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Method for preparing glycerol carbonate from glycerol and dimethyl carbonate

A technology of glycerol carbonate and dimethyl carbonate, which is applied in the comprehensive utilization of resources and fine chemical industry, and can solve the problems of long reaction time, strong toxicity and high reaction temperature

Inactive Publication Date: 2018-06-29
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The literature [J.Ind.Eng.Chem, 17, 2011, 777-781] uses KF modified hydroxyapatite as a catalyst, which can achieve a high yield of glycerol carbonate, but the toxicity of KF is very strong, which is not conducive to Applied to industrial production
In summary, although some heterogeneous catalysts show good catalytic performance in the reaction of glycerol and dimethyl carbonate to produce glycerol carbonate, there are still many problems, such as poor cycle performance, high reaction temperature, and the need to use solvent, long reaction time, etc.

Method used

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  • Method for preparing glycerol carbonate from glycerol and dimethyl carbonate
  • Method for preparing glycerol carbonate from glycerol and dimethyl carbonate
  • Method for preparing glycerol carbonate from glycerol and dimethyl carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1)La 2 o 3 preparation of

[0017] Weigh 2.1651g La(NO 3 ) 3 .6H 2 O was dissolved in 20mL deionized water to obtain a 0.25mol / L salt solution, and 1.3045g NH 4 HCO 3 Dissolved in 20mL deionized water to obtain a 0.83mol / L precipitant solution, under stirring conditions at room temperature, the NH 4 HCO 3 The solution was added dropwise to La(NO 3 ) 3 .6H 2 In O solution, a milky white suspension was formed. After stirring at room temperature for 6 hours, it was centrifuged to obtain a white precipitate, which was dried in an oven at 110°C for 12 hours and calcined at 800°C for 6 hours to obtain La 2 o 3 catalyst.

[0018] (2) 5% Li-La 2 o 3 Catalyst preparation

[0019] Weigh 0.2429g LiNO 3 , dissolved in 30mL deionized water, weighed 1.0g La after the Li salt was completely dissolved 2 o 3 The carrier was added to the salt solution, stirred and impregnated at room temperature for 12 hours, and then deionized water was removed by rotary evaporation....

Embodiment 2

[0028] (1) Use 5% Li-La 2 o 3 as a catalyst.

[0029] 5%Li-La 2 o 3 The preparation process is the same as in Example 1.

[0030] (2) 5% Li-La 2 o 3 Catalyzed Glycerol and Dimethyl Carbonate Reaction Operation (Changing Catalyst Consumption) and Product Analysis

[0031] Except that catalyst consumption is 0.3g (catalyst / glycerol mass ratio is 0.1), other reaction operations and product analysis are the same as in Example 1, and the reaction results are listed in Table 1.

Embodiment 3

[0033] (1) Use 5% Li-La 2 o 3 as a catalyst.

[0034] 5%Li-La 2 o 3 The preparation process is the same as in Example 1.

[0035] (2) 5% Li-La 2 o 3 Catalyzed Glycerol and Dimethyl Carbonate Reaction Operation (Changing Catalyst Consumption) and Product Analysis

[0036] Except that catalyst consumption is 0.4g (catalyst / glycerol mass ratio is 0.133), other reaction operations and product analysis are the same as in Example 1, and the reaction results are listed in Table 1.

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Abstract

The invention relates to a method for preparing glycerol carbonate from glycerol and dimethyl carbonate by adopting Li-La2O3 composite as a catalyst, which belongs to the technical field of resource comprehensive utilization and fine chemical industry. The method is characterized by adopting a Li component to be doped into La2O3 to prepare xLi-La2O3 composite by virtue of an immersion method (x represents the content of the Li component in the composite, and calculating according to the weight percent of Li2O in the xLi-La2O3 compound, x is equal to 1 to 5 percent), the Li-La2O3 composite is used as a catalyst, the glycerol and the dimethyl carbonate are adopted as raw materials, and the glycerol carbonate can be efficiently prepared in the case of no solvent and mild reaction condition. In the process for preparing the glycerol carbonate from the glycerol and the dimethyl carbonate, by utilizing the catalyst and technological method of the invention, high raw material conversion rate,high target product selectivity and high yield can be obtained; and moreover, the catalyst preparation process is easy, and the catalyst is easy to separate from the product and to recycle after thereaction.

Description

technical field [0001] The present invention relates to a kind of Li-La 2 o 3 The composite is a catalyst, and the method for producing glycerol carbonate by using glycerol and dimethyl carbonate as raw materials under mild conditions belongs to the technical field of resource comprehensive utilization and fine chemical industry. Background technique [0002] In recent years, due to the development of biodiesel industry, the output of by-product glycerol has increased year by year, so it is imperative to realize the conversion of glycerol to high value-added chemicals. Among the derivatives of glycerol, glycerol carbonate is a non-flammable, low-toxic, high-boiling and biodegradable substance, and it is also an important cosmetic raw material, which can be used to produce biological lubricants, glycidol , polycarbonate, polyester and polyurethane, etc., have lively chemical reactivity and a wide range of industrial uses. [0003] Synthetic glycerol carbonate has a variety...

Claims

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Application Information

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IPC IPC(8): C07C68/06C07C69/96B01J23/10B01J37/02B01J37/08C01F17/00
CPCB01J23/10B01J37/0201B01J37/08C01F17/206C07C68/06C07C69/96
Inventor 贺德华李亚晋
Owner TSINGHUA UNIV