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Method for preparing glycerol carbonate by using mixed catalyst

A technology of glycerin carbonate and mixed catalyst, which is applied in the field of preparation of glycerol carbonate, can solve the problems of low purity of finished glycerol carbonate, expensive ionic liquid, poor filtration effect, etc., achieve high conversion rate, mild reaction process, The effect of high product purity

Active Publication Date: 2022-07-26
ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ionic liquids are expensive, and the latter two involve the separation of catalysts
Wherein the heterogeneous catalyst usually adopts CaO, and the CaO in the reaction solution is usually directly filtered out at present, but the filtering effect is poor, which makes the purity of the finished product glycerol carbonate not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. In a 1000ml three-necked flask equipped with a thermometer, agitation, and a condenser, add catalysts: CaO mass 0.8g, Ca(OH) 2 Mass 1.2g; Glycerol: Mass 230g, Moisture Content 280ppm; Dimethyl Carbonate: Mass 675g, Moisture Content 80ppm. After the feeding is completed, the temperature is raised to a reflux temperature of 74° C. while stirring, and the reflux temperature is maintained for 2 hours to obtain a reaction solution containing glycerol carbonate. 2. Cool the reaction solution to room temperature, add 7.2 g of glacial acetic acid, and 2065 g of dimethyl carbonate as an organic solvent, stir for 2 h and filter to obtain 2916 g of filtrate. 3. Add 295g of deionized water to the filtrate to wash and separate, the organic layer: 2743g, the water layer: 458g; the organic layer is vacuum concentrated to remove the solvent, the vacuum degree is: -0.098Mpa, the product obtained: 195g, GC purity: 96.5%. 4. The water layer is concentrated by rotary evaporation in an ...

Embodiment 2

[0028] 1. In a 1000ml three-necked flask equipped with a thermometer, stirring and condensation tubes, add catalysts: CaO mass 1.2g, Ca(OH) 2 Mass 0.6g; Glycerol: Mass 230g, Moisture Content 260ppm; Dimethyl Carbonate: Mass 675g, Moisture Content 150ppm. After the feeding is completed, the temperature is raised to a reflux temperature of 61° C. while stirring, and the reflux temperature is maintained for 6 hours to obtain a reaction solution containing glycerol carbonate. 2. Cool the reaction solution to room temperature, add 6.7 g of formic acid, and 3245 g of dichloroethane as an organic solvent, stir for 2 h and filter to obtain 4121 g of filtrate. 3. Add 490g of deionized water to the filtrate for washing and separating, the organic layer: 3953g, the water layer: 647g; the organic layer is vacuum concentrated to remove the solvent, the vacuum degree is: -0.098Mpa, the obtained product: 192g, GC purity: 97.8%; 4. The water layer was concentrated by rotary evaporation in an...

Embodiment 3

[0030] 1. In a 1000ml three-necked flask equipped with a thermometer, stirring and condensation tubes, add catalysts: CaO mass 1.1g, Ca(OH) 2 Mass 2.2g; Glycerol: Mass 230g, Moisture Content 370ppm; Dimethyl Carbonate: Mass 675g, Moisture Content 136ppm. After the feeding is completed, the temperature is raised to a reflux temperature of 68° C. while stirring, and the reflux temperature is maintained for 4.5 hours to obtain a reaction solution containing glycerol carbonate. 2. Cool the reaction solution to room temperature, add 7.75g of concentrated sulfuric acid, 2655g of organic solvent diethyl carbonate, stir for 2h and filter to obtain 3526g of filtrate. 3. Add 390g of deionized water to the filtrate for washing and separating, the organic layer: 3364g, the water layer: 545g; the organic layer is vacuum concentrated to remove the solvent, the vacuum degree is: -0.1 Mpa, the obtained product: 193g, GC purity: 96.7%; 4. The water layer was concentrated by rotary evaporation...

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PUM

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Abstract

The invention discloses a method for preparing glycerol carbonate by using a mixed catalyst. 2 The mixture; be warming up to 60~75 ℃ while stirring, obtain the reaction solution containing glycerol carbonate after the insulation reaction; 2. After the reaction solution is cooled to normal temperature, add an organic solvent for dissolving glycerol carbonate, and for reacting with the catalyst 3. The filtrate is washed with deionized water, layered to obtain an aqueous layer and an organic layer, and the organic layer is vacuum concentrated to remove the solvent to obtain the finished glycerol carbonate. The present invention has the advantages of mild reaction process, high conversion rate and high product purity.

Description

technical field [0001] The present invention relates to the technical field of preparation of glycerol carbonate. Background technique [0002] Glycerol carbonate is a small molecular substance with bifunctional groups (five-membered ring and hydroxyl group). Because of its easy biodegradation, high boiling point, low toxicity, odorless, non-polluting, non-corrosive, non-flammable and other characteristics, it is widely used. It is used in various fields such as medicine, textile, cosmetics, polyurethane, paint, plastic, new energy and so on. [0003] The synthesis methods of glycerol carbonate mainly include: phosgene method, carbonylation method (carbon monoxide and carbon dioxide), urethane method and transesterification method. Among them, the phosgene method uses highly toxic phosgene, which is not conducive to industrialization; the conversion rate of the carbonylation method is too low; although the raw materials of the urethane method are cheap and easy to obtain, t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/36B01J23/02
CPCB01J23/02C07D317/36
Inventor 卢云龙常楠时二波岳立陈明凯印李达程勇
Owner ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD