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Preparation method of cation exchange resin with high-temperature thermostability

A cation exchange and stability technology, which is applied in the field of cation exchange resin preparation, can solve the problems of ion exchange resin exchange capacity decline, demanding polymerization equipment, low polymerization efficiency, etc., to achieve improved dispersion stability, increased initiation efficiency, high Yield effect

Inactive Publication Date: 2014-01-15
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The addition of dichloroethane dilutes the concentration of sulfuric acid on the one hand, so that the exchange capacity of the ion exchange resin finally obtained is reduced; The process recycles it, which increases energy consumption
This method adopts conventional benzoyl peroxide as an initiator in the polymerization stage, and the polymerization efficiency is relatively low, and the pressure polymerization is adopted, which requires relatively harsh requirements on the polymerization equipment; high energy consumption

Method used

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  • Preparation method of cation exchange resin with high-temperature thermostability
  • Preparation method of cation exchange resin with high-temperature thermostability
  • Preparation method of cation exchange resin with high-temperature thermostability

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Polymerization: In a 1000mL four-necked flask equipped with a stirring, reflux condenser and thermometer, add 550g of water, 0.7g of polyvinyl alcohol with an alcoholysis degree of 70%, and 0.1g of hydroxypropyl methylcellulose, heating and stirring, It dissolves completely and forms a homogeneous aqueous solution. Warm up to 45℃, add 4g of methine blue aqueous solution with a mass concentration of 0.4%, then add 100g of styrene (styrene content ≥99%), 75g of divinylbenzene (divinylbenzene content of 50%), 44g Liquid paraffin, 0.8g tert-butyl peroxyneodecanoate, 0.4g tert-amyl peroxypivalate, the organic phase mixture, adjust the appropriate stirring speed, heat to 65℃, react at constant temperature for 2 hours, and then heat to 80 ℃, constant temperature reaction for 4 hours. The reaction product was filtered, and then placed in 3 times the volume of tap water and stirred for 5 minutes, washed the residual dispersant, filtered, so washed and filtered three times, and d...

Embodiment 2

[0055] Polymerization: In a 1000mL four-necked flask equipped with stirring, reflux condenser and thermometer, add 450g water, 2.6g gelatin, 0.3g polystyrene-maleic anhydride ammonium salt, heat and stir to make it completely dissolved and form a uniform Add 1mL of 0.4% methine blue aqueous solution and 12g potassium chloride. Heat to 45℃, add 104g styrene (styrene content≥99%), 96g divinylbenzene (divinylbenzene content 50%), 60g 36# white oil, 1.0g lauryl peroxide and 0.6g For the organic phase mixture composed of benzoyl peroxide, adjust the appropriate stirring speed, heat up to 65°C, react at a constant temperature for 3 hours, then heat up to 85°C, react at a constant temperature for 4 hours. The reaction product was filtered, and then placed in 3 times the volume of tap water and stirred for 5 minutes, washed the residual dispersant, filtered, so washed and filtered three times, and dried at room temperature (water content ≤ 3%) to obtain a dry copolymer 230g white ball...

Embodiment 3

[0062] Polymerization: styrene-divinylbenzene copolymerization was carried out in the same way as in Example 1, except that 1.16g tert-butyl peroxyneodecanoate was used as the initiator instead of 0.8g tert-butyl peroxyneodecanoate and 0.4g peroxide A mixture of tert-amyl pivalate. 198g of dried white copolymer balls were obtained, of which the particle size ranged from 0.3mm to 1.0mm, accounting for 89.6%.

[0063] Porogen extraction: The same method as in Example 1 was used to perform porogen extraction on 100 g of white copolymer balls, except that the number of solvent extractions was increased from 20 to 25. 77.6g of dry copolymer white balls with suitable pore structure were obtained, and the content of volatile matter was less than 1%.

[0064] Bromination: In a 5L enamel kettle, add 500g of dry copolymer white balls with suitable pore structure, 2500mL of dichloroethane, and 32g of iron powder, stir and swell for 3 hours, and use an ice water bath to reduce the temperature...

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Abstract

The invention belongs to the field of chemical synthesis, and particularly relates to a preparation method of cation exchange resin with high-temperature thermostability. C5-C40 saturated alkane is used as a pore-foaming agent, an efficient initiator is used, styrene and polyethylene monomer are copolymerized in a suspension state so as to prepare a styrene-polyethylene benzene copolymer white ball containing the pore-foaming agent, and then the pore-foaming agent and low-molecular-weight impurities in the copolymer are extracted by an organic solvent, so that a macroporous copolymer with an appropriate pore structure is formed. A mixture of the extracted pore-foaming agent and the organic solvent is simply distilled and separated, and then, the pore-foaming agent and the organic solvent both are recyclable. In the presence of the catalyst, the white ball subjected to extraction is further treated with halogenating reaction. The halogenating product can directly generate sulfonation reaction without being reamed by dichloroethane, then, the high-temperature resistant macroporous cation exchange resin is obtained. The resin has uniform pore size distribution and high strength, and has higher catalytic activity and longer service life when being used in high temperature organic catalytic reaction.

Description

Technical field [0001] The invention belongs to the field of chemical synthesis, and specifically relates to a method for preparing a cation exchange resin with high temperature thermal stability. Background technique [0002] Styrene-based macroporous strong acid cation exchange resins are widely used in acid-catalyzed organic chemical reactions such as etherification, esterification, alkylation, hydration, dehydration, etherolysis, and hydrolysis. However, some chemical reactions need to be carried out at higher temperatures, such as esterification, alkylation, dehydration and other reactions. The reaction temperature is generally above 130°C. The maximum heat resistance temperature of conventional ion exchange resins is only 120°C, which exceeds this temperature. It will cause the active group to fall off quickly and become inactivated. [0003] In the organic catalytic reaction, the active group of the ion exchange resin for catalysis is the sulfonic acid group on the benzene ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08C08F212/36C08F8/36C08F8/22C08J9/28B01J39/20
Inventor 于永玲吕爱梅李留忠
Owner CHINA PETROLEUM & CHEM CORP
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