DE1769913A1 - Flame retardant textiles - Google Patents

Description

FARBENFABRIKENBAYERAG 1769913

LEVERKUSEN-ltayerwerk P.ten.-Abbey, Reu / Ws

Flameproof textiles

■ The invention relates to flame-resistant textile structures such. B. floor coverings, upholstery fabrics, wall coverings, curtain fabrics and industrial textiles made from fully synthetic, regenerated and natural fibers, as well as their mixtures, the flame retardant mixtures of phosphorus-containing compounds, polyalkyl halides, antimony compounds and polyurethanes.

Numerous compounds have been described which have been proposed for flame retarding molded structures made of fibers and filaments. As flame retardants are z. B. halogen-containing polymers and / or polymers with antimony trioxide additives, also known salts of phosphoric acid. However, these products do not meet all of the conditions that are required for making textile structures flame-resistant. The use of such methods must not reduce the physical properties, in particular the strength of the textiles. The textile character of the goods, for example the softness and suppleness of the handle, should not be influenced. Furthermore, the use of flameproof agents must not cause any additional soiling or a

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produce a superficially visible coating and the effects achieved must be resistant to cleaning, shampooing, be vacuum cleaner, abrasion and aging resistant.

For flameproofing of text lien structures, especially of upholstery fabrics, floor coverings, heavy curtain goods, tent fabrics, needled nonwovens and industrial fabrics flame retardants are now proposed that phosphorus from homogeneous mixtures of halogenated Phosphorsäureestern, plasticizers, polyalkylene halides!, Antimony oxides, and polyurethanes are made. The surprisingly good flame retardant effects obtained by these mixtures are due to the synergistic behavior of the individual components and cannot be achieved, or only to a significantly lesser extent, by the individual compounds. The textiles are coated or finished on at least one side, for example the back. The coating can also be present as an intermediate layer by applying a lamination fabric after the knife process and at the same time fulfill the function of lamination compounds or adhesives. Another advantage of the process is the improvement in the rebound behavior of textiles treated according to the invention and the associated low tendency to form creases or creases during processing and in use.

The amount of substance applied based on the weight of the fabric of the textile structure is between 5 and 150 ßew. #, Preferably

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se at 40 to 70 #. The order quantities are substantial under the lamination weights of normal coatings, z. B. for waterproof tarpaulins or rainwear. The textiles treated according to the process are steam-proof and air permeable. The individual components are preferably used in proportions (phosphoric acid compound-polyalkyl halide-antimony oxide-polyurethane) from 1: 0.2: 0.05: 0.1 to 1: 1: 0.5: 1 used.

As phosphorus-containing compounds which, in addition to their function as flame retardants, are also effective as plasticizers are, for example, phosphoric acid esters such. B. tritoluyl phosphate, tricresyl phosphate, triphenyl phosphate, Diphenyl cresyl phosphate, trioctyl phosphate, diphenyloctyl phosphate, Tris (chloroethyl) phosphate, tris (dichloroethyl) phosphate, tris (dichloropropyl) phosphate, tris (dichlorobutyl) phosphate, tris (bromoethyl) phosphate, tris (dibromoethyl) phosphate, Tri3 (dibromopropyl) phosphate, bis (dichloropropyl) (propyl phosphate and their mixtures are used.

As polyalkyl halides, polyvinyl chloride and polyvinyl bromide compounds with a molecular weight of 30,000 to 150,000 are possible as an example. The products must be processed as pastes and at least 25 to 30 percent. * Included $ plasticizers. Your copolymers with z. B. vinyl acetate, vinylidene chloride, maleic and fumaric acid esters, styrene, acrylic esters and acrylonitrile are also suitable »

