SU383320A1 - - Google Patents

Description

METHOD FOR FIRE-PROTECTIVE AND NONMINABLE FINISHES OF TEXTILE PRODUCTS

This invention relates to the technology of oriie protective and non-wrinkle finishing of textile products made from Cellulose fiber. The known method of fire-retardant and non-laminating of finishing textiles from cellulose fibers by impregnating them with an aqueous composition on the basis of N-methylolphosphonamide derivatives and acid curing catalyst, followed by drying at 70-80 ° C and heat treatment at 130-200 ° C. P-CH -CH-UU-NC where Ri, R2, Rl, R2 is alkyl, halogenopropyl or aryl alkenyl, containing not more than four avjs of carbon; X and X are methyl or hydrogen atom. Cs-O CHfOp-cH -cHn-ai-NC R, -U IICNt-where Ra is methyl or ethyl, 5 10 CH7-UH2i x., C SCHS However, the known method does not provide a wet-resistant effect of flame retardant finishing of products without the use of nredkondensatov aminoplast, and also does not give the desired effect of pingaminoimost. In order to increase the finishing effect in the proposed method, Nmethylol phosphonamide derivatives of the general formula (I) / O-R; li -CO-CH-H2C-Pv If necessary, the product is impregnated in the form of an amino pre-condensate. (Preferably, compounds of the formula (II) / "- Ke 1 {-CO-S.N.HH2C-PC II 0-R are used.

The phosphorus compounds of formula (I) are obtained by reacting:

a) at least 2 moles of phosphoncargunic acid amide of formula (III)

GO, 0 K

Mr. about., -an-so-k1 ()

in which Rb Rs and X have said ziachini;

c) at least 4 mol of anhydrous formaldehyde in the presence of an acidic catalyst and, under certain conditions, an inert organic solvent in the presence of water at elevated temperatures.

Preferably, am, id 3- (dimethylphosphono) -propionic acid is used.

According to the proposed method, the products are plus an aqueous composition containing at least one compound of formula (I) and, if necessary, an amnnoplast precondensate, and then dried at a temperature of up to 100 ° C and thermally treated at 130-200 ° C.

The pH of the aqueous compositions containing the compounds of formula (I) is kept below 5, in particular below 3. For this purpose, inorganic acids are introduced into the composition, for example, sulfuric, nitric, ortho-phosphoric hydrochloric acids. Instead of acids, in particular hydrochloric, compounds can be introduced, of which in water easily, for example without heating, the corresponding acids are formed by hydrolysis. For example, three- and p-phosphorus chloride, phosphorus oxychloride, thioyl chloride, sulfuryl chloride, cyanuric chloride, acetyl chloride and chloroacetyl chloride can be mentioned. These compounds form acidic cleavage products during hydrolysis, for example cyanuric and hydrochloric acids. Instead of one of the strong acids, it is also possible to introduce a mixture of hydrolysis products of one of these compounds, or, for example, instead of hydrochloric or orthophosphoric acid, a mixture of hydrochloric and phosphoric acids, corresponding to phosphorus chloride, is expedient in a 5: 1 ratio.

The composition contains an acid catalyst that promotes acceleration of otladelin predko.ndensat aminoplast and the formation of a net structure of compounds of formula (I). Known amino acid curing catalysts on cellulosic materials, such as ammonium chloride, monosodium phosphate, magnesium chloride, zinc nitrate, etc. can be used as catalysts.

To obtain a flame retardant effect that is resistant to wet treatments, the addition of an aminoplast forcondensate is recommended, but not necessary. For example, the following amino acid precondensates are used: 1,3,5-aminotriazine, N-substituted melamines, for example N-butylmelamii, N-trihalomethylmelamine, and also ammeline, guanamin, for example benzo, aceto- or diguanamine. Then alkyl- or arylurea and thiourea, alkyleneurea or diurea can be used, for example ethylene-, propylene-, acetylenedimourea or, in particular, 4,5-dioxyimlyldazolido.n-2 and its derivatives, for example 4,5-dioxy, im dazole ; 1 Don-2, substituted in position 4 instead of oxy groups by the residue -CH 3 CH 2 CO-NH - CrbOH. Metholic derivatives of urea, ethylene or Melamine are preferably used. Especially valuable products are the most methylated compounds. Suitable precursor aminos of monoplasts are monomolecular and higher molecular precondensates of aminoplasts.

As an additive, esters of miniplast preconditions are also introduced into the composition. For example, ethers of alkapols, nanopolymers of methanol, ethanol, n-propanol, isopanol, m-butanol or peitanols are preferred. However, this is advisable in those cases where the amino precursor of the aminoplast is soluble in water (for example, menthylmethylamine dimethyl ether).

