The method of obtaining slightly basic anion exchange resin

 

(57) Abstract:

Usage: the invention relates to the production of slightly basic anion exchange resin curing type, which can be used in various reactions of ion exchange for water treatment plants nuclear and thermal power plants, sorption, waste acidic gases from chemical plants, adsorption of ions from solution. The invention allows to obtain an ion-exchange resin having a high dynamic exchange capacity (not less than 1000 mol/m3at high osmotic stability (at least 94%) and high resistance to travlemate due to the fact that the copolymerization is performed at a content of divinylbenzene 8,5-12 wt. % concentration of 50-55% in the medium fraction alkylbenzene with the boiling temperature of 80-180oC in the amount of 110-130 wt. % by weight of monomers with the addition of 6% of diethylbenzene by heating and aging at 70oC - 4 h, 80oC - 3 h, 93oC - 2 h followed by chlorotoluene and aminating Diethylenetriamine.

The invention relates to the production of slightly basic, macroporous anion exchange resin curing type, which can be used in various reactions of ion exchange for water treatment plants is ASS="ptx2">

A method of obtaining macroporous of andonico, consisting in the copolymerization of styrene and divinylbenzene in the last 6-7,5 wt. in the presence of 55-70% by weight of monomers of Isobutanol when heated to 75oC and further increase in temperature from 75 to 90oC with a speed of 0.12 to 0.15oC/min, followed by exposure at 90oC for 8-10 hours In the obtained copolymer introduce ionic groups chlorotoluene and aminating (ed. St. N 1312084, class C 08 J 5/20, C 08 F 212/14, published. 23.05.87).

The closest in technical essence to the present invention is a method of obtaining a slightly basic anion exchange resin composed and aminating swollen in an organic solvent klimatisierung copolymer of styrene and divinylbenzene listeriosis connection with this amination is conducted first at 1-10oC for 20-40 minutes under stirring, and then when 40-95oC (ed. St. N 1571050, class C 08 F 212/14, 8/32, C 08 J 5/20, published. 15.06.90).

The described methods do not allow to obtain a resin having a high dynamic exchange capacity (not less than 1000 mol/m3), high resistance to poisoning and a sufficiently high osmotic stability.

The task of the invention is the creation of NISMO is) and which has a high resistance to poisoning by organic substances and high osmotic stability.

The problem is solved due to the fact that when getting slightly basic, macroporous anion exchange resin by copolymerization of styrene with divinylbenzene in the presence of alkylbenzene as pore-forming upon heating and subsequent chlorotoluene and aminating, the copolymerization is carried out at the content of divinylbenzene 8,5-12A wt. the concentration of 50-55% in the medium fraction alkylbenzene with the boiling temperature of 80-180oC in the amount of 110-130 wt. by weight of monomers with the addition of 6% of diethylbenzene by heating and aging at 70oC 4 h, 80oC 3 h, 93oC 2 h followed by chlorotoluene and aminating Diethylenetriamine.

This set of essential features allows you to get slightly basic, macroporous anion exchange resin having a high osmotic stability, high dynamic exchange capacity (not less than 1000 mol/m3and resistance to poisoning by organic substances due to selection of the blowing agent, determine the percentage of styrene and divinylbenzene, determining the mode of chlorotoluene, selection amineralo agent and amination.

Example 1. A. Mixture consisting of 132,9 g of styrene, 25,43 g of divinylbenzene (8.5 wt.) 52,81% concentration, 198 g fra, containing 3,66 g of potato starch. Loading is carried out at 60oC.

The copolymerization is carried out by the program:

within 30 minutes raise the temperature of the mixture to 73oC and kept at this temperature for 4 h;

within 30 minutes, raise the temperature to 80oC and kept at this temperature for 3 h;

within 30 min raise temperature to 93oC and kept at this temperature for 2 h

The resulting copolymer is expressed from the mother liquor, otparivat live steam from the blowing agent and the residual monomers at a temperature of 100oC for 8 h

B. the Dried copolymer obtained by p. A. in the amount of 130 g stand in 572 ml (4,66 wt.h.) within one hour at room temperature, add 110,5 g of titanium tetrachloride at a temperature not exceeding 20oC, then raise the temperature to 42oC and kept at this temperature for 6 hours Klimatisierung copolymer is washed with metallum to weakly acid reaction, wring out from matilla, then add 585 g (4.5 wt.h. on copolymer) Diethylenetriamine concentration of not less than 90% Amination carried out for 3 h at 50oC by distillation from the reaction environment metallicana 4 hours Slightly basic anion exchange resin is washed with hot (90oC) demineralized water until the pH of the wash water is equal to 8, and analyze.

