on the carpet and then in the ground or in the atmosphere derived. In order to support the discharge of these charges into the earth, the polymeric coatings 3 and 8 a material such as carbon black or any agent that reduces the dielectric properties of the polymeric layers, be incorporated.

A series of preferred compositions for antistatic Cover layer 6 of the carpet structure according to the invention are described in U.S. Patent 3,519,561. Particularly preferred are those antistatic compositions described in this patent in which as humectants Potassium formate is used because it has been shown that potassium formate is not only particularly effective as a moistening agent in such coating compounds, but also which contain it, compatible with the latex underlay are and therefore in particular cause premature coagulation

409830/0789

or gelation of the latex underlay on the basis of a compounded natural rubber can be prevented so that there is no disturbance of the good bond between the latex cover and the toppich underlay , since they cause premature coagulation or gelation of the latex, which results in poor adhesion of the latex to the base, so that in the event of loosely woven or tufted layers, the latex does not adhere to the surface in a satisfactory manner right place.

Although antistatic layers based on the antistatic coatings described in the above-mentioned patent are particularly preferred, any other antistatic layer based on any known antistatic material suitable for textiles and electrostatic charges can of course also be used " Such agents normally include nitrogen-containing or carboxyl-containing organic antistatic agents and suitable examples of these are the following products:

Buchester H1499 - a. Lauric acid polyethylene glycol ester; Amine oxides or quaternary ammonium salts of yinylpyrrolidone / dimethylaminoethyl methaerylate copolymers; Vinyl pyrroli-

don / acrylamide copolymers, for example a copolymer of 75 ° / ° vinylpyrrolidone and 25 % acrylamide; Selec SP - lauryl alcohol phosphate;

Oatanac SN - Stearylamidopropyl-dimethyl-ß-hydroxyethyl-ammo

nium nitrate;

Ethoquad G / 12 - a quaternary polyoxyethylated asmonium

Phosphonamide sulfonate of an alcohol ethosylate, i.e. a product

the formula

409830/0789

R- (OCH ₀ CH ₀ ) -OP-NCH,

CH ₀ CH ₀ SO ₅ -Ca

d d O

where R is a hydrocarbon radical of an alkanol (e.g. _# Alfol 1412) and η is an integer from 8 "to 20; partial esters of vinylraethyl ether / maleic anhydride copolymer with non-ionic surface-active agents ₉ as described in French patent 1,360 are described? ester of phosphoric acid and ethoxylated aliphatic alcohols, for "B _e the Phosphatester of lauryl alcohol, condensed with 4 moles of ethylene oxide, or from Doedecylalkoholj condensed with about 2 moles Ithyleaoxyd, polyglycol 4000, sucrose octaacetate, Polyäthoxyainide of stearic acid and oleic acid ₉ Methyldiäthanolaiainäthoxylat, ethoxylated 2.3 »7 % 9- ^ e1; ramethyl" -5- "Cl © cin- ^{/ i>} » 7 "" oil, polyoxyethylemionooleate, lauryltrimethylaMttoniiimohloirdj ündecylimidasoloa, lauryldimethylbenzylammonium chloride ₉ Polyoxyäthylst © arylas-mono-acidic acid isopropyl acetate / Acrylic acid copolymers, ethoxylated diamines, long-chain amine oxides of the formula

Hydroxybutyramides, quaternized vinyl pyridine polymers and quaternized yinylpyridine / yinylpyrrolidone mixed polymers, and phosphate esters of that described in U.S. Patents 3,004,056 and 3 004 057 and in Belgian patent specification 641 097 " 3? Yps.

^{The phosphate esters of the} type described in the above patents can be prepared by reacting 1 mole ^ 2 ⁰ 5 ^mi * ^{2 tis} ^ * ^ Mo1 of a nonionic surfactant having the molecular configuration of a condensation product of at least 1 mole of ethylene oxide with 1 mole of a at least 6 carbon atoms and one reactive

A09830 / 0789

In the process, no excess of the organic hydroxyl compound (in this case the defined nonionic surface-active agent) need be used to bring the? 2 ° 5 ^ ¹¹ ^ suiiS. It is practically not formed tertiary Phosphatester and there remains little or no ^ 2 ^ 5 ^ ¹¹ ^ ^ ^he usamiaensetzung. Depending on the particular ratio of 2Pp ^ ¹ S ^{to the used} nicate-ionic surfactant and the nature of that nicate-ionic surfactant, the product may in some cases contain some non-used, nonionic surfactant, for certain For similar reasons, the proportions of secondary phosphate ester on primary ester to free nonionic surfactant in the products thereof are generally within the range of about 20 to 4-5% by weight of secondary phosphate esters to about 30 to 80 G-ew .- ^ priaar-e :? Esters at about 0% by weight nonionic surfactant.

Lighter colored or practically colorless products are obtained when the phosphatization reaction is carried out in the presence of a small or catalytic amount of a phosphorus-containing compound from the group of hypophosphorous acid, the salts of hypophosphorous acid, phosphorous acid and the salts and esters of phosphorous acid. The process consists in that 1 MoIP ₂ Oc with 2 to 4 _S 5 moles of a nonionic surfactant with the molecular configuration of a condensation product of at least 1 mole of ethylene oxide with 1 mole of a compound containing at least 6 carbon atoms and a reactive hydrogen atom under practically anhydrous Conditions and at a temperature below about 110 ° C in the presence of a small amount of one or a mixture of the above

409830/0789

Reacts under phosphorous acid or phosphorous acid compounds.

By using these compounds in the phosphating reaction described, it is possible to achieve an unexpected and considerable improvement in terms of the (lack of) color of the products and in terms of the resistance of these products to discoloration on storage erv / extension of these compounds are obtained in general VÖS have ~ values (varnish color scale, Gardner scale, default values of 1933) that ism are at least 1 lower than those of the products in the same process in the absence of Hypophosphorigsäure- or phosphorous acid compound. In this way, products with a x * VCS-2? ar "of about 1 or less can be obtained, compared to VGS paints of about 2" to about 7 or more for products ₉ that lie without .Application the goal invention have been made "Besides, has inclined _s that the ex'finaungsgemäßen products to discoloration or · Ifeehdui'.kelungen se l are stable even after 3 to 6 months of storage «

The nonionic surfactants used as reactants are known per se and are described together with suitable ancestors for their preparation ia numerous patents and other publications. They can generally be prepared by condensing a polyglycol ether having the required number of alkenoxy groups, or Alkylene oxide, such as propylene oxide, butylene oxide or preferably ethylene oxide, with an organic compound containing at least δ carbon atoms and a reactive hydrogen atom * Examples of such compounds ₅ which contain a reactive hydrogen atom are alcohols, phenols, thiols ₉ primary and secondary amines as well as carboxylic acids and sulfonic acids and their amides. The amount of alkylene oxide condensed with the reactive chain or

409830/0789

Equivalents thereof depend primarily on the particular Connection with which it is condensed. As a rule of thumb, use such an amount of alkylene oxide or its equivalent of which should be used, which leads to a condensation product which is about 20 to about 85% by weight bound Contains (combined) alkylene oxide. The necessary to achieve the desired hydrophobic-hydrophilic balance The optimal amount of alkylene oxide can easily be determined in each individual case by simple preliminary tests.

