Preparation method for high temperature resistant macroporous cation exchange resin catalyst

A technology of macroporous cation and exchange resin, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., which can solve problems such as environmental pollution, no improvement in service life, and increased energy consumption, and achieve economical improvement. Improvement of performance, dispersion stability, and reduction of energy consumption

Active Publication Date: 2012-03-14
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
Although the detachment

Method used

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  • Preparation method for high temperature resistant macroporous cation exchange resin catalyst
  • Preparation method for high temperature resistant macroporous cation exchange resin catalyst
  • Preparation method for high temperature resistant macroporous cation exchange resin catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Polymerization: In a 1000mL four-necked flask equipped with stirring, reflux condenser and thermometer, add 400g of water and 0.7g of hydroxymethyl cellulose, heat and stir to dissolve completely and form a uniform aqueous solution. Heat up to 65°C, add 0.03g methylene blue, then add 60g styrene (styrene content ≥ 99%), 50g divinylbenzene (divinylbenzene content 55%), 53g cottonseed oil, 0.9g over Oxidize the organic phase mixture composed of benzoyl, adjust the appropriate stirring speed, raise the temperature to 86°C, and react at constant temperature for 8 hours. The reaction product was filtered and dried at room temperature (water content ≤ 3%) to obtain 160 g of dry polymer white balls, of which 84.8% were polymers with particle sizes ranging from 0.3 mm to 1.0 mm.

[0047] Porogen extraction: Take 120g of dry white balls with a particle size of 0.3mm-1.0mm, put them in a Soxhlet extractor, and connect the extractor to a 2000mL round-bottomed flask containing 1000...

Embodiment 2

[0061] Polymerization: Add 500g of water, 0.8g of carboxymethyl cellulose, and 0.5g of sodium polyacrylate with an average molecular weight of 3 million to a 1000mL four-neck flask equipped with stirring, reflux condenser, and thermometer, heat and stir to dissolve completely , to form a uniform aqueous solution, and then add 0.08g of methylene blue. Be warming up to 75 ℃, add by 124g styrene (styrene content ≥ 99%), 55g divinylbenzene (divinylbenzene content 65%), 72g peanut oil, the organic phase mixture that 1.2g benzoyl peroxide forms, Adjust the stirring speed appropriately, raise the temperature to 86° C., and react at constant temperature for 8 hours. The reaction product was filtered and dried at room temperature (water content ≤ 3%) to obtain 248 g of dry polymer white balls, of which 87.8% were polymers with particle sizes ranging from 0.3 mm to 1.0 mm.

[0062] Porogen extraction: Take 210g of dry white balls with a particle size of 0.3mm~1.0mm, put them in a Soxhl...

Embodiment 3

[0075] Polymerization: In a 1000mL four-neck flask equipped with stirring, reflux condenser, and thermometer, add 500g of water, 0.4g of hydroxyethyl cellulose, and 0.3g of sodium salt of styrene-maleic anhydride copolymer, heat and stir to make it Dissolve completely to form a homogeneous aqueous solution, then add 50g of sodium chloride and 0.05g of methylene blue. Heat up to 65°C, add 50g styrene (styrene content ≥ 99%), 52g divinylbenzene (divinylbenzene content 55%), 55g rapeseed oil, 0.7g organic phase composed of benzoyl peroxide The mixture was adjusted to an appropriate stirring speed, heated to 86° C., and reacted at a constant temperature for 8 hours. The reaction product was filtered and dried at room temperature (water content ≤ 3%) to obtain 155 g of dry polymer white balls, of which 82.7% were polymers with particle sizes ranging from 0.3 mm to 1.0 mm.

[0076] Porogen extraction: Take 120g of dry white balls with a particle size of 0.3mm~1.0mm, put them in a S...

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Abstract

The present invention provides a preparation method for a high temperature resistant macroporous cation exchange resin catalyst. According to the preparation method, a linear chain saturated acid with carbon atoms of 4-25, any one component selected from a unsaturatcd fatty acid glyceride, or a mixture is adopted as a pore-foaming agent to prepare styrene-divinylbenzene copolymer containing the pore-foaming agent, wherein the mixture comprises two or more components selected from the unsaturatcd fatty acid glyceride; an organic solvent is adopted to extract the pore-foaming agent and low molecular weight impurities in the copolymer; the macroporous polymer is subjected to a halogenating reaction in the presence of a catalyst; the resulting halogenated product is subjected to a sulfonationreaction. According to the present invention, the polarity of the used pore-foaming agent by the preparation method of the present invention is similar to the polarity of the monomer, such that uniform porous channels can be formed during the polymerization process; the used materials by the preparation method of the present invention have characteristics of environmental protection, no toxicity,cheap price and easy availability; during the preparation process of the present invention, only a hydrocarbon solvent with low boiling point and low toxicity is adopted to clean the pore structure, such that the operation is simple and three wastes are not discharged; the pore structure-cleaned styrene-divinylbenzene copolymer is subjected to the halogenation and the sulfonation to obtain the resin catalyst with uniform pore structure, good high temperature resistance and high catalytic activity.

Description

technical field [0001] The present invention relates to a preparation method of a high temperature resistant macroporous cation exchange resin catalyst, in particular to a high temperature resistant macroporous cation exchange resin catalyst used for etherification, esterification, alkylation, hydration, etherolysis and other organic catalytic reactions The preparation method of porous strong acid type cation exchange resin. 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, etherolysis, and hydrolysis. However, some chemical reactions need to be carried out at higher temperatures, such as esterification, alkylation, and synthesis of dimethyl ether. The reaction temperature is generally above 130°C, and the maximum heat-resistant temperature of conventional ion exchange resins is only 120°C. Exceeding this temper...

Claims

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Application Information

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IPC IPC(8): B01J31/10B01J37/00C07C43/04C07C41/09
Inventor 于永玲吕爱梅赵居杰毕晓龙车万里范大鹏张勇
Owner CHINA PETROLEUM & CHEM CORP
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