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Method for preparing dimethyl carbonate by transesterification

A technology of dimethyl carbonate and transesterification, which is used in the preparation of organic carbonates, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., and can solve the problems of rapid decline in activity and easy swelling of resin catalysts. , to achieve the effect of enhancing swelling resistance

Active Publication Date: 2018-01-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is that there are problems in the prior art that the resin catalyst is easy to swell and the activity drops rapidly, and a new method for preparing dimethyl carbonate by transesterification is provided

Method used

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  • Method for preparing dimethyl carbonate by transesterification
  • Method for preparing dimethyl carbonate by transesterification
  • Method for preparing dimethyl carbonate by transesterification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 58.0 grams of styrene, 0.6 grams of divinylbenzene, 30 grams of polystyrene and 0.6 grams of benzoyl peroxide initiator in a 500 milliliter three-necked flask, and stir for 2.0 hours at 60°C; then add 2.8 grams of multi-walled carbon Nanotubes, continue stirring for 1 hour for pre-polymerization. 260 mL of deionized water in which 2.5 g of polyvinyl alcohol had been dissolved was added. Adjust the stirring speed, and at the same time gradually raise the temperature to 80°C, and react for 5 hours; then raise the temperature to 90°C, react for 5 hours, and finally raise the temperature to 98°C, and react for 6 hours. After the reaction, pour out the upper liquid, wash with 85°C hot water, then wash with cold water, then filter, put in an oven to dry at 80°C, sieve, and collect composite microspheres with a particle size within the range of 0.35 to 0.60 mm a.

[0032] Chloromethylation of composite microspheres: In a 500-ml three-necked flask, add 50 grams of composi...

Embodiment 2

[0036] In a 500 milliliter three-necked flask, add 20 grams of compound chlorine spheres A obtained in [Example 1], 150 milliliters of tetrahydrofuran, and 35.0 grams of tributylamine, stir and react under reflux for 30 hours, filter and remove the mother liquor after the reaction, and Wash with dichloromethane, acetone and water in sequence, and dry under vacuum to obtain chlorine-type nanocomposite quaternary ammonium salt resin A3.

[0037] The transformation of chlorine-type nanocomposite quaternary ammonium resin: in a 200 milliliter beaker, add 10 grams of chlorine-type nanocomposite quaternary ammonium resin A3, 20 grams of Ba(OH) 2 And 40 grams of deionized water, after stirring at room temperature for 18 hours, filter, wash with deionized water, repeat the above process 2 times, filter, wash with deionized water, dry under vacuum to obtain strong alkali type nano-composite quaternary ammonium salt Resin A4.

Embodiment 3

[0039] Add monomer mixture solution (60.0 gram styrene, 1.7 gram divinylbenzene, 60 gram polystyrene, 1.6 gram multi-walled carbon nanotube and 1.0 gram benzoyl peroxide containing initiator in 500 milliliters of three-necked flasks, The solution was first stirred and reacted at 70°C for 0.5 hours), started the agitator, added a mixed solution of 200 milliliters of deionized water and 5 grams of gelatin, raised the temperature to 85°C, reacted for 3 hours, then raised the temperature to 90°C, reacted for 9 hours, and finally The temperature was raised to 100° C., and the reaction was carried out for 10 hours. After the reaction, pour out the upper liquid, wash with 85°C hot water, then wash with cold water, then filter, put in an oven to dry at 80°C, sieve, and collect composite microspheres with a particle size within the range of 0.35 to 0.60 mm b.

[0040] Chloromethylation of composite microspheres: In a 500-ml three-necked flask, add 50 grams of composite microspheres B ...

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Abstract

The invention relates to a method for preparing dimethyl carbonate by transesterification, which mainly solves the problems in the prior art that the resin is easy to swell and the activity decreases rapidly. The present invention adopts the conditions that ethylene carbonate and methanol are used as reaction raw materials, the reaction temperature is 60-160° C., the molar ratio of methanol to ethylene carbonate is 2-10, and the weight ratio of catalyst to ethylene carbonate is 0.005-1. Under this condition, the raw material is contacted with the catalyst for 1 to 8 hours to obtain dimethyl carbonate; wherein, the technical solution of the catalyst being a strong base type nanocomposite quaternary ammonium salt resin solves this problem well, and can be used for ethylene carbonate and methanol In the industrial production of dimethyl carbonate prepared by transesterification.

Description

technical field [0001] The invention relates to a method for preparing dimethyl carbonate by transesterification. Background technique [0002] Dimethyl carbonate (DMC) has lively chemical properties, excellent physical properties, and is non-toxic and easy to biodegrade. Electrolyte and carbonylation, methylation and carbonyl methoxylation reagents are widely used in chemical industry. At present, all countries are actively studying the green chemical process based on DMC, an environmentally friendly chemical raw material. Among them, the transesterification method has become a method with great industrial prospects because of mild reaction conditions, high yield and co-production of ethylene glycol or propylene glycol. [0003] Generally speaking, alkali metal hydroxides, alkali metal carbonates, and alkali metal alcohols (F.Risse et al., US2011040117; C.P.Allais et al., WO2010063780) are used as catalysts for transesterification reactions, but because of their Homogene...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/96C07C68/06B01J31/08
Inventor 陈梁锋何文军
Owner CHINA PETROLEUM & CHEM CORP
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