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The polyurethanes used are compounds made from aliphatic and aromatic polyesters and / or Polyethers with a molecular weight of 500 to 10,000 are made with aliphatic and aromatic polyisocyanates are. For example, toluene diisocyanate 2.4 / 2.6, 1.6-hexamethylene diisocyanate, triisocyanate from 1 mol of trimethylolpropane and 3 moles of tolylenediocyanate-2.4 and Adipic acid / 1.6-hexanediol polyester of molar weight approx. 2000 or from terephthalic acid / ethylene glycol and / or Polypropylene oxide ether can be used. The polyurethanes are in the form of prepolymers in a molar ratio of 1: 1. you will be together with polyisocyanates the coating compounds added, the ratio of the NH groups of the urethanes to the NCO groups of the isocyanates 1: 0.5 to 1: 1 is. Antimony trioxide in powdered or suspended form is used as the antimony compound. the Textiles to be treated are made of fibers and threads of natural and synthetic origin, for example made of polyamides, polyacrylonitriles, polyesters, polyalkenes, polycarbonates, polyurethanes, halogenated polyolefins, Regenerated cellulose, cotton and "whole" or from their fiber blends.

The structures formed according to the invention such as coated fabrics made of fibers and filaments of the type described above or Textiles that have an intermediate layer of the stressed flame

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contain solid dimensions, I draw in front of materials without treatment in that their flammability is essential is decreased. This process is particularly important for textile structures made of polyacrylonitrile fibers suitable. A special advantage of the method is that when it is exposed to flames, none dripping melt is created.

The technological data of the textiles are not or only slightly changed. The elasticity of the treated materials increases. Another advantage are the wash resistance and solvent resistance of the claimed effects are remarkable.

For Hers RECOVERY flammf.ester textiles procedure can be followed in that the sweeps materials to be coated on a coating installation by means of elastic doctor blade, knife over roll or air knife with the claimed pastes and then in a drying tunnel at 70 - dried 160 ⁰ G. ^{The knife setting of the doctor blade should be such that the applications of the dry c} / o coating, based on the weight of the textiles, amount to between 5 and 150% by weight, preferably 40 to 70 c / o. The coating should be carried out in such a way that the treated goods remain largely permeable to air and water vapor.

ova

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example 1

Tufted carpets made of polyamide 6 fibers with a fabric weight of 13OC g / m * are back-coated by means of a roller doctor blade, the knife setting of which ensures an application of 65% by weight. The used Coating paste from 2 mixing components (A and B) is mixed immediately before use by vigorous mixing produced as a homogeneous mass. It has the following composition:

Share A

$ Polyvinyl chloride (M.W. approx. 40,000) 30 wt.>

Tricresyl phosphate 42 "

Tris (dibromopropyl) phosphate 10 "Diphenyl thiourea (PVC stabilizer) 1"

Antimony trioxide 2.5 ""

Part B

Polyurethane (made from aliphatic polyester

Mole weight 2000 and Toiuy] diisocyanate-2.4 11.6 wt. #

Triisocyanate (from trimethylolpropane and toluylene diisocyanate-2.4) 75 Ψ in acetic acid ^ äthylester 2 "

Conversion product of N-methyl diethanolamine

and phenyl isocyanate (1: 2) x 0.9 "

The proportions of B are in a weight ratio of 1: 1 with Acetic acid ethylene ter gelatinized and mixed with A.

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BATH ORIGINAL

The coated goods are then treated in a drying tunnel at 145 ^{° C. for 5 minutes.}

The fire test according to DIN 53906 is passed without dripping melt. After 5 shampoo treatments on the carpet the burning behavior remains unchanged according to DIN 53906.

Example 2

ο Cotton fabric with a fabric weight of 350 g / m 2 is coated on a rubber squeegee with a flame retardant paste of the composition described below. The Paetenauf order of the back coating is 45 wt. ^. ^{It is then dried at 150 °} C. for 4 minutes on a drying frame. The fire test according to the flambility 45 ° test (SWV 98896 and ASTM D 1230-52 T) results in flame-retardant, self-extinguishing goods.

Share A

Polyvinyl chloride (mol. Weight 50,000) 28 weight #

Triphenyl phosphate 40 "

Tris (dichloroethyl) phosphate H «

Triphenyl phosphite 0.5 "

Antimony trioxide 3 "

Part B

The composition used corresponds to the parts described in Example 1.

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ORIGINAL INSPECTED

The proportions of B are in a weight ratio of 1: 1 with Ethyl acetate dissolved and mixed with Part A.

