A method of obtaining a sulfonic cation exchanger

 

(57) Abstract:

Usage: obtain sulfonated cation exchange resin based on a copolymer of styrene and divinylbenzene. The inventive swelling with divinylbenzene is carried out in dichloroethane in the presence of 83 88% sulfuric acid, and then at a temperature of 60 To 75°C, add oleum for 5 to 30 min and conduct sulfonation at 90 to 125°C.

The invention relates to the field of production of sulfonated cation exchange resins based on copolymers of styrene and divinylbenzene (DVB) used in water treatment and other ion exchange processes.

Known methods for producing sulfonic cation by sulfanilamide copolymer of styrene and DVB sulfurous agent with the preliminary swelling in organic solvents, mainly aromatic or chlorine substituted hydrocarbons, for example benzene, toluene, xylene, ethylbenzene, chlorobenzene, and so on [1, 2]

A disadvantage of known methods is a clear separation of the stages of pre-swelling of the copolymer in the solvent and subsequent sulfonation. The separation of these stages over time, and sometimes in hardware design, but also the necessity of removal from the reaction mixture a large amount of in the ASS="ptx2">

The closest to the technical nature of the proposed method is a way of conducting emulsion swelling of the copolymer in the environment sulfureuse agent and dichloroethane (EDC) followed by sulfonation of the swollen copolymer [3]

To implement this method, a copolymer of styrene and DVB are mixed in a reactor with 91-95% sulfuric acid, heated to 50-80aboutAnd before or during the heating of injected EDC in the amount of from 0.15 to 1.2 wt.h. 1 wt.h. copolymer. After raising the temperature in the reactor up to 85-95aboutC for 2-2,5 hours start to add 98-99% sulfuric acid, then increase the temperature to 125aboutWith and conduct sulfonation within 3 hours of the Obtained product sulfonation after hydrolysis contains 3-10% of grains with mechanical defects.

However, more stringent quality control sulfonic cation exchanger is evaluated for the percentage of whole pellets after serial (100-fold) treatment with solutions of acid and alkali, i.e., after recyclacie.

The disadvantage of this method is that it has a low osmotic strength, and when exposed to loads of sulfonation destroyed, leading to loss of the cation and reduction of its lifetime.

Espiguette up to 50%

The aim of the invention is to improve the quality of sulfonic cation exchanger, characterized by the percentage of whole pellets after recyclacie.

This goal is achieved by the fact that the swelling of the copolymer of styrene with DVB carried out in dichloroethane in the presence of 83-88% sulfuric acid, and then at a temperature of 60-75aboutTo add oleum within 5-30 min and conduct sulfonation.

P R I m e R 1. In a three-neck flask with stirrer poured 583 cm3uterine sulfuric acid with a concentration of 86% 168 cm3dichloroethane and conduct stirring for 20 minutes In the prepared emulsion load of 300 g of a copolymer of styrene with 8% of divinylbenzene, grain size of 0.25-0.8 mm, and spend emulsion swelling during heating from 20 to 60aboutWith speed 30aboutS/H. With the achievement of the 60aboutTo begin evenly within 30 min of dosing 397 cm3oleum (containing free SO324%), raise the temperature of the reaction mixture to 120aboutWith a speed of 60aboutWith an hour and kept at this temperature for 3 hours Hydration product of sulfonation is conducted with sulfuric acid continuously decreasing concentration of from 85 to 0% Received sulfonation contains not more than 5% damaged pellets. The percentage of whole granules is e for 20 min mix 200 cm388% sulfuric acid and 40 cm3dichloroethane, receiving the emulsion, where to download 100 g of the copolymer of styrene and 8% divinylbenzene (grain size of 0.25-0.8 mm), and spend emulsion swelling during heating from 20 to 70aboutWith speed 30aboutWith in the hour. When reaching the 70aboutFrom start to evenly dispense 110 cm3oleum (free content SO318%) for 20 min, then raise the temperature of the reaction mixture to 120aboutC and maintained at this temperature for 2 h

The hydration product of sulfonation is conducted with sulfuric acid continuously decreasing concentration of from 85 to 0% of the cation exchange resin contains not more than 5% damaged pellets. The number of whole pellets sulfonic cation exchanger after 100 cycles of transfer of N+in Na+form more than 90% of

P R I m e R 3. In the flask for 20 min mix 237 cm3uterine sulfuric acid with a concentration of 83% and 16 cm3dichloroethane. In the prepared emulsion load of 100 g of a copolymer of styrene and 6% of divinylbenzene (grain size of 0.25-0.8 mm) and spend emulsion swelling during heating from 20 to 75aboutWith speed 30aboutWith in the hour. At a temperature of 75aboutFrom start to evenly dispense 201 cm3oleum (18% free SO3in taratala product of sulfonation is conducted with sulfuric acid continuously decreasing concentration of from 85 to 0% of the cation exchange resin contains not more than 5% damaged grains. The number of whole granules in the cation exchanger after 100 cycles of transfer of N+in Na+form more than 90%

A method of OBTAINING a sulfonic cation exchanger by the swelling of the copolymer stired with divinylbenzene in dichloroethane in the presence of sulfuric acid and then adding sulfurous agent and sulphurization at 90 125o, Characterized in that the swelling is carried out in the presence of 83 88% sulfuric acid, then with 60 75oTo add sulfureuse agent oleum for 5 to 30 minutes

 

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