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Preparation method of catalyst applied to preparation of propylene carbonate from CO2 and epoxypropane

A technology of propylene carbonate and propylene oxide, which is applied in the field of catalyst preparation, can solve the problems of small heterogeneous catalyst particles, unsuitability for fixed bed process, easy loss of active components, etc., and achieve high temperature, high activity, high activity and stability Cost-effective, beneficial to filling effect

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] However, the catalysts currently used are not suitable for use in fixed-bed reactors, and the catalysts supported by inorganic ions such as alkali metal ions have the problem of easy loss of active components
For catalysts grafted with quaternary ammonium salts or ionic liquids, the particles of the usual grafted carrier (such as resin, silica microspheres or chitosan) are small, resulting in too small particles of heterogeneous catalysts, which are not suitable for fixed-bed processes

Method used

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  • Preparation method of catalyst applied to preparation of propylene carbonate from CO2 and epoxypropane
  • Preparation method of catalyst applied to preparation of propylene carbonate from CO2 and epoxypropane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 30 g of chlorine balls, 5 g of 1-methylimidazole and 180 g of toluene into a three-necked flask, and reflux at 110° C. for 24 hours. After filtration, it was washed three times with toluene, propylene carbonate and water respectively, and then vacuum-dried at 60° C. for 12 hours to obtain active component A1.

[0030] Grind and mix 18g of A1 with 12g of zinc bromide, 38g of phenolic resin and 3.8g of urotropine to make powder, and sieve at 120 mesh. Then tablet molding, the pressure during tablet pressing was 14MPa, and the holding time was 4 minutes to prepare the active precursor B1.

[0031] The active precursor B1 was heated at 180 °C for 2 hours under the protection of nitrogen. Then crush it into 20-40 mesh particles to make catalyst C1. The composition of catalyst C1 is listed in Table 1.

Embodiment 2

[0033] Add 30 g of chlorine balls, 10 g of 1-methylimidazole and 180 g of toluene into a three-necked flask, and reflux at 110° C. for 24 hours. After filtration, it was washed three times with toluene, propylene carbonate and water respectively, and then dried under vacuum at 60° C. for 12 hours to obtain active component A2.

[0034]Grind and mix 18g of A2 with 20g of zinc bromide, 40g of phenolic resin and 4.0g of urotropine to make a powder and sieve it at 120 mesh. Then tablet molding, the pressure during tablet pressing was 14MPa, and the holding time was 4 minutes to prepare the active precursor B2.

[0035] The active precursor B2 was heated at 180 °C for 2 hours under the protection of nitrogen. Then crush it into 20-40 mesh particles to make catalyst C2. The composition of catalyst C2 is listed in Table 1.

Embodiment 3

[0037] Add 30 g of chlorine balls, 10 g of 1-methylimidazole and 200 g of toluene into a three-necked flask, and reflux at 110° C. for 24 hours. After filtration, it was washed three times with toluene, propylene carbonate and water respectively, and then dried under vacuum at 60° C. for 12 hours to obtain active component A3.

[0038] Grind and mix 18g of A3 with 24g of zinc bromide, 60g of phenolic resin and 4.8g of urotropine to make a powder and sieve it at 120 mesh. Then tablet molding, the pressure during tablet pressing is 14MPa, and the time of holding is 4 minutes, and active precursor B3 is obtained.

[0039] The active precursor B3 was heated at 180° C. for 2 hours under the protection of nitrogen. Then crush it into 20-40 mesh particles to make catalyst C3. The composition of catalyst C3 is listed in Table 1.

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Abstract

The invention discloses a preparation method of a catalyst applied to preparation of propylene carbonate from CO2 and epoxypropane. The preparation method comprises the following steps: (1) reflowing alkyl imidazole and chloromethyl polystyrene microspheres in a methylbenzene solvent for 12-36 hours, filtering, washing with methylbenzene and propylene carbonate respectively, performing vacuum drying for 12-24 hours at 60-80 DEG C to prepare an active component A; (2) crushing and mixing the active component A together with zinc salt, phenolic resin and methenamine to obtain powder, tabletting and moulding to obtain an active precursor B; (3) heating the active precursor B for 0.5-4 hours at 120-200 DEG C under the production of nitrogen, and crushing the active precursor B into 20-40-mesh particles to obtain a catalyst C. The catalyst prepared by the preparation method achieves catalytic reaction for stably synthesizing the propylene carbonate from CO2 and epoxypropane by a long period on a fixed bed reactor.

Description

technical field [0001] The present invention relates to a CO 2 Prepare the preparation method of the catalyst of propylene carbonate with propylene oxide, specifically relate to CO on a kind of fixed-bed reactor 2 Process for the preparation of a catalyst for the preparation of propylene carbonate with propylene oxide. Background technique [0002] The reaction of cycloaddition of propylene oxide and carbon dioxide to generate propylene carbonate is an exothermic and volume-shrinking reaction, and the product propylene carbonate is an excellent organic solvent and organic synthesis intermediate. The reaction is to achieve CO 2 important way to reduce emissions. [0003] KI and TEABr are the most commonly used homogeneous catalysts. Its conversion rate and selectivity are high under high pressure. Quaternary ammonium and phosphonium salts such as octadecyltrimethylammonium bromide and tricyclohexylphosphine are good catalysts. Improving the ionization degree of the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/26C07D317/36
Inventor 张志智方向晨孙万富张喜文孙潇磊杨超陈楠鲁娇
Owner CHINA PETROLEUM & CHEM CORP
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