SU1249031A1 - Method of producing polionenes - Google Patents

Description

This invention relates to the chemistry of non-molecular compounds, specifically to an improved method for the preparation of polymeric quaternary ammonium salts (polnionenes), and may be used in the cosmetic industry, as auxiliary agents for treating and dyeing textile fibers, and for treating wastewater used to produce photosensitive and electrically conductive materials.

The purpose of the invention is to increase the speed of the process.

Elemental analysis data indicate the presence of occluded water (2-6%), which cannot be removed by prolonged heating of the samples in a vacuum. Inorganic impurities are absent.

Example 1. In 75 ml of dimethyl sulfoxide (DMSO), 0.42 g {0.0025 mol) of potassium iodide is placed, 10.8 g (0.05 mol) of 1, 4-dibromobutane, 5.6 g (0.05 mol) N, N, N, N-tetramethylethylenediamine (TMEDA and hold at room temperature for 15 hours. To the thickened reaction mass is added a mixture of water with DMSO (1: 3) and poured into acetone. The precipitated the polymer is filtered off, washed with acetone and dried under vacuum.Further purification of polyionene is allowed to precipitate from an aqueous solution with acetone, Yield 11 g (67%).

Found,%: C 36.17; H 7.55, Br 47.98; N 7.88} J - residue.

S.ON, 4 "g

Calculated,%: C 36.16; H 7 „28;

Br 48.12; N 8.44.

Example 2. In 150 ml of DMSO 5.15 g (0.05 mol) of bromistog is placed. sodium, 10.8 g (0.05 mol) of 1,4-dibromobutane, 5.6 g (0.05 mol) of TMEDA and held at room temperature for 48 hours. Further processing, the reaction mixture is carried out as in Example 1. Yield 13 g (80%).

Found,%: C 36.37; H 7.21; N 7.73; Br 46.95.

2

Calculated,%: C 36.16; K 7.28; N 8.44; Wg 48.12.

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Order 4197/25 Runs 470

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Example 3. 65 ml of a mixture of methanol and dimethylformamide (DMF) (1: 1) are placed in a glass ampoule, 15 g (0.1 mol) of iodide are added.

sodium, 21.6 g (0.1 mol) of 1,4-dibromobutane and 11.2 g (0.1 mol) of TMEDA. The ampoule was flushed with argon, sealed, and kept at room temperature for 24 hours. The precipitate was filtered off and rinsed with a mixture of methanol and DMF, then with acetone. The resulting product is precipitated from water in methanol, washed thoroughly on the filter with methanol and dried in vacuo at room temperature.

temperature to constant mass. The polymer yield 20 g (62%).

Found,%: C 32.43; H 7.41; Br 35.83; J 12.53; N 8.39.

Calculated%: C 34.23; H 6.89;

Br 36.43; J 14.47; N 8.43.

Example 4. The synthesis and processing of polyionone is carried out similarly

Example 3. To 90 ml of a mixture of methanol and DMF (1: 1) were added 15 g (0.1 mol) of sodium iodide, 23 g (0.1 mol) of 1,5-dibromopentane, 11.2 g (0.1 mol) TMEDA and incubated for 96 h at room temperature. Yield 17 g (50%). Found,%: C 34.12; H 7.33; Br 29.28; N 7.78; J 19.76.

T; .

Calculated,%: C 35.42; H 7.03; . Br 30.60; J 19.44; N 7.51.

Example 5. 2.92 g (0.05 mol) of sodium chloride, 10.8 g (0.05 mol) of 1,4-dibromobutane, 5.6 g (0.05 mol) of TMEDA are placed in 150 ml of DMSO. and left at room temperature for 30 hours. The isolation and purification of the polymer was carried out as in Example 1. The yield of ionene was 48%.

Found,%: C 37.91; H 7.87; Br 34.84; C1 7.07; N 8.80. .

C "V% 2.Cl2

Calculated,%: C 39.16; H 7.89;

N 9.13; Br 37.21; C1 6.60.

Thus, the proposed method, in comparison with the known, allows B to increase the speed of the process by 2-7 times, and also to obtain ionenes containing different counterions in the macromolecule in one stage.

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Claims (1)

METHOD FOR PRODUCING POLYIONENES by reacting βί, ω-dibromoalkanes and Ν, Ν, Ν *, Ν'-tetramethylpolymethylenediamines, characterized in that, in order to increase the speed of the process, the reaction is carried out in the presence of alkali metal halides in an amount of 0.05-1 mol per 1 mol of starting reagents. e <s With