SU1657513A1 - Method for obtaining anionites - Google Patents

Abstract

This invention relates to the synthesis of macroporous anion exchangers with reduced toxicity with silicic acid and increased mechanical strength. The invention consists in the suspension copolymerization of 2-methyl-5-vinylpyridine and divinylbenzene in the presence of a solvent-porous agent - a mixture of toluene or butyl acetate with alkylbenzene with a content of 10-20% in a mixture of toluene or butyl acetate and hectare acetate in the amount of 10-20%, and apliclene. 15 - 20% by weight of the mixture of monomers, followed by the introduction of ionic groups. 2 tab. g (L

Description

The invention relates to the synthesis of high molecular weight ion exchange sorbents and can be used to produce vinylpyridine type ion exchangers designed to extract valuable components in the hydrometallurgical processing of acid slurries of aluminosilicate ores.

The purpose of the invention is to reduce the toxicity of anion exchanger with silicic acid and preserve the mechanical strength during operation.

Example 1. In the reaction flask load 260,0 mach. 1% starch solution, 0.086 wt.h. me-, tola and with stirring are introduced

a mixture consisting of 86.6 wt. 2-methyl-5-vinylpyridine (COI) with a content of the main product of 90%, 20.0 wt.h. technical divinylbenzene (DVB) with the content of the main product 50%, 2.0 wt.h. benzoyl peroxide, a polymerization initiator, 10.0 wt.h. toluene and 15.0 ma.h. alkylbenzene (10 and 15% by weight of monomers).

The monomers are polymerized in the following stepwise temperature-time mode: the temperature rises from 20 to 80 ° C for 40 minutes; exposure at 80 With 3 h; temperature rise from 80 and

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XI SP

with

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90 C for 20 minutes; holding at 90 ° C for 2 h.

After filtering off the mother liquor, spherical copolymer granules are obtained. The granules of the obtained copolymer are washed with water from the mother liquor and boiled in water for 6 hours to remove the blowing agent. The weight of the obtained copolymer 97 wt.h.

For the synthesis of the strong base anion exchanger HBYApT, the copolymer obtained is subjected to N-alkylation with dimethyl sulfate in methyl alcohol. For this purpose, 100.0 mach. copolymer is poured 400,0 wt. of methyl alcohol, and after swelling of the copolymer, 94.1 wt.h. dimethyl sulfate. The N-alkylation reaction is carried out for 3 hours at room temperature.

The granules of the obtained HBYApt anion exchanger are filtered off, washed with 10% sulfuric acid and then with water to pH 3 of the wash water.

Physico-chemical properties of the obtained anion-exchange HBYApt; total C1-ion exchange capacity of 4.8 mEq / g; specific volume of anionite swollen in water, 3.0 ml / g; mechanical strength of anion exchanger swollen in water for 1 h 99%, for 6 h 99%.

Example 2. In the reaction flask load 270,0 MAH. 1% starch solution, 0.086 wt.h. a mixture consisting of 86.6 parts by weight was introduced with stirring. Profit center (content of the main product is 90%), 20.0 ma.ch. Technical DVB (content of the main product 50%), 2.0 wt.h. benzoyl peroxide, 20.0 ma.ch. toluene and 20 ma.ch. alkyl gasoline (20 and 20% by weight of monomers).

The polymerization reaction is carried out according to the method described in example 1. The strongly basic anion exchanger VHYApT is obtained by N-alkylation of the copolymer according to the method of example 1.

Physico-chemical properties of the obtained anion-exchange resin: full C1-ion exchange capacity 4.8 mg-eq / g: specific volume of anion-exchange resin swelled in water 3.1 ml / g; mechanical strength of swollen anion exchanger for 1 h 99%, for 6 h 99%.

Example 3. In the reaction flask load 260,0 mach. 1%

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five

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starch solution, 0.086 wt. a mixture consisting of 86.6 parts by weight was introduced with stirring. Profit center (content of the main product is 90%), 20.0 ma.ch. technical divinylbenzene (content of the main product 50%), 2.0 wt.h. benzoyl peroxide, 5.0 m.ch. toluene and 10.0 ma.h. al-kilbenzine (5 and 10% by weight of monomers).

The polymerization reaction is carried out according to the method described in Example 1. The strongly basic anion exchange resin VP-1ApT is obtained by N-alkylation of the copolymer according to the method of Example 1.

Physico-chemical properties of the anion exchanger obtained: total C1-ion exchange capacity 4.7 mg-eq / g; specific volume of anion exchanger swollen in water, 3.2 ml / rj, mechanical strength of anion exfoliated in water for 1 h 90%, for 6 h 80%.

