The method of producing anion exchange resin

 

(57) Abstract:

The invention relates to a method for producing anion exchange resin curing type used in various reactions of ion exchange in water treatment and hydrometallurgy, which allows to increase the osmotic stability and mechanical strength of the resulting anion exchange resin. This method consists in the copolymerization of styrene and divinylbenzene with subsequent chlormethyl-management and aminating, with chlorotoluene carried out by feeding the catalyst is titanium tetrachloride in the form of a donor-acceptor complex with monochloromethyl ether at 20oWith the amount of 0.6 to 1.0 wt.h. 1 weight.h copolymer and then raise the temperature to 42oC and maintained in this mode, 3 hours Such filing catalyst eliminates overheating of the reaction mixture, to reduce the time of chlorotoluene.

The invention relates to the field of production of anion exchange resin curing type, which can be used in various reactions of ion exchange in water treatment and hydrometallurgy.

Known methods for producing anion exchange resin, for example, lies in the fact that klimatisierung copolymer of styrene and giveawaya carried out in the presence of a catalyst (SU, 1571050 A1, 1990).

The closest in technical essence to the present invention is a method of producing anion exchange resin, which consists in the copolymerization of styrene with divinylbenzene in the presence of alkylbenzene as a blowing agent and heating with subsequent processing chlorotoluron means, for example monochloromethyl ether in the presence of a catalyst is titanium tetrachloride, and aminating Diethylenetriamine (EN, 2080338 A1, 20.04.97).

According to the existing technology of production of anion exchange resins using as a catalyst the reaction of chlorotoluene titanium tetrachloride in the reaction mass (swollen in monochloromethyl ether copolymer) directly injected 99.99% of TiCl4. With this input the catalyst is heated by local overheating of the reaction mixture, which leads to deterioration of the strength, and sometimes the capacitive characteristics of the anion due to the additional crosslinking of the copolymer.

The present invention aimed at solving the problems of improving the strength characteristics of the anion - osmotic stability and mechanical strength.

The problem is solved due to the fact that upon receipt of the anion exchanger gel and is the user with the following chlorotoluene and aminating, chlorotoluene carried out by feeding the catalyst is titanium tetrachloride in the form of a donor-acceptor complex with monochloromethyl ether.

This solution - enter the catalyst in the form of a complex industrial environment allows 4 times to reduce the time it was entered in the reaction medium due to smaller ectothermy, reduces local overheating, reduces the possibility of additional crosslinking of the copolymer and, thus, improves the strength characteristics of the resulting anion exchange resin. The anion exchange resin of the gel structure due to removal of additional crosslinking of the copolymers in the process of chlorotoluene have a higher dynamic exchange capacity.

Example 1. A. a Copolymer gel structure in the amount of 100 g stand in 270 ml (2,86 wt.h.) monochloromethyl ether for 1 h at room temperature, add 65 g of titanium tetrachloride at a temperature of t = 20oC, then raise the temperature to 42oC and kept at this temperature for 6 hours Obtained klimatisierung copolymer is washed from the byproducts of the reaction metallum.

B. Klimatisierung copolymer obtained in paragraph a, miniroot 500 ml of 25% aqueous-metallinou solution is imacillin filtering and then washed with water.

The osmotic stability of the obtained anion exchange resin 93%, dynamic exchange capacity of 700 g-mol/cubic meters

Example 2. A. a Copolymer gel patterns of the same party as in example 1, 100 g incubated in 200 ml monochloromethyl ether for 1 h at room temperature, was added when the temperature t = 20oC complex of titanium tetrachloride with monochloromethyl ether, consisting of a mixture of 65 G. of TiCl4and 70 ml monochloromethyl ether, then raise the temperature to 42oC and kept at this temperature for 6 hours Obtained klimatisierung copolymer is washed from the byproducts of the reaction metallum.

B. Klimatisierung copolymer obtained in paragraph a, miniroot solution of trimethylamine as described in example 1.

The osmotic stability of the obtained anion exchange resin to 98.5% dynamic exchange capacity of 720 g-mol/cubic meters

Example 3. A. Copolymer porous structure with a grain size 0,63 of-1.6 mm in the amount of 100 g stand in 440 ml (4,66 wt.h.) monochloromethyl ether for 1 h at room temperature, add 95 g of titanium tetrachloride at a temperature of t = 20oC, then raise temperaturowych reaction products by metallum.

B. Klimatisierung copolymer obtained in paragraph a, miniroot 27% water-mecillinam solution of dimethylamine in an amount of 500 ml at a temperature of 42oC for 3 h the resulting anion exchange resin is separated from the excess dimethylamine by filtration, and then washed with water.

After 10 cycles of sequential processing of the anion solutions of 1 N H2SO4and 1 N Paon osmotic stability of the anion 94%, the mechanical strength of 95%.

Example 4. A. Copolymer porous structure of the same batch as in example 3, 100 g stand in 340 ml monochloromethyl ether (3.6 wt.h.) for 1 h at room temperature, was added when the temperature t = 20oC complex of titanium tetrachloride with monochloromethyl ether, consisting of a mixture of 95 g of titanium tetrachloride and 100 ml monochloromethyl ether, then raise the temperature to 45oC and kept at this temperature for 4 h Obtained klimatisierung copolymer is washed from the byproducts of the reaction metallum.

B. Klimatisierung copolymer obtained in paragraph a, miniroot solution of dimethylamine as described in example 3.

After 10 cycles of sequential processing of the anion exchanger 1 N H2SO4

B. Klimatisierung copolymer obtained in paragraph a, miniroot 96% Diethylenetriamine in 400 ml according to the following modes:

the distillate matilla at a temperature of t = 50oC for 3 h;

temperature rise for 30 min to 90oC and holding at that temperature for 5 hours

The resulting anion exchange resin is separated by filtration from excessive Diethylenetriamine, and then washed with water.

The resulting anion is the osmotic stability of 80%.

Example 6. A. Copolymer porous structure of the same batch as in example 5, chlorotoluron as described in example 4.

B. Received by klimatisierung copolymer miniroot as described in example 5. The resulting anion is the osmotic stability of 97%.

The method of producing gel anion exchange resin and a porous structure by copolymerization of styrene with divinylbenzene, followed by processing chlorotoluron means in the presence of a catalyst and aminating, characterized in that the catalyst used donor-CBL is P>oC in an amount of 0.6oC 1,0 wt.h. 1 weight. 'clock copolymer, then raise the temperature to 42oC and kept at this temperature for 6 hours

 

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