Bei.den nonionic surface-active agents which have the molecular configuration of a condensation product of at least 1 mole of an alkylene oxide, preferably ethylene oxide, with 1 mole of a compound containing at least 6 carbon atoms and a reactive hydrogen atom, are generally preferably polyoxyalkylene derivatives of alkylated and polyalkylated phenols, multi-branched primary aliphatic alcohols with the molecular configuration of an alcohol prepared by the oxo process from a polyolefin with at least 7 carbon atoms and straight-chain aliphatic alcohols with at least 10 carbon atoms. Examples of these derivatives and other suitable non-ionic surface-active agents which can be phosphated according to the invention are given below. which have been reacted with 1 mole of the specified, reactive hydrogen-containing compound: Nonylpheno1 + 9-11 EO,! Tonylpheno1 + 2 EO, dinonylphenol + 7 SO, dodecylphenol + 18 EO ·, castor oil + 20 EO, 0? all oil + 18 EO , Oleyl alcohol + 20 EO, lauryl alcohol + 4 EO, lauryl alcohol + 15 EO, hexadecyl alcohol + 12 EO, eexadecyl alcohol + 20 EO, octadecyl alcohol + 20 EO, oxo-tridecyl alcohol: (from tetrapropylene) +7 E.0., (From tetrapropylene) +10 EO, (from 2? Etrapropylene) + 15 EO, dodecyl mercaptan + 9 EO, soybean oil amine + 10 EO, hosin amine + 32 EO, coconut fatty acid amine + 7 E.0. _t cocoa fatty acid + 10 EO, dodecylbenzenesulfonamide + 10 EO, decylsulfonaraid + 6 E.0 _r , oleic acid + 5 E.0 _ff ,

409830/0789

Polypropylene Glycol (30 Oxypropylene Units) +10 E.O.

In carrying out the phosphating reaction, the PpDj is gradually added to the nonionic surfactant in liquid form, preferably with vigorous stirring. If the latter agent is solid at room temperature, it should be heated to a temperature above its melting point. The addition of the nonionic surfactant to the PpOc ^ ³ ^ is not advisable as this has been shown to lead to the formation of tar and the like and thereby prevent the reaction from proceeding to completion. The reaction is exothermic and in some cases, cooling is required to prevent the temperature rises above 110 ⁰ C addition, because this leads to Bildimg of discolored and nachgedunkeltem products. The reaction proceeds continuously during the addition of the PpO ₁ - and the dissolution of the same in the nonionic surfactant and is at the point in time at which all of the PpO 1 has been added, essentially 90 % or m © ks? finished «The few particles. of solid PoOc ₉ remaining in the reaction medium ₉ can be removed at this point in time "if time is important - from an economic point of view, however, it is advantageous to continue the reaction for a further period of time within the range of 1/2 to 5 hours or is at ambient temperatures can be more until zm about 11O ⁰ G proceed to ₉ can be dissolved until all PPOC, which indicates a complete reaction between the reactants. A strong stirring during the reaction is highly desirable to facilitate the completion of the reaction and to accelerate · An advantageous feature is that the ^ 2 ^ 5 * ⁿ * ^roc3cener "solid particulate as a granular powder or other finely divided or Form can be used for reaction with the non-ionic surfactants defined above, if necessary

409830/0789

however, the Pq ^ c can first in an inert organic Diluents, e.g. benzene, xylene, ether, pentane or in low and high boiling hydrocarbon fractions.

After the reaction has ended, the reaction mixture can be cooled and discharged. If it is carried out under strictly anhydrous conditions, the product should be off a mixture of the primary and secondary phosphate esters of the bound nonionic surfactant consist, depending on the proportions of the reactants, in in some cases with a small amount of unreacted non-ionic surfactant. Any small amount of water present in the reaction mixture inevitably leads to the formation of some phosphoric acid in the product · The degree of esterification in the product can poten « tiometric elimination or by titration with alkali against Methyl orange and da2: “^ egen Plieno! Phthalein can be determined.

The products can be in free, non-esutralized form or in the form of partially or completely neutralized salts, which are cations of alkali metals, alkaline earth metals, metals, Containing ammonium and organic amines. Of course, these salts are to be regarded as equivalent to the products according to the invention in their free form. Examples of suitable cations are 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, e.g. the mono-, di- and tri-methylamines, -Athylamine, -Propylamine, -Laurylamine, -Stearylamine, -Ethanolamines, -propanolamines, -Butanolamines, -hexanolamines, -Cyclohexylamine, -Phenylamine, -Pyridylamine, -Morpholinylamine and the like

If desired, the above-mentioned products can be added by adding

409830/0789

a small amount of a hypophosphorous acid or phosphorous acid compound to be modified to the reaction medium. In general, from about 0.01 to about 5 %, preferably from about 0.1 to about 2% of this compound, based on the weight of the nonionic surfactant to be phosphated, is sufficient to provide the desired improvement in preventing discoloration of the To achieve products and to improve the resistance of the products to discoloration during storage. Hypophosphorous acid and its alkali metal salts, ZcB. their sodium and kaldun salts are generally preferred, although other metal, alkaline earth metal, ammonium, or amine salts of hypophosphorous acid or phosphorous acid can be used in addition to phosphorous acid per se is used, it is preferably in 3? orn a 30 to 50% aqueous solution. Solution is used, although aqueous solutions of this acid and other water-soluble eypophosphorous acid and phosphorous acid compounds can also be used in the form of aqueous solutions, the concentration of which is within the range of less than f> up to ¹ % or more. It should be remembered that the reaction should be carried out under practically anhydrous conditions and that accordingly the water introduced with these solutions should be kept to a minimum. The salts of hypophosphorous acid and of phosphorous acid used here can be in hydrated or dehydrated form. Examples of such salts are aluminum, cadmium, sodium, potassium, lithium, calcium, strontium, barium, magnesium, ammonium, mono-, di- and tri-methylamine, ethylamine, Propylamine, ethanolamine and »propanolamine, pyridinyl and morpholinyl phosphites and hypophosphites. Phosphorous acid esters can also be used. These esters can be mono-, di- and tri-alkyl, aryl and cycloalkyl phosphites. It will be understood that mixed esters can also be used. Some specific examples of such esters, in which the esterification group generally contains from about 1 to about 20 carbon atoms, are ethyl phosphite, lauryl phosphite,

409830/0789

Oxo-tridecyl phosphite (the esterification alcohol has the molecular configuration one of tetrapropylene or triisobutylene alcohol prepared by the oxo process), stearyl phosphite, phenyl phosphite, cyclohexyl phosphite, the corresponding di ~ and fcrisubstituted phosphites, ethylphenyl phosphite, ethyldiphenylpho sphite, laurylcyclohexyl phosphite, dipropylphenyl phosphite and the like. The hypophosphorous acid or phosphorous acid compound is preferably mixed with the nonionic surfactant before adding it to the nonionic surfactant. It is therefore clear that the hypophosphorous acid or phosphorous acid yer - bond or a mixture thereof at the beginning of the reaction or continuously or intermittently as the reaction proceeds Reaction can be added

The examples given in the following table are intended only to illustrate the invention, but not to limit it. In each of these examples, the nonionic surfactant was first introduced into a reactor equipped with a stirrer. When the charge was solid at room temperature, it became heated to sinew them. The additives indicated in the following items were then added and dissolved in the non-ionic surfactant with vigorous stirring usually introduced within about 15 minutes in the, reactor "After the anfängliehe exothermic reaction had ceased, the Heaktionsmischung was erhitat to 10O ⁰ S and held at that! temperature for about 5 hours, after which the mixture imrde cooled and discharged · A Sample of the reaction mixture was titrated with alkali against methyl orange ii & d then against phenophthalein as a control for the esterification. The YCS color values were measured in the prescribed manner. A value of 1 is the lowest measurable color value according to this method, the highest value is 18i The using

409830/0789

the additives indicated in the following table Products showed no color change after storage for 3 to 6 months · Preference is given to the monoesters, the Diesters and the mixtures thereof

409830/0789

Table A.

