DE1004585B - Process for making fibrous material water repellent - Google Patents

Description

GERMAN

Subject of the uswtpt ^ patent application F 9205 IVc / 8k is a process for making fibrous material water-repellent, the fibrous material being treated with solutions of 1 mol of aluminum alcoholate, from 0.2 to 2.5 mol, advantageously 0.3 to 0.8 mol, of higher molecular weight carboxylic acids and of solid to semi-solid paraffinic hydrocarbons treated in anhydrous organic solvents and then dries.

The invention now relates to the modification of the method for making fibrous material water-repellent according to Hfttrp * JJatentanmeldung F 9205 IVc / 8k, whereby this with solutions of 1 mol of aluminum alcoholate and 0.2 to 2.5 mol, advantageously 0.3 to 0.8 mol, of higher molecular weight Carboxylic acids in anhydrous organic solvents in the absence of solid to semi-solid Treated paraffin hydrocarbons, then dried and a heat treatment, preferably at Temperatures above 100 °, subject. Instead of the aluminum alcoholates, one can also use their carbon dioxide or sulfur dioxide addition products (cf.Tishchenko, Chem. Zentralblatt, 1900, I, p. 585) to use for the preparation of the aluminum alcoholate solutions. A slight impregnation is achieved, as is the case for many outerwear materials, for example such made of rayon or rayon and wool or cotton is desired. Since networkability and If the water absorption of rayon is considerably greater than that of natural fibers, a hydrophobic finish contains more rayon wool Fabrics of particular interest because this finish reduces absorbency and the tendency to crease and improves grip, appearance and load-bearing capacity. On the other hand, there is a more extensive hydrophobization due to the use of paraffin hydrocarbons, undesirable in many cases, as this reduces the absorbency and ability to absorb body moisture and sweat unfavorably and under certain circumstances can even reduce the air permeability of the fabrics.

The fibrous materials which have been hydrophobized according to the invention are dried and subjected to a heat treatment. Heating to temperatures above 100 °, for example to 125 to, has proven to be particularly advantageous 160 ° C. The heating can be carried out by known methods, e.g. B. by ironing, mangling, Decating, calendaring, in the drying cupboard, tumbler, on the steaming doll or the like.

In the German patent specification 496 444 a method described for the water repellent treatment of rayon, using compounds that are limited to 3 equivalents Aluminum contain less than 3 equivalents of fatty acid. The remaining valences are through Saturated hydroxyl groups. The compounds are only somewhat soluble in hydrocarbons and do not dissolve in those in dry cleaning

Process for making fibrous material water-repellent

Addition to notification F 9205 IVc / 8k

(See Pat Cl. Ν..ϊΊ

Applicant:

Farbwerke Hoechst Aktiengesellschaft

formerly Master Lucius & Brüning,

Frankfurt / M.

Dr. Ludwig Orthner, Frankfurt / M.-South,

and Dr. Martin Reuter, Frankfurt / M.,
have been named as inventors

common chlorinated hydrocarbons. In addition, the impregnation effects achieved are insufficient.

It is known from US Pat. No. 2,469,041 to mix fiber material with solutions of neutral aluminum salts of carboxylic acids, which are produced by reacting aluminum alcoholate with carboxylic acids, in to treat organic solvents. However, the water-repellent effect achieved is extraordinary low and not sufficient even for a light impregnation.

This is evident from the following comparative experiments, in which the impregnation solutions are dissolved by dissolving 0.03 mol = 7.4 g of aluminum butoxide and varying amounts of stearic acid (0.002 to 0.09 mol; EP 80 °) in 11 Perchlorethylene obtained at ordinary temperature became. The impregnation and sprinkling tests were carried out as follows:

In 170 ecm perchlorethylene solution each, a cellular wool muslin cloth (Vistra), size 600 cm², weight 7 g, was soaked for 1 minute at 60 °, squeezed off to an approximately 65% increase in weight and _{dried for 2} hours at 120 ° in a drying cabinet. Then the

Rag overnight at 20 ° and 60% relative humidity air-conditioned.

For sprinkling, 1.5 l of each impregnation and lobes measuring 10 x 10 cm were added one after the other Water of 20 ° in about 20 seconds from a height of 85 cm

609 840/399

showered over (angle of impact 45 °), thrown off by hand and squeezed off sharply. The lobes were weighed closed before and after the irrigation, from which the irrigation humidity (BF) is calculated as a percentage increase in weight.
The following results were obtained:

Added stearin
Mole constitution according to the present registration
according to the USA patent
2,469,041, example 4 BF
% Not impregnated cloth ...
0.002
0.006
0.018
0.030
0.042
0.075
0.090 Al (OC ₄ H ₉ ) ₃
Al (C ₁₇ H ₃₅ COOW (OC ₄ H _{9) 2, 9}
Al (C ₁₇ H ₃₅ COO) ₀₈₂ (OC ₄ H ₉ ) _{2) 8}
Al (C ₁₇ H ₃₅ COO) _rB (OC ₄ H ₉ ) _{2) 4}
Al (C ₁₇ H ₃₅ COO) _1n (OC ₄ H _{9) 2, 0}
Al (C ₁₇ H ₃₅ COO) _n , (OC ₄ He) ₁ ,,
Al (C ₁₇ H ₃₅ COO) ₂₁₅ (OC ₄ H _{9) 0) 5;}
Al (C ₁₇ H ₃₅ COO) ₃₁₀ (OC ₄ H _{9) 0, 0} 140
130
51
45
55
56
54
62
75

The above figures clearly show that even the addition is extremely low Amounts of stearic acid have a significant effect. If the experiment is carried out according to the USA patent specification -, Example 4, with the addition of 20 g of paraffin per liter, a value for the rain moisture is obtained of 65%, a value that is still above the values specified for the the components used in the process of the invention are obtained. It must be here it should be pointed out that the addition of paraffin does improve the water repellent effect is, however, at the same time a much higher tissue loading is achieved, which is synonymous with decreased breathing and increased soiling.

35 example

A half-wool dress is impregnated in a bath made by mixing a solution of 15 g of aluminum ethylate

formed in 11 ethyl acetate with 15 g of oleic acid is. After drying in a tumbler, the dress is heated to 100 ° for another 10 minutes. The carrying capacity of the dress has gained a lot as a result.

Claims (1)

PATENT CLAIM: Modification of the procedure for making fibrous material water-repellent according to the patent application F9205IVc / 8k, characterized in that one this with solutions of 1 mol of aluminum alcoholate and 0.2 to 2.5 mol, advantageously 0.3 to 0.8 mol, Treated higher molecular carboxylic acids in anhydrous organic solvents, then dried and subjected to a heat treatment. Considered publications:
U.S. Patent Nos. 2,469,041, 2,225,197;
Elliott, "The Alkaline-Earth and Heavy-Metal Soaps" (1946), p. 184. © 609 840/399 3.57