SU533602A1 - Method for producing carboxyl cation exchangers - Google Patents

Description

one

This invention relates to the field of creating synthetic ion exchange resins, in particular carboxyl cation exchangers used as sorbents.

Known for the acquisition of carboxyl cationic acids and the polymerization of unsaturated carboxylic esters in the presence of a divining structuring agent and the subsequent saponification of the polymer 1, 2 are known.

The disadvantages of these methods are the difficulty of regulating the structure and permeability of the polymer due to the different AKTpness of the monomers during sonolymerization, as well as the low degree of saponification of the copolymer (about 80%).

A known method for the preparation of carboxyl cation exchangers by polymerization of an unsaturated dialkyl dicarboxylic ester, fumaric acid dibutyl ester in the presence of a divine cleavage agent and the subsequent saponification of the polymer 3.

The method of this method is a low degree of saponification (about 85%) and the complexity of the technology due to the harsh conditions of the polymerization processes (9 hours 95-98 C) and saponified (10 hours, 165-, pressure 10-15 atm).

With the aim of a new degree of saponification of the polymer and improvement of the technology for the production of cation exchangers by the proposed method as

the initial source diary ether. Dicarbonose kps.yutsy pspo.zuzu dpmstarplovy ether dialkylgalactaric acid.

At 1mopolnosrizdpidim, one hundred percent effluent D1 alkyltartaric acid (amyl, azoamyl, butyl, ethyl, etc.) are obtained by treatment with a structured saponification, which is given in a flexible set by washing the mask, and the rest is given.

The homopolymer process is carried out by the suspension method in the presence of radical initiators at a temperature of 70-75 ° C for 2-2.5 hours.

Polymerization of polymers is carried out by removing the alcohol solution of alkali at 50-60 ° C for 6-7 hours. The degree of saponification reaches 98-99%.

Example 1. 35 g of diisoamyl galactaric acid are dissolved in 200 g of dry pyridine at 0 ° C, 40 g of anti-mstacrylic acid is added and left at 20 ° C for 65 hours. The reaction mixture is diluted with 17 ml of water, extracted with diethyl ether (500 tons), the extract is washed with 0.1 and. . water, dried over HAZO.;; remains iiridii ne1 1 stralzuyut when cop the chain and p he r and

A2504. The filtrate of the reaction mixture vacuum. The residue is dissolved in 15 ml of diethyl 3

The solution was diluted with 50 ml of α-petroleum zfir. The precipitated crystals are filtered, dried.

24.3 g (50%) of diisoamnyl galactaric acid dimethacrylic ester are obtained, i.e. ill. 130 ° C.

Found,%: C 59.47; H 8.01.

Calculated,%: C 59.22; H 7.81.

The process of emulsion polymerization is carried out by using a three-neck flask, spab 1 eppoy mixed Koii, around-1m. CHOLODYLYIIKO.CH, with a thermometer. 200 ml of a 1.1% aqueous starch solution are charged to the flask, 25 g of methylacrylate diisoamyl galactaric acid and 0, g of azodiisobutyronitrile dissolved in 50 ml of butanol are injected with running meelalcine. The reaction mixture is heated with stirring and held at this temperature for 2.5 hours. The resulting solid granules are filtered, washed with water, ethanol, and dried. The yield of 24.6 g (98%).

The resulting diisoamyl galactaric acid polydimethacrylic ester (20 g) was washed with 890 ml of 0.25 and. alcohol solution of KOH at 55 ° C b h. The granules are filtered, washed with ethanol, water, and dried. Get 16 g (93%) of cation in the K + form.

Found,%: C 40.97; H 4.87; By 17.41.

10 g of cation exchanger in K + form are treated with 150 ml of 3% -Hoii salt solution with stirring for 1 hour at 55 ° C. The reaction product is washed with water, dried. 8.1 g (98.7%) of polydimethacryloyl galactar are obtained.

acids - cationioite in the H + form.

Found,%; C 50.30; H 6.48.

four

The cation exchanger has a static exchange capacity: 1 each; it has a value of + -5.6 mg eq / g, C + + –4.75 mg eq / g, and Tubazide ions –4.4 μm eq / g. Specific volume in H + -form

2.2ml / g, specific volume in Na + -form

5.3ml / g.

Boiling cation exchanger in 5 n. solutions of sulfuric acid and caustic soda leads to a decrease in exchange capacity by less than 0.1%.

Using the proposed method will allow to obtain carboxyl catioins with a higher degree of saponification (98-99% versus 80-85% by known methods), as well as to simplify the technology of their production (excluding the use of pressure, reduction of temperature and duration at the stages of polymerization and washing. ).

Claims (3)

1. US Patent 2798053, cl. 260-2-2, 1957. 2. Avt. St. L 304262, class From 08/19/20, 1971. 3. Avt. St. No. 322344, cl. C 081 19/20, 1971 (nrotype).