At the same time ionic

Nonylphenol + 2 E.O.

Honylphenol + 4 E.O.

E, O.

If
M.

E.0 _e

10, - ■ ■ "

Konylphenol + 100 ^ E.O.

"

Dinonylphenol + 7 E «0 ·

Dodecylph.enol + 6 EO
^C 12 ^E 25 ^C 6 ^H 3 ^(0G 2 ^H 4 ⁾ 6 ^OH

Parts of the not »ioni ~ see.Agen Share parts

used addition

VOS-Parbe

2,888

2 288

2,855

2,855

1 821

1 821, 605

605 327

327 1,052

1 052

284 Control - ... 2

284 3.4 hypophosphorous acid (50%) <1 213 control '

213 4.2 Hypophosphorous acid (50%)

47.3 control -, 4

47.3 "IfO hypophosphorous acid (50%) <Λ

47? 3 0.5 sodium hypophosphite <1

47.3 2.0 triphenyl phosphite 2

103 Control - '4

• Ί08 7.0 Uaterphosphorous acid (30%),
11.9 control - 2

11.9 1.2 hypophosphorous acid (50%)
23.6 control. - · 5

23.6 1.0 Hypophosphorous acid (30%) <"\ 94.4 Control - 4

94.4 3.0 hypophosphorous acid (50%) <1

co

Continuation of τοπ table A

1 I. 17th 1
Oxo-sideeyl alcohol +
3 SO O 18th SS 9830 / 19th If σ 20th Lauryl alcohol + 4 E.O. * 21 Il

166 166 7? Λ

724

made from ^ etrapropylea naeb.

23.7 control - 7th

23 s7 1 * 0 hypophosphorous acid (50%) 2

23.7 1.0 Phosphorous acid x 2

71 control -. 7th

I ₉ S Hypophosphorous acid (50%) 1

s £ 9> «ir @ rfahr @ n.

A suitable quaternary ammonium compound can be represented by the following general structural formula

R -

Γ T

R ¹

R ¹

where E - (CHT) _n -UH ₅ with η - 6 to 26, R "and R '- (CEY) _n -CH, with η = O to 6. The alkyl radical can be branched or straight-chain and Y is hydrogen or an alkyl group as defined above, R "and R * need not be the same.

The quaternary ammonium compounds can be prepared in a manner known per se, for example by dissolving. 1 mol of dimethyistearylamine in isopropyl alcohol, subsequent addition of 1/2 mol of diethyl sulfate by means of a separating funnel, the temperature being kept below 50 ⁰ G, after which the exothermic reaction stopped after the addition of the last diethyl sulfate, refluxed for one hour and cooled and the Alcohol is evaporated. Examples of preferred quaternary ammonium compounds are those compounds in which R ¹ and R "denote lower alkyl; compounds in which R * or R" denote methyl are particularly preferred. R can be a saturated or unsaturated C ^ 2_> tg-Sest, ie a. Cocoa, stearic, oleic acid residues and the like. Be.

In the case of the quaternized copolymers specified, it can are those in which the monomeric compounds are first copolymerized and then quaternized, or those in which the monomers are first quaternized and then copolymerized. To carry out the above specified methods can be used methods known per se will.

"409830/0789

In the case of the quaternary copolymers used according to the invention it concerns those, soft the following specified unit I and either the unit II or III or all three units:

II ^m

ch

^CH 2t: -

—'N

CH ₂ C

m
O

I © €

O-R2 -N (R3) 2- ^R 4 ^X

where η 40 to 90 mol%, m 10 to 60 mol%, ρ 10 to 60 Mol% and η + m or ρ or η + m + ρ »100, E ^ H or

CH ₂ CH-CH ₂ or

OH

CH,

C ₂ H ₅ ,

where χ = 2-18, E ₇ , X Cl, Br, J, SO ^,

CH, or

CH ₂ SO ₂ and M is a monomeric unit that consists of

3 3
Heteropolymerisation under Verwendung'eines of η different and copolymerizable Monoviny! Monomeric · M 5 can mean up to 40 if ρ 0 $ 0 rock, the latter occurs when n, m and ρ be applied all results ·

As indicated by the above formula, these quaternary copolymers can be prepared by copolymerization of an N-vinyl lactam, such as N-vinylpyrrilidone, with di-lower alkylaminoalkyl (or hydroxyalkyl) acrylate or methacrylate and optionally a further monovinyl monomers different from η and thus copolymerizable. According to the invention, the monomers are copolymerized in such a way that, based on 100 mol%, the vinylpyrrolidone units 40 to 90 mol% of the di-lower alkylaminoalkyl

409830/0789

(or hydroxyalkyl) acrylate or methacrylate derived units 10 to 60 Hol- # tmd from the. further, so units derived from copolymerizable tinyl monomers also make up 10 to 60 mol%.

Suitable heterocyclic li-vinyl lactams have the general formula

I ₁ - CH

C = O

:H -

wherein R is a to complete a 5-, 6- or 7-gene heterocyclic hanging system required alkylene bridge grouping with 2 to 4 carbon atoms, and ILj either hydrogen or a lower alkyl group and η is an integer of at least 3

All of the specific polymeric materials characterized by the above general formula are commercially available and are referred to as polymeric N-vinyl lactams · They will obtained by polymerization of organic 5-i 6- or 7-part devoted people who in their hangings the -HH-CO group, such as:

II-vinyl-2-pyrrolidone _s H-ViBTl-2-piperidone,! F- ¥ i2i3rl-2-caprolactam, H-finyl-J-methyl-pyrrolidone, if-vinyl-3-ethyl-2-piperidone or H. - ¥ inyl-3 - jaethyl-2-caprolactam, H-vinyl-4-methyl-2-pyrrolidone _f B-vinyl-A-methyl ^ -piperidone or H-vinyl ~ 4-methyl-2-eaprolactam, H- Vinyl-5-methyl-2-pyrrolidone, lί-vinyl-5-βethyl-2-piperidone, U-7ynyl-3-a.thyl-2-pyrrolidone, H-Vii ^ i- ^ j ^ diiaethyl ^ -pyrrolidone, H-vinyl-5.5-

40983Q / 0789

. 24Q1221

dimethyl-2-pyrrolidone, N-V5jiyl-3 _s 3, i ^ trimethyl-2-pyrrolidone, Xmrinyl- ^ methyl- ^ ethyl-2-pyrrolidone, N-vinyl-3,4,5-trimethyl-3-ethyl-2 -pyrrolidon, li-vinyl-6-methyl-2-piperidon _f N-vinyl-ö-äthyl ^ -piperidon, N-vinyl-3, 5-dimethyi2 ~ piperidon, N-vinyl-4 -, ^ - dimethyl ^ - piperidone, lί-vinyl-7-methyl-2-caprolactam, K- ¥ inyl-7-ethyl-2-caprolactam,. K-vinyl- ?, 5-dimethyl-2 ~ caprolactaEi, ÜF-vinyl- ^ je-dimethyl ^ -caprolactam and N-vinyl-3,5,7-trimethyl ~ 2-caprolactam.