As an additive, a copolymerizate of 0.25-10% alkaline earth salt of a mono-carbopic acid with a-, p-ethylene bond is introduced into the composition; 0.25 - 30% N-metnolamide or N-methylol-amido ester of unsaturated mono- or dicarboxylic acid with a-, p-unsaturated (ethylene) bond; 99.5% to 60% of another copolymerizable compound.

The use of such copolymer increases the tensile strength and durability of the processed fibrous materials.

Of the other additives, softeners are used, FjanpHMCp aqueous emulsion of polyethylene or ethylene emulsion soiolimerizate, as well as a non-ionic emulsifier.

10-28% (by weight of the product) compounds of formula (I) are applied to the products. The aqueous compositions contain from 100 to 500 g / l, preferably from 250 to 400 g / l, of the phosphorogapic compound of formula (I).

The amount of said polymerizate additives and soft is 1-10% by weight of the compound of formula (I). The products are treated with fiber, linen, cotton, acetate lye and viscose fibers, or a mixture of these fibers with wool, polyamide or iolio |) irregular fibers.

The products are plus with an aqueous composition, they are present at a temperature of up to, and then subjected to heat treatment at temperatures above 100 ° C, for example, in the range of 130-200 ° (preferably 150-180 °). The processing time at 150-180 ° is 2-6 minutes. Then, in order to neutralize the acid, the products are washed for 3 minutes with an aqueous solution of calcined soda at a temperature of from 40 ° C to the boiling point.

The effect of fire resistance and incompatibility persists even after repeated washing.

or dry cleaning, and the textile-mechanical properties of the material thus treated are not impaired.

At the same time, processed cellulosic fibrous materials acquire the properties of fire resistance and wrinkle resistance without the use of an aminoplast precondensate.

SNGO-N, C

/ h

0 an9-sn2-so-k

shgo-n

Cl-CHrCHjO o0 OCHrCHrCl

X / n. On.)

Cl - CHi-C, H.20 CH CH CON K-OC-CH2H2C OCH-CHrCl

C.

CH CH-CH20 0

CH,

p

CH2 CH-CH20 CHfH2COK /

SNO o0 OStsNe

.

СНХ СНгСН СО-К-ОС-СН7Н2С ОСНН

m-iQR C.

Example 1. Water compositions A-D plus cotton fabric to a weight gain of 80%. Dried at 70-80 ° C and heat treated for 4.5 minutes at 160 ° C. Then, the fabric is washed for 5 minutes in a solution containing 2 g / l of anhydrous soda at boiling temperature, rinsed with water and injected. The tissue sample is boiled 5-10 times for 30 minutes in an aqueous solution containing 2 g / l of soda and 5 g / l of soap. The sample is then tested for fire resistance, tensile strength and crush resistance.

Aqueous compositions A and B contain 280 g / l of the product of formula (IV), compositions C and D - 320 g / l. The pH of formulations A and C is 2.2; The pH of compounds B and D is 2.5.

The test results are shown in Table. one.

The neck of the treated fabric is almost the same as the neck of the untreated cloth.

In addition, organophosphorus compounds of formula (I) can also be added to the spinning mass, for example, from cellulose acetate, depending on their solubility in organic solvents, for example in acetone.

In the examples, N-methylolphosphonamide derivatives of the following formulas are used:

0 O-CH

V, w

N-CO-CH2-H7C O-CHj

0 oan2-sn 11

N- o CIV.,

(F)

Example 2. Cotton fabric plus water composition EJ to gain 80%, dried at 80 ° C and then heat treated for 4.5 minutes at 160 ° C. Then the fabric is boiled for 5 minutes in an aqueous solution containing 2 g / l (anhydrous) soda ash, rinsed and dried.

Compositions E, F, C contain 320 g / l of the product of formula (IV), composition H-395 g / l of the product of formula (VI), composition J-380 g / l of the product of formula (VII) and 10 g / l of condensation product 1 mol n-gret -..no.nilphenol with 9 mol of ethylene oxide. In addition, E-J formulations contain 30 g / l of 85% phosphoric acid (including untreated tissue). pH of E-2.2; F-2.0 composition; composition C-1,9; compositions H HJ -2,1.

The flame resistance of the fabric is then determined by the vertical test (norms DIN 53906). The test results are shown in Table. 2

Note and e:

1) Vertical test in accordance with the regulations

2) “Monosanto according to the norms of ААТСС 88А-1964Т.

3) Average of 10 measurements.

4) Breaking load according to SNV-98461 norms.

table 2