Example 4. In the reaction flask load 270,0 MAH. 1% starch solution containing 240 g / l of sodium chloride, 0.086 wt.h. a mixture consisting of 86.6 parts by weight was introduced with stirring. Profit center (content of the main product is 90%), 20.0 m.ph. Technical DVB (content of the main product 50%), 2.0 m.ph. benzoyl peroxide, 20.0 mas. h. acetic acid butyl ester (butyl acetate) and 20.0 wt.h. alkyl gasoline (20 and 20% by weight of monomers).

The copolymerization reaction is carried out according to the method described in Example 1. The strongly basic anion exchange resin VP-1ApB is obtained by N-alkylation of the copolymer according to the method of Example 1.

Physico-chemical properties of the anion exchanger obtained: complete C1 exchange capacity of the ion 4.8 mg-eq / g; specific volume of anion exchanger swollen in water 3.1 ml / g; mechanical strength of anion exchanger swollen in water for 1 h 99%, for 6 h 99%.

Example 5. In the reaction flask load 270,0 MAH. A 1% starch solution containing 240 g / l of sodium chloride, 0.086 g of metol and with stirring a mixture consisting of 86.6 parts by weight. Profit center (content of the main product is 90%), 20.0 ma.h. Technical DVB (content of the main product 50%), 2.0 mach.ch. benzoyl peroxide,

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1b, and ma.ch. butyl acetate and 15.0 m.h. alkylbenzene (15 and 15% by weight of monomers).

The copolymerization reaction is carried out according to the method described in Example 1. The strongly basic anion exchange resin VP-1AbB is obtained by N-alkylation of the copolymer according to the method of Example 1.

Physico-chemical properties of the anion exchanger obtained: total C1-ion exchange capacity 4.8 mg-eq / g; specific volume of anion exchanger swollen in water 3.0 ml / g; mechanical strength of swollen anion exchanger for 1 h 99%, for 6 h 99%.

Example 6. In the reaction flask load 270,0 MAH. 1% starch solution containing 240 g / l of sodium chloride, 0.086 may. a mixture consisting of 86.6 parts by weight was introduced with stirring. Profit center (content of the main product is 90%), 20.0 ma.ch. Technical DVB (content of the main product 50%), 2.0 mach.ch. benzoyl peroxide, 25.0 ma.ch. butyl acetate 20.0 mas. h. (20 and 20% by weight of monomers) alkylbenzene. The copolymerization reaction is carried out according to the method described in Example 1.

The strongly basic anion exchange resin HMAPB is obtained by N-alkylation of the copolymer according to the method of Example 1.

Physico-chemical properties of the anion exchanger obtained: total C1-ion exchange capacity 4.7 mg-eq / g: specific anion-exchange resin swelled in water 3.2 ml / g; mechanical strength of swollen anion exchanger for 1 h 93%, for 6 h 80%.

Examples 7-11. Carried out as in example 1, but using different amounts of solvents.

The obtained strong-base anions of VP-1ApT and VP-1AbB are subjected to repeated contacts with freshly alkaline acid pulp of aluminosilicate ore under equal conditions. A portion of the pulp is replaced every 24 hours.

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The total contact time is 2400 hours. Every 480 hours of contact with the pulp, anion exchange resin is analyzed for its silica content. In addition, after 480, 1440 and 2400 hours of contact, an anion exchange sample is taken from the process and its sorption capacity for molybdenum is determined from a solution of the following composition, g / dm: molybdenum 0.3; iron hydroxide 6.8; sulfate ion 30. The ratio of anion exchange resin. solution 3: 250ml / ml. The duration of saturation 24 hours, pH 2.0-2.5. The results are shown in Table. one.

The study of the dependence of the mechanical strength of anion exchangers on the amount of a pore-forming agent — a mixture of solvents (solvent — precipitator and solvent of solvation type) is carried out with repeated alternating treatment of anion exchangers with acid (10%) and carbonate (10% NazC09) solutions with the duration of each treatment 6 hours

The test results of anion exchangers VI-1App and VP-1ApB in comparison with the base object anionite VP-1Ap are presented in Table. 2

Claims (1)

Formula of the present The method of producing anion exchangers by suspension copolymerization of 2-methyl-5-β-vinylpyridine and divinylbenzene in the presence of a pore-forming solvent followed by the introduction of anionic groups, characterized in that in order to reduce poisoning of anion exchangers with silicic acid and preserve their mechanical strength during operation , a mixture of toluene or butyl acetate with alkylbenzene is used as a pore-forming solvent with a content of 10–20% in a mixture of toluene or butyl acetate, and 15–20% of alkylbenzene. aces monomer mixture. When tagging. k - test case; - the duration of grinding of anion exchange resin in a ball mill.