Among these various compounds is the N-vinyl-2-pyriOlidone most 'preferred because it is readily available and provides products with excellent properties «

Böispie3.e of suitable Diniedrigallsylaminoalkyl (or Hydroscy "alkjrl) acrylates or methacrylates are the following compounds: Mraethylaininomethylacry3.at, Diiaethylaminomethylmethacrylat, Diäthylaminomethylacrylat, Biüthylaminomethylmethacrylat _s dimethylaminoethyl, Diiaethylaminoäthylmethacrylat, Biffiethylamino-2-hydroxy-propyl acrylate, Bimethylaraino-2-hydroxy-propyl methacrylate, 2) iäthylamino-2-hydi'oxyäthylacrylat, di äthyloj £ ino-2-hydro ^ ethylmethacrylate, Dimethylaniinobutylacrylat, dimethylaminobutyl methacrylate, Dimethylaminoamylmethacrylat, Diäthylaminoamylmethacrylat, Dimethylaminohexylacry-1at, Diäthylaminohexylmethacrylat, Dirnethylaminoοctylacrylat, Dimethylaminooctylmethacrylat, Diäthylaminooctylacrylat, Diäthylaminooctylmethaerylat, Dimethylaiainodecylmethacrylat _s Dimethylaminododecylmethacrylat, Diäthylaminolaurylacrylat, Diäthylaminolaurylmethacrylat , Dimethylaminostearyl acrylate, dimethylaminostearyl methacrylate, diethylaminostearyl acrylate, diethylaminostearylm ethacrylate and the like, with the hydroxy-free alkyl units being preferred.

The monovinyl or vinylidene monomer represented by M in the structural formula above can be (any conventional vinyl monomer include, which is copolymerizable with H-yinylpyrrolidone is »Examples of suitable common vinyl monomers are the alkyl vinyl ethers, such as methyl vinyl ether, ethyl vinyl ether, octyl

409830/0789

vinyl ether and the like; Acrylic acid and methacrylic acid and the esters thereof, e.g., methacrylate, methyl methacrylate and like »; vinyl aromatic monomers such as styrene, α-methylstyrene and the like «; 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, and the like. Again, it should be noted that this copolymerizable vinyl monomer 3, which may comprise conventional vinyl monomers, init N-vinylpyrrolidone is copolymerizable and that if a Terpolymer is produced with both units η and m is copolymerizable and different from both.

The quaternized copolymers preferably used according to the invention can therefore be characterized by that they have a repeating structural unit which is derived from

(A) 40 to 90 mole percent vinyl lactam,

(B) 10 to 60 mole percent of a di-lower alkylaminoalkyl acrylate or ^ methacrylate or a di-lower alkylaminohydroxyalkyl acrylate or methacrylates or

(0) 10 to 60 mol% of one different from A and B and hence copolymerizable vinyl monomers.

These copolymers are expediently prepared by adding a solution of vinyl lactam and amino acrylate or Aminomethacrylate monomers with or without a vinyl monomer optionally copolymerizable therewith such conditions which lead to vinyl polymerization at the double bond. The polymerization can, for example, be appropriate initiated by the action of free radicals, the polymerization once initiated is, exothermic. Examples of suitable free radicals. 1-

409830/0789

Catalysts which are commonly used and are suitable for the production of the copolymers are organic and inorganic peroxides, for example hydrogen peroxide, t-butyl peroxide and the like, aliphatic azo compounds, for example azobisisobutyronitrile, and other free radical-forming catalysts, such as those in the field of Polymerization are known per se «, The polymerization is preferably carried out in solution at temperatures which ^{vary from about 50 to about 10O 0} O or more, but in order to avoid" runaway conditions "and to obtain a copolymer with the desired molecular weight, it is sometimes it is preferred to carry out the copolymerization at a temperature of about 75 to about 85 ° C

As stated above, the copolymers are in the form of their quaternary salts. Therefore, the polymer after completion of the polymerization reaction, a heat treatment subjected to the quaternization of the tertiary amino group using a common quaternizing agent. Examples of suitable quaternizing agents are, taking into account the above structural formula for the copolymers * Dimethyl sulfate, diethyl sulfate and the like; Alkylsulfonic acid, such as methylsulfonic acid, ethylsulfonic acid and the like; Benzyl halides such as benzyl chloride, benzyl bromide, benzyl iodide and the like; Alkyl halides and the like. For the preparation of those used in the coating compositions according to the invention Any quaternary N-vinylpyrroJLidon copolymers can be used Customary quaternizing agents can be used with advantage · The molecular weight of the quaternized copolymers should be between 800 and 50000.

* D.ialkylsulfate, such as

409830/0789

Suitable sulfonates and sulfates of metals of groups IA, IIA and IIB of the Periodic Table of the Elements can be represented by the following general formulas: 1. Alkylarylsulfonates (e.g. Kaccanol 402B)

2 · Alkylbenzenesulfonate -nf ^ X on -α η · + " KHU / ~ övJ, n R is

H η is O200

3. linear sulfonates R-C-SO ^ H (e.g. Nansa HS-55, i.e.

Λ * * sodium lauryl sulfate)

RistCH,

4, Thoxylated alcohol sulfates -_ (z: B * lAlipals); ..

H
EOO -i CH ₂ -CH ₂ -O) _n SO ₃ H η »1-1000

H -

5 _# sulfonated esters

R- - C = C-R'-C ^ ⁰ _{+ S0} H ₂ O

HH - ^

, SO ₃ HH ^ O ^Vfl H ^ OR "R is ^: CH ₃ - (CH ₂ ^ y _{1 n =} 2-14

R ¹

R »iiit - (CH ₂ ^ _n CH _{3 n =} X ^ ₃₀

6. Alkylnaphthalene sulfonates (e.g. Nekal BA-75)

7. Igepon A 0

RC -0-CH ₂ -CH ₂ -SO ₃ Na

8. Igepon T

R ¹ RC-ä -CH2-CH ₂ -S03Na

0 Γ. (where E, E * and R "denote alkyl ~ or aromatic groups)

4,99830 / 0789

Of course, any of the above components can be used in place of the alkoxylated tertiary amine the moistening agent (and if necessary, der'Elektrolyte) must however be used in connection with it will.

Particularly preferred antistatic layers are those on Base on alkoxylated tertiary amines of the following general formula

/ (CHR ¹ -CHR ¹ -O) _n H '

RN

^ (CHR ¹ -CHR ¹ -O) _n H

where R is an aliphatic hydrocarbon radical with about 8 to about 22 carbon atoms, R ^{1 is} each hydrogen or methyl and η is an average whole number of at least 1, preferably from about 1 to about 50, although if desired also more highly alkoxylated derivatives, ie the Products can be used which are obtained by condensing 1 mole of a primary aliphatic (saturated or unsaturated) amine with up to 50 moles of an alkylene oxide, usually ethylene oxide. Such alkoxylated amines are known per se and are prepared by condensing the primary saturated or unsaturated aliphatic amine having 8 to 22 carbon atoms with an alkylene oxide, usually ethylene oxide, although propylene oxide and butylene oxide can also be used, if desired, until glycol groups with the desired chain length are obtained have been. Such products are described, for example, in U.S. Patents 1,970,578, 2,171,762, 2,510,284 and 2,595,466.