The resulting anion exchange resin has an osmotic stability 100% dynamic exchange capacity of 1320 mol/m3.

Example 2. A. Mixture consisting of 125,3 g of styrene, 25,65 g (9 wt.) divinylbenzene 52,7% concentration, the fraction of alkylbenzene 166 g (110%), and 9.1 g (6 wt. ) diethylbenzene and 1.06 g of benzoyl peroxide, load in 326 g of an aqueous solution containing 3,26 g of potato starch. Loading is carried out at a temperature of 60oC. the Temperature and time mode copolymerization is carried out, as described in example 1.

B. the Dried copolymer obtained in paragraph a, in the amount of 130 g will chlorotoluron Diethylenetriamine as described in example 1.

The resulting anion exchange resin has an osmotic stability 100% dynamic exchange capacity 1465 mol/m3.

Example 3. A. Mixture consisting of to 120.4 g of styrene, of 35.6 g (12 wt.) divinylbenzene 52,7% concentration, 195 g (125%) fraction of alkylbenzene, 9,36 g (6% ) of diethylbenzene and 1.1 benzoyl peroxide, load in 360 g of an aqueous solution containing 3.6 g of potato starch. Loading is carried out at 60oC. the Temperature and time regimes copolymerisate 130 g will chlorotoluron in the presence of 130 g of titanium tetrachloride and miniroot Diethylenetriamine, as described in example 1.

The resulting anion exchange resin has an osmotic stability 99% dynamic exchange capacity 1200 mol/m3.

Example 4. A. Mixture consisting of 120,4 styrene, 35,6 g (12 wt.) divinylbenzene 52,7% concentration, 195 g (125%) fraction of alkylbenzene and 1.1 g of benzoyl peroxide, load in 350 g of an aqueous solution containing 3.5 g of potato starch. Loading is carried out at 60oC. the Temperature and time regimes carried out as described in example 1.

B. the Dried copolymer obtained under item 1, in the amount of 130 g will chlorotoluron in the presence of 130 g of titanium tetrachloride and miniroot Diethylenetriamine as described in example 1.

The resulting anion exchange resin has an osmotic stability 94% dynamic exchange capacity 1050 mol/m3.

Example 5. A. Mixture consisting of 142.3 g of styrene, of 13.2 g (4.5 wt.) divinylbenzene 52,7% concentration, 194,4 g fraction alkylbenzene, 9,3 (6%) of diethylbenzene and 1.1 g of peroxide benzene, load in 360 g of an aqueous solution containing 3.6 g of potato starch. Loading is carried out at 60oC. the Temperature and the temporary mode copolymerization is carried out as in example 1.

B. the Dried copolymer obtained in paragraph a, in kolichestvo osmotic stability 100% dynamic exchange capacity 850 mol/m3.

Example 6. All, as in example 1, but as amineralo agent used matriliny 40% solution of dimethylamine. Amination was carried out at 45oC for 8 h Received the anion exchange resin was extracted from the mother liquor, washed with hot (50oC demineralized water from the amine to a pH of wash water 8 and analyzed.

The resulting anion exchange resin has an osmotic stability 98% dynamic exchange capacity 760 mol/m3.

The method of obtaining slightly basic anion exchange resin by copolymerization of styrene with divinylbenzene in the presence of alkylbenzene as pore-forming upon heating and subsequent chlorotoluene and aminating, characterized in that the copolymerization is performed at a content of divinylbenzene 8,5 12 wt. a concentration of 50 to 55% in the medium fraction alkylbenzene with a boiling point of 80 - 180oWith the amount of 110 to 130% by weight of monomers with the addition of 6% of diethylbenzene by heating and aging at a temperature of 70o4 h, 80o3 h, 93o2 h followed by chlorotoluene and aminating Diethylenetriamine.

 

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