CS239273B1 - Auxiliary textile preparation to improve waterproofing - Google Patents

Abstract

A moisturizing preparation that allows application in baths in the presence of catalysts for crease-resistant treatment, prepared by reacting 1,2-epoxy compounds with amines in a ratio of 1 to 1.1 to 3.5.

Description

BACKGROUND OF THE INVENTION The present invention relates to an auxiliary textile composition for improving the waterproofing performance of silicones based on the reaction product of an epoxy resin and an amine or polyamines.

It is known that epoxy resins can react with amines or polyamines to form soluble or insoluble products. Their properties vary according to the reaction conditions and the relative ratio of the reacting epoxy resin to the amine or polyamines. With a small amount of polyamines relative to the epoxy resin, either insoluble polymers or additive products with limited stability are obtained.

When the reaction is carried out in an environment of solvents in excess of amine or polyamines, where the amount of reactive hydrogen atoms contained in the polyamines is many times greater than the number of epoxy groups, the resulting adduct does not lose stability even at high temperatures of about 150 ° C. British Patent No. 933,729 protects, for example, the preparation of a 1,2-epoxy resin and polyamine addition product in a solvent environment at a ratio of 1: 3 epoxy to 1 reactive hydrogen atom of polyamines. The resulting product is stabilized by adjusting the pH in the range. to 7.

The disadvantages of the prior art formulations are the necessity of their stabilization at a pH in the range of 2 to 7 and the high sensitivity to the metal ions contained in the catalysts used for the creasing of fabrics, thus eliminating the possibility of carrying out hydrophobic and creasing of fabrics simultaneously. In practice, this situation is addressed by carrying out both operations separately, resulting in reduced labor productivity and increased costs and the need for more costly equipment.

The prior art compositions are furthermore intolerant to some types of urea-formaldehyde resins used for non-creasing textiles and cause precipitation of the treatment baths, even at reduced bath concentration. This again limits the possibility of their universal use.

It has now been found that the disadvantages of the current state of the art are eliminated by a textile auxiliary agent for improving the waterproofing performance of silicones, obtainable by reacting 1,2-epoxy compounds having an epoxy equivalent of 170-400 with amines having at least 2 reactive hydrogen atoms bound to the nitrogen atom of amino. up to 45 ° C in the presence of an inert, water-soluble solvent and a low boiling organic acid according to the invention such that it is a product of the epoxy compound with an amine in a ratio of 1 to 1.1 to 3.5; from 7 to 9.

Advantages of the preparation according to the invention consist mainly in the possibility of stabilization of the preparation at pH 7 to 9, the preparation is not sensitive to metal ions of creasing catalysts, which brings simplification of the technology of both treatments.

Example 1

To 206.3 g of an epoxy resin prepared by the addition of 2,2-bis (4-hydroxyphenyl) propane to 1-chloro-2,3-epoxypropane, whose epoxy equivalent weight is 192 (corresponding to 1.074 epoxy groups) is added at 20 ° C with stirring, 345 g of methanol and 44.8 g of diethylenetriamine (corresponding to 2.16 reactive nitrogen-bonded hydrogen atoms). The temperature of the reaction mixture rises spontaneously, after a short time the resin dissolves and immediately thereafter 38 g of acetic acid is added. The temperature of the mixture was maintained at 40 ° C.

The progress of the reaction is monitored by sampling the reaction mixture and testing for water solubility. When the sample of the reaction mixture is clearly soluble in water, the reaction is terminated by adding 1022 g of water to the reaction mixture. The solution has a first compound content of 15.16% and a pH of 8 and is stable for more than 2 years.

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Example 2

To a mixture of 100 g of methanol and 15 g of diamineodipropylmethylamine (0.413 reactive H atoms) was charged with stirring at 30 ° C 62 kg of an epoxy resin whose epoxy equivalent weight was 200 (corresponding to 0.31 epoxy groups in the resin). The reaction mixture was maintained at 35 ° C, after which solubility in acidified water was reached after 95 minutes. The reaction was assembled by adding 16 g of acetic acid and 295 g of water. The resulting product is a clear solution, cationic in any water-soluble ratio, containing 15.7% solids having a pH = 8.5.

Example 3

To 31.25 g of the present epoxy resin prepared by the reaction of 2,2-bis (4-hydroxyphenyl) -propane and 1-chloro-2,3-epoxypropane, whose epoxy equivalent weight is 195 (equivalent to 0.16 epoxy groups), is added with stirring 30 g of ethanol and 15 isopropanol, 5 g of ethylenediamine (corresponding to 0.33 N-reactive H atoms) and 3.9 g of acetic acid.

The temperature of the reaction mixture was maintained at 40 ° C. After 120 minutes, the reaction mixture was already clear water soluble. The reaction was quenched by the addition of 135 g of water. The solution obtained, containing 16.5% of active ingredient, was clear with poor opalescence, pH ⁸⁸ 8.2.

Example 4

To a solution of 40 g of an epoxy resin prepared in accordance with Example 1 having an epoxy equivalent weight of 250 (equivalent to 0.16 of the epoxy groups) dissolved in 60 g of methanol was added 8.3 g of diethylenetriamine and 7 g of acetic acid was added dropwise over 10 minutes.

The temperature of the reaction mixture was maintained at 45 ° C, after 1 hour 15 minutes perfect water solubility was achieved. The active compound concentration was adjusted by dilution to 15% by addition of 206.7 water. The pH of the reaction mixture was 8.5. The solution was stable for more than 1.5 years.

Example5

To a solution of 50 g of ethyloelosol (ethylene glycol monoethyl ether) and 31.5 g of epoxy resin prepared as in Example 1 having an epoxy equivalent of 205 (equivalent to 0.154 epoxy groups) added at 20 ° C with stirring 9 g of dimethylaminopropylamine (equivalent to 0.176 reactive hydrogen atoms) , 85 g of acetic acid.

The reaction mixture was maintained at 34 ° C. Water solubility was achieved after 1 hour and 10 minutes. Diluted by the addition of 130 g of water to a concentration of 17.9% active ingredient. Achieving a pH of more than 10 blunted by the addition of 2 g of acetic acid to pH 9 (final concentration is 17.7%) ·

Claims (2)

SUBJECT OF THE INVENTION An auxiliary textile preparation for improving the waterproofing performance of silicones, transportable by reacting 1,2-epoxy compounds having an epoxy equivalent of 170 to 400 with amines having at least 2 reactive hydrogen atoms attached to the nitrogen atom of an amino group, at a temperature of 20 to 45 ° C. the presence of an inert, water-soluble solvent and a low boiling organic acid, characterized in that it is formed by the reaction of the epoxy compound with an amine of 1 to 1.1 to 3.5. 2. An auxiliary textile preparation for improving the waterproofing performance of silicones according to claim 1, characterized in that its pH value is adjusted to 7 to 9.