As wetting agents in the coating composition according to the invention various deliquescent salts of metals in groups I and II of the Periodic Table of the Elements, especially the alkali metals and alkaline earth metals can be used. Specific deliquescent salts, which are preferred as

409830/0789

Moistening agents used are the alkali metal salts of lower aliphatic carboxylic acids, such as sodium formate, potassium formate, lithium formate, cesium formate, Sodium and cairum acetate, calcium butyrate, and mineral acid " salts, such as calcium chloride. Organic humectants such as glycerine, urea, ethylene glycol, Sorbitol, ethoxylated sorbitol, lauric acid ester and mixtures of which, can be used.

It is clear that when a deliquescent salt is used as a moistening agent, it can also function as an electrolyte. However, when glycerin or other non-ionic humectants are used, they should be combined with an electrolyte. In the case of using deliquescent salts, such as sodium and potassium formate, which have a relatively low dissociation constant, it is preferred to use a small amount of a salt of a strong base and a strong acid with a high dissociation constant, such as sodium chloride, Potassium chloride or calcium chloride, to incorporate salts _{that are not sufficiently deliquescent, such as sodium chloride, sodium sulfate s} potassium nitrate, so that they do not function in a completely satisfactory manner as both a humectant and an electrolyte, can in combination with a non-ionic humectant such as glycerin or Urea, or in combination with a more deliquescent salt such as potassium formate or calcium chloride. In the coating composition according to the invention, the wetting agent and the electrolyte can therefore be either a single compound or a mixture of compounds.

If desired, a further underlay (reinforcement), such as a jute reinforcement, as shown in the drawing with the number 10, applied to the latex coating However, this is not an essential element of the carpet structure according to the invention. The invent is img by

409830/0789

the following specific examples explained in more detail without however, to be limited to that. The parts, proportions and percentages given therein relate to unless otherwise stated, by weight. Examples ... .1-, 1JZ

In these examples, the antistatic coating composition made by adding the base and organic acid to water to make the humectant in situ. It was the alkoxylated alaine used stearylamine., which contains 20 moles of ethylene oxide per mole of amine had been ethoxylated. The antistatic coating composition thus produced can, if desired, be thickened by means of a known thickening agent such as sodium polyacrylatef Methyl cellulose or the like., Modified. A pH adjustment down to a range of about * 7 to 13 can be used in certain cases also be desirable if a lower tendency to migrate and a higher degree of flammability are desirable * If a wetting agent is used, it can be (dridecyl alcohol, which contains 6 mol Ethylene oxide has been ethoxylated per mole of alcohol.

In all cases the anti-static coating was on the underside the latex precoat layer was applied, the latter was applied on the back of a tufted carpet with a loosely woven one Primary jute underlays applied and those in the tufted Fibers used in pile are as well as the amount of antistatic applied to the underside of the precoat layer Indicate the coating mass in the following table on the left. After the antistatic coating was applied, the carpet was dried to remove excess moisture. A latex coating was then applied to the antistatic coating. The one used in these examples The test procedure was the AATG

409830/0789

j .nf sealants Part organ. ßaure Part 60 46 • ie- "Part Tabel NaCl I. 2 Part Acid pH carpet Coating I 1 , in g / m He- • "basi le acid ti le 23 Ie le ■ - le or fiber Gew, j Il ' , per sq..yd.) , «■■■) · sch 60 23 Amin Elec- NaCl Part 2 What Eäse (oz. : j Sr * Ver Araeisen-46 60 tZ'O- NaCl le 2 ser for pH ";
I>' bind. acid Netz- lyte Once el ti 36 j Il 60 ' with NaOl 2 lung; i i (5) j 40 macaws ■ 56 W. 74 20th tel 210 'Vinegar- 6.5 acrylic • JI70: 'P 70 j Λ NaOE ti 74 NaCl 2 acidic I 1";
ί ' 40 56 vinegar Ants-56 20th 2 NaCl 2 210 it; .1 polyester i-! (136; ί I 2 NaOH 40 Asian iron-56 acid acid 20th 210 Ants-i " Polypropy! "i 1204; \ I - 3 NaOH acid Il 2 NaCl 2 acid · j 'len I.
ι i
t ; . j • ί
ο 40 vinegar H 20th 2 KGi 1 210 ■■ "ν" J ₉ : Nylon '·· " I ·, { IO 4th NaOE acid dd KCl 1 . . · 17Ο; j; OO
co 40 Il 20th 2 NaCl 2 210 "· 6.5 Wool ¹ ti,
I,
j: (4) ) CD 5 NaOE 56 20th 180 ι
Il - Q nylon I «
! ■ 1 '■ !
! 1 "• Ν.
O 6th EOH / 2 NaOl 2 I. 1
! ; C5) {·. 56 20th 2 'NaCl 3 180 Vinegar- 6.5 Wool I j OO
tf ~ \ 7th EOH 20th 10 ITaCi 3 150 acid. _{according to} nylon (4); UJ ■ s NaOE 20th 10 · 2 NaCl 2.5 150 Ants- '. " Wool is); 9 NaOE 56 20th 1 . . . 200 acid. ,,
Il j nylon 10 KOE 1 i 'M ■ to 56 20th 1- 200 Il Il Wool <5) | S. 11 EOH 56 25th 500 ti,: it
j nylon 12th KOS 56 25th 1· 5OO Il! Il Wool I ro 13th KOH 69 25th 1 245 I! ί " nylon ί ί 14th KOH .1 ί
1 , 2

Continuation of table I.

15 EOH 69 Ant 56 25 .2 ^ ^{51 01 2} ί5 24-5 Aneisen- 6 _V 5 Polyester I70 (5)

satire _ acid

16 ¹ ; Acrylic.

"Polypropylene *

Il TI

CO CO OO O "» Sy

O OO

to

uiibehan & eld control sample

ro

Table II ^ Electrostatic results according to AATC 154-1969

^: ■ "after the steam

; At- before the RexnifsunR I. PP
No. Chrome leather lieolite ι
]
I.
I. 1 +100 volts: -100 volts ί 2 -250 -250 .3
4th -100
-800 -100
-400 * ■>
CD
to
OO 5 -100 + 200 ίΟ / 0 6th
7th -500
400 -800
600 00
to S. 300 500 9 200 300 10 800 1,000 11 600 700 12th 200 800 13th 400 1,200 14th 600 400 15th 800 600

Chrome low +450 volts +400 +200 -1,200 -400 -1,000 400 800 600 1,400 800 600 1,400 810 800 lieolxte

+500 volts

+600

-150

-600

-600

-1.200

-400

1,000

800

900

600

800 1.100

950

500 control - none

treatment
Chrome leather Neolite

■ 10 to 11,000 volts-4 to 5,000 volts

+ 7,000 _c +2,500

+ 6.500 -2.000

9,000 7,000

-12,000. -8,000

CD

ro

Examples

In these examples, the treated samples were carpet structures tufted with nylon and wool, In all cases the antistatic coating was applied to a latex pre-coating sheet and dried then a latex coating was applied to the antistatic coating brings. In these examples the humectant was prepared in situ by reacting a basic component with an acidic component. The test procedure used was the same as in the previous examples.