Example 5

Upholstery fabric made of polyamide 6 velor with a product weight of 320 g / m 2 is coated on the back with the paste described below on a rubber squeegee. The paste application is 70 wt. ^, Based on the weight of the fabric of the velor. The drying took place on a drying frame for 5 minutes at HO ⁰ C.

The test of the burning behavior according to DIN 53906 was passed without dripping melt.

Share A

Polyvinyl chloride (mol. Wt. 40,000) 32 wt. £

Diphenyl cresyl phosphate 40 "

Trie (bromopropyl) phosphate 9.5 "

Diphenylthiourea 0.8 "

Antimony trioxide 3.2 "

Part B

Polyurethane

Toluylene diisocyanate 2.4 in a molar ratio of 1: 1 with Polyester made from adipic acid and hexane

diol-1.6 mole wt. 2100 11.8

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Thiophosphoric acid-O.O.O-triphenyl-

β8ΪβΓ-4.4'.4'-triisocyanate 1.8 wt. #

Reaction product of N-methyl-

diethanolamine and phenyl isocyanate (1: 2) 0.9 "

The proportions of B are dissolved in ethyl acetate in a weight ratio of 1: 1 and mixed with portion A.

Example 4

Curtain fabric made of polyacrylonitrile fibers (velor fabric) with a fabric weight of 500 g / m 2 is coated on the back with the paste described below using an air knife and sandwiched with a Perlon lining fabric. The paste application is 65% by weight based on the weight of the fabric. ^{It is then dried at 145 °} C. for 5 minutes on a drying frame.

The test of the burning behavior according to DIN 53906 results in self- extinguishing, non-dripping textile material. The same result is obtained after 3 treatments in perchlorethylene (cleaning).

Share A

Polyvinyl chloride (mol. Wt. Approx. 80,000) 32 wt. # Tricresylphoephate 42 "

Tris (dibromopropyl) phosphate 8 "

Diphenylthiourea 0.8 "

Antimony trioxide 2.7 "

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Part B

Polyurethane from polyester (adipic acid / hexanediol-1.6, mol. Ratio 1: 1) and tolylene diisocyanate-2. ^ Toluylene diisocyanate- ^. 6 mixture in a molar ratio of 1: 1 11.3 triiosocyanate (from trimethylolpropyn and toluylene diisocyanate 2.4) 75 $> in ethyl acetate reaction product of N-methyl diethanolamine and phenyl isocyanate (1: 2) 1.2

Part B is in a weight ratio of 1: 1 with ethyl acetate dissolved and mixed with part A.

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Claims (4)

Claims 4f 1. Flameproof textile structures made from natural and / or synthetic threads, fibers or yarns containing 5 to 150 wt. # as flame retardants - based on the weight of the goods a homogeneous mixture consisting of a halogen-containing phosphoric acid ester, a polyalkyl halide, a phosphorus-containing halogen-free plasticizer, a Antimony oxide and a polyurethane or its reactive polymer mixture. 2. A process for the production of flame-resistant textile structures from natural and / or synthetic threads, fibers or yarns by applying flame retardants ^ characterized in that the textile structures are on at least one side with 5 to 150 wt.96 - based on the weight of the goods - a flame retardant consisting of a homogeneous coated MisQhung of a halogen-containing organophosphate, a Polyalkylhalogenid, a phosphorus-containing plasticizer, antimony oxide and a polyurethane or its reactive polymer mixture and then after-treated at temperatures of 70-160 ⁰ C. 3. Process according to Claim 2, characterized in that the phosphoric acid ester used is Iri (haloalkyl) phoephate will. ^{A11621 19} - ¹¹ - 109829/1787 4. The method according to claim 2, characterized in that Polyvinyl chloride pasteable as polyalkyl halide or its copolymers with vinyl acetate, styrene, maleic and pumaric acids, Acrylic acid ester and acrylonitrile is used. 5. The method according to claim 2, characterized in that as polyurethane a prepolymer made from polyesters and / or polyethers and diisocyanates in a molar ratio of 1: is used in mixtures with a polyisocyanate. 109829/1717 Le A 11 621 -12-