The composition of the antistatic coating and the Results obtained in this test and other important information for these examples are given below Table III given «,

409830/0789

'Humectant i , 27 "basi Part organi- part acid 60 (liex- Part Table III ■ • carpet Coating University 5 ^s - I. N) At- ! 28 sch le Sche le It Ie le Part Partic acid 'pH fiber w. in g / m < 5 VM CD sp. Ver acid Propion 60 Amine network Elec le Ie or base Qos / sq..yd.) I. ro No, I.
I i bind, acid 46 with tro Was- snr pH- Ni I ²⁹ I. ti tel lyt this setting , · Ϊ30 NaOH 40 vinegar Ants 46 20th 2 lung nylon 136 '; (4) , ίΐΊΓ ~ acid acid 23 2. 210 vinegar- 6.5 i • NaOH 40 ti It .23 20th 2 NaCl acid ) Wool j 19 KOH 56 Ants vinegar 60 20th 2 2 210 "'.» nylon η 'j j ■ Ο
(O ! 20 acid acid NaCl 2 180 ants'" y y 00 KOH 56 Il 60 20th 2 NaCl acid j Wool O NaOH 20th ⁰ 74 10 1 2 180 "» nylon 204: (6) "" Ν. NaOH 20th η 10 1 NaCl 1 15QEriäthap.pl-9 Wool tt ,: O ! 1 KOH 56 vinegar 74 20th 2 KCl 1 I5O "". w nylon 136 "(4) CD
CO '21 56 KCl 1 200 acetic acid, 5 I. j 22 KOH 56 20th 2 NaCl re ^; Wool ti ';''
1 KOH 56 56 25th 2 1 200 "! N. nylon η 'I 60 'NaCl 3 5OO ants; " . I.
I. [23 KOH 56 25th 2 NaCl. acid \ Where]. Ie 'ti · Ι i i 24 KOH 69 25th 3 .3 500 "i it nylon 204; (6) I ι NaCl 2.5 2 ^ 5 Mo ^u rpholin | 9 i KOH 69 25th 3 NaCl I. Wool 29% 121 20th 2 2.5 245 "η nylon NH4OE NaCl 2 200 NH ₄ OH '" 25th NaCl 26th "Yy: ti i!

Continuation of Table III

31, 29 % 121 Ant 46 20th 2 ITaOl 2 200 KH.OH KH ^ ,OH acid 32 29 % 121 Propion 74 20th 2 HaOl 2 400 ti KH ^ acid 33 '

untreated control

9 ffylon 204 ^Λ (6) i5 "136 (4)

n.

Wool

"· - 36 -

Table IV

electrostatic results according to AATC 134-1969

At- before the cleaning after Steam- Neolite sp. Chrome leather ' Meoiite cleaning; -14C0 Mr. Chrome leather -1400 18th -2000 -1300 1500 200 19th -2000 -1300 ' 1500 1200 20th - 500 - 500 300 800 21 : -1300 -1400 -1100 1100 22nd -1000 -1100 500 1300 23 -1700 -1300 1500 1000 24 -1300 -1200 ^; 1200 1100 25th -1300 -1200 7000 1900 26th -1700 - 900 1500 900 27 -1700 -1800 1600 1200 28 -1200 -1200 800 3,200 29 -1800 -1300 1500 950 30th - 700 -1100 900 850 31 '-1100 -1200 800 5200 32 -1200 - 900 1100 6200 33 -7000 -4200 11000 34 -17000 -5400 9000

409830/0789

Examples 35-4-9

The samples treated in these examples were carpet structures tufted with HyIon and wool. In all cases the antistatic coating was applied in the same manner as in the above examples. In these examples, the humectant was not made in situ, but was added directly to the antistatic coating composition. In Examples 41 through 44, the calcium chloride functioned as both an illuminating agent and an electrolyte.

The composition of the antistatic coating as well as the results obtained in the test and other important ones Information for these examples is given in Table V below.

0 9830/0789

Table V

At- moistening sp. middle
No.

Ie

Partly amine wetting agent

Elec- Tel- ¹ SeI- trole le
lyt 'what.

s he

Sorbitol ester CaOl ₂

CaCl ₂

CaCl ₂

CaCl ₂

CaCl ₂

CaCl ₂

CaCl ₂

CaCl ^

10 20 20 20 50 30 30

CaCl

urea

CaCl ₀

40 40 10 30

30th

20 20 20 20 20 20 20 20 20 20 10 ³ OK

1 NaCl 1 70

2 - (2) 100 2 - (2) 100 2 ~ (2) 100 2 - (2) 110 2 - (2) 110 2 - (2) 110 2 - (2) 120 2 - (2) 120 2 - (2) 120 1 CaCl ₂ 10 100

1 NaCl 1 110

2 - (2) 100

Acid, od · pH carpet Besehichtungs Base "for fiber. Wt. In g / m pH Einstel- ςοζ / sq.yd ·) lung _t '

Acetic acid 6, "5 I nylon; 17O;, (5>

Formic acid

Acetic hairs

π π > ti f It U i '» Il Wool 'tt ti nylon » It ti. dd It Wool dd ti nylon 'It π Il It Wool Il It nylon It

1
ethoxylated sorbitol lauric acid ester

"" the humectant was the electrolyte ^ N-Octyl-N-ethyl-morpholinium ethosulfate

quaternary diethyl sulfate imidazoline '' non-treated control robe II

It

Ii j

'- 39 -

Table VI

-electrostatic results according to AATO 134-1969

At-
sp.
Hr> before ± c iieolite Chrome leather 35 Chrome leather 2200 1800 36 1700 2100 1600 37 1800 3200 2800 38 2600 . 2810 2900 39 2700 2600 2600 40 ' 2500 3 * 00 3200 41 2900 2900 3400 42 3100 3400 3200 43 3400 2,700 2400 44 2800 2600 3300 45 3200 3200 2900 46 3100 2600 2800 47 2500 - 3500 3400 48 3300 3200 2500 49 2800 6500 12200 50 11000 5500 9200 ^: 9500

Chrome leather HeöTrbe after steam cleaning

2100 1900 3300 3200 2400 2800 3200 3600 2800 2800 3500 1600 3200 3000 6700 5400

4 0 9830/0789

Examples 50-78

The samples tested in these examples were conventional woven and non-woven fabrics. In all cases the antistatic coating was applied and dried to remove excess moisture. In these examples the humectant was prepared in situ by reacting a basic component with an acidic component as in Examples 1 to 18. In these examples the following procedure was used: The samples were cut and first covered with a latex backing and then with the antistatic coating Mistake. In these examples the coating weight is based on the weight of the fabric in question. Then, a polymeric substrate (gain) was applied to the fabric and dried to about 30 minutes at a temperature of about 93 to about 163 ° C (200-325 ⁰ F for a period of about 10 degrees. The dried tissue was then at least 6 hours Caustic conditioned at a temperature of 21 ± 3 ° C (70 ° -5 ° F) and at a relative humidity of 35 to 40 % . The coated material was then subjected to an Atlab test device (developed by Atlas Chemical Co., Wilmington, Del./USA) Essentially, the test procedure consisted of a controlled rubbing of a fabric strip on a pair of electrostatic charge generating (Teflon) rods and on a stainless steel rod holding the friction generated charge for measurement on an electrostatic voltmeter This test was carried out at 25 + ¹⁰ C (77 + 2 ° F) and at a constant relative humidity of 35 to MO% .

The composition of the antistatic coating as well as the results obtained from the test and other important information these examples are given in Table VII below.

409830/0789

Humectant basi Part organ. Part 46 Part Elec Tabel - VII 200 • e Il π I. Nylon- ti Coating f · < i Charge app NJ Egg sch le acid le 46 le tro Part 200 π I. textile pad conditional ^v i * ⁱ
JI
; 1 enrichment 0.1 - ^ sp. Ver _ Amine lyt Part le It ( Egg material material ! 1 in KV 0.6 -a Sr bind 46 le What- 200 π 9.0 I. 8.1 " I! NJ NaOH 40 vinegar 60 23 20th NaCl s he Acid or pH ! Taffeta - Taffeta 2.: j (·
¹ 1.2 0.2 ^ acid 23 210 ■ Base to ί ί
¹ dd I.
J > _t NaOH 40 η 60 23 20th NaCl 2 pH-on Pad- 5 ' ! 0.5 P- ' NaOH 40 η 60 23 20 · NaCl 210 position pad material
It 2 ; I. .1.0 60 2 210 Acetic acid 6 ₉ 5 j material Taffeta I. .ί-
Ο NaOH 40 η .60 20th NaCl 2 ' right ■ '. ; \ ■ \ ! 5 ! (
! 0.2 co 52 I. KOH 56 Ants-46 60 20th NaCl 210 ti: 'ti (
! ί Taffeta ί It 2 j j 0.5 οο,
c *> I. . acid 60 2 180 9.0!. • pad ! O KOH 56 20th NaCl 2 material 5 i
i 0.1 O 53 y KOH 56 It 60 20th NaCl 180 " 6.5, ' It 2 \ 0.5 -ο 2 180 Ant; ⁿ y i CD T
»
I. KOH '■ 56 It 20th NaCl 2 acid J I 5! 1 0.0 NaOH ' 20th ti 10 KCl 180 ti- · ti; 2; 0.5 eat NaOH 20th It 10 KCl .2 150 ItT J ti .5 ί NaOH 20th Il 10 KGl 1 150 ί 2 O ^ NaOH 20th It 10 KCl 1 150 ti j Il 5 ! . 0 * KOH .56 vinegar 20th NaCl 1 150 ■ - «; f ti 2 j O ^ acid 1 it. ! 11
t • ! · I KOH 56 It 20th NaCl 2 ■ TI {M ·
j • 5 ; KOH 56 It 20th NaCl Il C »
ι · ^: 2! 58 2 200 vinegar eii ~ KOH 56 η 20th NaCl 2 I. '■ • 5;
; ί
'i $ 0 61 2 & 2 I.
I. 63 64 \ i '
J 1 \ I.
1 I.
i I \
ί '! ; ■ '

i'ContinueR KOH 1 from Tabel YII 56 25th • NaCl 3 500 Ants . '■ - . dd I. dd ο Taffetafc 2 ■ ι \ ! ; | i
Jf j 12th ι
\ se I. 56 vinegar 74 56 acid It * 5 ft i j
•; J I j ' ?,1, i KOH I.
I. acid 25th NaCl 3 500 η tr , 0 It I.
I. I. i | I ι I.
t 67 KOH I. 56 H 74 56 25th NaCl 3 500 dd , 1 " pad 2 I.
1
f i '| i I. 6S 56 Il 74 60 ti ^k ti material \\ ·. P, 8 j i KOH 25th NaCl 3 500 ti I. Il 5 i
i ! r 0.4: j € 9 KOH 56 It 74 Ants-46 25th NaCl 25th 245 " ti Taffeta ; 2 i ¹ y I.
I ( O I 69 Ants-56 acid π \ j. 0.2 i S. KOH acid 25th NaCl 25th 245 dd • Il 5 ¹ (, 0.6! OO:
ω; 71 KOH 69 ti Vinegar- 74 25th NaCl 25th 245 j '^; pad 2 ι • i O 72 ■ · 69 Il acid It 8th material i, ' KOH 25th NaCl 25th 245 i « 5 ! 0-11 KmJ 73 29 % 69 Il 20th NaCl 2 200 ; Taffeta 2 OO
co 74 NHOH 121 vinegar 1 j 0-1 29 % acid 20th NaCl 2 '200 3 '. » "2 ! [.j 75 ' I nip: 121 • i I I 29% 20th NaCl 2 200 2 I \ ί 76 NBpH 121 ! . a: pad _m 77 ^ material Taffeta 78 ¹

untreated

ro ο

K) K)

Examples 79-111

The samples treated in these "Examples" were conventional woven and nonwoven fabrics of the type and type set forth in Table VIII. In all cases the antistatic coating was applied in the same manner to the back of the latex -Vorübersugs applied and the textile sample was dried to remove excess moisture to remove Then, a polymeric Unterlap was applied to the tissue; e. (gain) is applied and at a temperature from 93 to 163 ⁰ C (200 to 325 ° F) 10 to 30? Cured for Minutes The coated material was then tectet using an Atlab testing device in the manner described above in connection with Examples 50 to 78. In these examples, the humectant was not made in situ but was added directly to the antistatic coating .

The composition of the antistatic coating as well as the Results obtained in the test and other important data for these examples are given in Table VIII below.

409830/0789

Table VIII

At- moisten- Teisp. tion- Ie middle

79; Sorbitol

! ester

80 '"
^! 81> i

^r 82J »

^; 83, "

: 87

: 88 "

89. "

90, "

• 91 CaCl

92

93 CaCl ₂

CaCl ₀

CaCl ₀

10 10 10

10 10

ί 85, 'Glycerin 20 86! «

20 20

20 20 20 20 20 20 20 20

Amin Netz- EIe- Tei-Teimit- tro- Ie Ie tel parts

10 10

20 20 20 20 20 20 20 20 20 20 20

1 1 0 0

0 0 0 0 0 0 0 0 0

KaCl 1

10

10 1 NaCl 1 10 1 NaCl 1

NaCl 1 NaCl 1 CaCl ₂ CaCl ₂ CaCl ₂ CaCl CaCl

2

CaCl ₂ 0 0 0 0 0

(5) (5) (5) (5) (5)

Sei- acid le z-jr Uas- pH-ser setting

pH textile material coating charge

Enrichment in KV

Acetic 5.5-6.5 taffeta acid

75 75 75 75 75 75 1 CO

It

ti

It
It
It
U

η
u
ti

Il

it

ti

Il

5.5-6.5 5.5-6.5

5.5-6.5

5.5-6.5 5.5-6.5 6.0-6.5 6.0-6.5 6.0-6.6 6.0-6.5 6.0-6.5 6.0-6.5 5.5-6.5 5.5-6.5 5.5-6.5 5.5-6.5 5.5-6.5

with liylon rayon filled. PoI-s t er ma t er i al

Taffeta

It

5 10

5 10

5 10

Padding material 2

5 "

Taffeta

"5 "

Padding material

3 5

0 0 1

5 0 1 0 0 1 0 0 0 0 0 O 0

"Continued from Table YIII

ί!
ί ι CaCl ₂ 20th 20th 0 (5) 0 100 vinegar
acid 5.5-6.5 5.0-5.5 Padding material 10 O i Ι97ί CaCl ₂ 30th 20th 0 (5) 0 110 dd 5.0-5.5 5.0-5.5 Taffeta 3 O 1 j 98; CaCl ₂ 30th 20th 0 (5) 0 110 ti 5.0-5.5 ti 5 O Vl : 99ι
• JI CaCl _2. ' 30th 20th 0 (5) 0 110 It 5.0-5.5 ti 10 O t 100; CaCl ₂ 30th 20th 0 (5) 0 110 M. 5.0-5.5 Padding material 3 O 101 ί
; ι CaCl ₂ 30th 20th 0 (5) 0 110 U 5.0-5.5 Il 5 O 102 ί
ι CaCl ₂ 30th 20th 0 (5) 0 110 ti 5.0-5.5 η 10 O 103 ί CaCl ₂ 40 20th 0 (5) 0 120 R. 5.0-5.5 Taffeta 3 O 104 y CaCl ₂ 40 20th 0 (5) 0 120 U 5.0-5.5 . 'tt 5 O 105 · ί CaCl ₂ 40 20th 0 (5) 0 120 dd 5.0-5.5 Il. ■ 10 O 106.! CaCl ₂ 40 20th 0 (5) 0 120 U 5.0-5.5 Po I s t erniat er i al 3 O 107 CaCl ₂ 40 20th O (5) 0 120 Il 5.0-5.5 dd 5 O 108 \ CaCl ₂ 40 20th 0 (5) 0 120 ti 5.0-5.5 Il 10 O 109 y
1 urea 30th ¹ 10 1 NaCl 1 . 110 Ants
acid 5.0-5.5 Taffeta 2.5 0-1 | 1Ο. |
• I
j I η 30th 1 NaCl 1 110 π with nylon rayon
filled pole
star material 5 • 0-1 π 30th .. 1 NaCl 1 110 dd Nylon rayon,
not woven 5 0.5
K.

N-Octyl-N-Ethiiyimorpholiniumäthylsulfat Condensate of tridecyl alcohol with 6 moles of ethylene oxide ^ ethoxylated sorbitol lauric acid ester Nylon, unless otherwise stated

* Ma's humectant was also, the electrolyte

OK)

Examples 112-121

In these examples, the floor covering sample was with the components given in Table IX below treated. The antistatic coating was applied in "sandwich form" to the underside of the flooring product after applied method specified above. The electrostatic test results are shown below Table X given.

409830/0789

OJ

VD

- 4-7 -

W. I. φ I. br ph co {χ] S. ί: ! 43 j: - ε ^ * S. · ** - I. H pi CO M. H Ctf Ö W. I. H H «Η S. B. S. • Η 00 % W.
frt OJ • 3 H el ri I. ¹ U
ti- O V JO Pf KN H !> ■ • Η
Λ \ VJ
H
"N «J V- V H IQ ^) IA O ti * *! !> · H I. η> O I. UJ res S. CD • Η
ft) r-J • ri O CO Ά ! * —I rj H I. I. O OJ PQ Ρ-; I. Ö 45 O 4> H OJ EH :CD φ O CD H H • Η I.
: · Η CvI S. Pl CO pi Pl O U M. •. φ • Η φ tM O O CQ H • H • Ρ Φ ft Pl O O 4-1 {25 © Φ U H • -j 1 CD ω Φ H CD φ 0 CiJ H H <* ί Φ
'S O) 4 * T -. · H ρ] H IA ·; : τ! £ * O IA co 9 I. S. S. 4 ^ ρ] ρ) O CQ Ρ ( Φ φ O 5 S. S. ^ _- Φ P. ω CD ■ Ρ CQ a CO ^ • Η Φ Ώ _{τ ι} Φ ^ i S. ^^ η3 • Ä ^ _- 1 en φ V V • Η (O Φ V * S. S. OJ • Φ • Η 14 IA ^ * - Ö f ι
rg Φ ^ ν * V »3 ν VO V ω O b £ ■ cd CQ ν- ν- V- OJ ί-Ι CQ V V V * V- O • Η Φ I. Φ O I. Φ & « • Η O O CO I. • • • Η P. Φ CQ \ - PQ V

409830/0789

Table X

Test AATC -123-1969 (all values in electrostatic volts)

CD CO OO Cu

σ ~ j oo co

Ex.
No. Chrome leather Neolite 112 +1200 -900 113 + 1500 -1000 114 +1700 -1200 115 + 1100 -1400 116 ^ -1500 -900 117 + 1900 -1700 118 -1800 -2000 119 + 1600 -1800 120 + 1100 -900

after steam cleaning, chrome leather Neolite

+1 700 + 1600: 1SOO +1 500 -1200 + 2000 + 1700 + 1500 + 1200

-1000 I. -900 £ -1500 -1200 -1400 -1900 -2100 -2000 ro -1100 CD K)
K)

Claims (12)

Patent claims 1. Antistatic textile and flooring product, characterized in that it comprises (T) a wear layer, (2) one arranged on at least one surface © of this layer Latex precoat j (5) a layer of an antistatic coating material arranged on the pre-coating layer, which in resent consists of a mixture of a) an organic antistatic agent _& (b) a humidifying agent from the group of ionic and non-ionic humidifying agents wad (c) a. Electrolytes, if the humectant © in is non-ionic humectant, imd (4) a polymeric backing layer which covers the antistatic layer so that the antistatic layer is between the pre-coat layer and the polymeric backing layer is arranged «, 2. Antistatic product according to Anspr-acfe T ₉ dadtjrch characterized in that it has as Abnutzungsschicht.eis fiber textile material or a fiber textile layer of the pile type. 3 · Antistatic product of claim 2 _$ characterized in that the batt is attached to a primary backing layer · 4. Antistatic product according to claim 2, characterized · ^ It can be seen that the fiber textile layer is tufted Carpet structure is made of pile fibers that are looped through a woven underlay * 5 »Antistatic product according to claim T, characterized in that that the floor covering is such 409830/0789 from the group of co-polymers and co-polymers. Yinyl Slab and Tile Products, of asbestos panel and tile products, of polyurethane and polyolefin flooring products and the Linoleuia Erdcl products. 6. Antistatic product according to one of claims 1 to 5 »characterized in that it contains the antistatic coating composition in a narrow range of about 0.34 to about 680 g / m (0.1 to 20 oz / yd. ² ) , Contains 7 · Antistatic product according eineza of claims 1 to 4, characterized in that it comprises the antistatic coating composition in an Eenge of about 68 to about 340 g / m (2 to 10 _t O os / yd. ^2), 8 antistatic product according to one of claims 1 to 7, characterized in that it is used as an organic antistatic agent contains an alkoxylated tertiary Aiii ^; · 9. Antistatic product according to one of claims 1 to 7 » characterized in that it is used as an organic antistatic agent contains a quaternary Imsociuia compound * 10. Antistatic product according to one of claims 1 to 7 » characterized »that the organic antistatic agent contains H-octyl-ir-ethyl-morpholinium ethosulfate as the amine. 11. Antistatic product according to one of claims 1 to 7 t characterized in that it contains a phosphate ester as an organic antistatic agent * 12. Antistatic product according to one of claims 1 to 9 »characterized in that it is a moistening agent contains ethoxylated sorbitol lauric acid ester * 409830/0789