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Method for preparing dipropyl carbonate through catalytic synthesis by using alkaline ionic liquid

A technology of dipropyl carbonate and basic ions is applied in the field of preparation of basic ionic liquid catalyzed synthesis of dipropyl carbonate, and can solve the problems of low catalyst efficiency, low yield of dipropyl carbonate, cumbersome recycling and the like, and achieves the The effect of reduced catalytic performance, good thermal stability, and high selectivity

Inactive Publication Date: 2012-03-28
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The used catalyzer of bibliographical report mainly contains gac-loaded potassium carbonate etc. at present, and these catalyzers efficiency is lower, and mostly recycling is comparatively loaded down with trivial details, and the yield of the product dipropyl carbonate of final gained is low etc. shortcoming, and yield is only 30% ~40%

Method used

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  • Method for preparing dipropyl carbonate through catalytic synthesis by using alkaline ionic liquid
  • Method for preparing dipropyl carbonate through catalytic synthesis by using alkaline ionic liquid
  • Method for preparing dipropyl carbonate through catalytic synthesis by using alkaline ionic liquid

Examples

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Effect test

Embodiment 1

[0030] A kind of preparation method of alkaline ionic liquid catalytic synthesis dipropyl carbonate, specifically comprises the following steps:

[0031] (1) In a 250mL four-neck flask equipped with a stirrer, a thermometer, a condenser, and a constant pressure dropping funnel, add 24g of n-propanol and 2% of the total mass of reactants 1-butyl-3-methyl hydroxide Imidazolium salt catalyst, heated to 90°C, slowly and uniformly added 9g of dimethyl carbonate dropwise, and transesterified for 1h;

[0032] (2) Connect the water separator to the device in step (1), raise the temperature to 100°C to evaporate the methanol generated by the reaction, continue the transesterification reaction for 3 hours, then cool to room temperature, control the vacuum degree to 20mmHg and carry out vacuum distillation for 20 After min, let stand and stratify;

[0033] (3), the upper layer liquid obtained after static layering in step (2) is then subjected to vacuum distillation, the vacuum degree o...

Embodiment 2

[0039] A kind of preparation method of alkaline ionic liquid catalytic synthesis dipropyl carbonate, specifically comprises the following steps:

[0040] (1) In a 250mL four-neck flask equipped with a stirrer, a thermometer, a condenser, and a constant pressure dropping funnel, add 24g of n-propanol and 2% of the total mass of reactants 1-butyl-3-methyl hydroxide Imidazolium salt catalyst, heated to 90°C, slowly and uniformly added 9g of dimethyl carbonate dropwise, and transesterified for 1h;

[0041](2) Connect the water separator to the device in step (1), raise the temperature to 100°C to evaporate the methanol generated by the reaction, continue the transesterification reaction for 4 hours, then cool to room temperature, control the vacuum degree to 20mmHg and carry out vacuum distillation for 20 minutes After that, let stand to stratify;

[0042] (3), the upper layer liquid obtained after static layering in step (2) is then subjected to vacuum distillation, the vacuum d...

Embodiment 3

[0045] A kind of preparation method of alkaline ionic liquid catalytic synthesis dipropyl carbonate, specifically comprises the following steps:

[0046] (1) In a 250mL four-neck flask equipped with a stirrer, a thermometer, a condenser, and a constant pressure dropping funnel, add 24g of n-propanol and 3% of the total mass of reactants 1-butyl-3-methyl hydroxide Imidazolium salt catalyst, heated to 90°C, slowly and uniformly added 9g of dimethyl carbonate dropwise, and transesterified for 1h;

[0047] (2) Connect the water separator to the device in step (1), raise the temperature to 100°C to evaporate the methanol generated by the reaction, continue the transesterification reaction for 4 hours, then cool to room temperature, control the vacuum degree to 20mmHg and carry out vacuum distillation for 30 After min, let stand and stratify;

[0048] (3), step (2) The upper layer liquid obtained after the static layering is then subjected to vacuum distillation, the vacuum distill...

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Abstract

The invention discloses a method for preparing dipropyl carbonate through catalytic synthesis by using alkaline ionic liquid, which is implemented through the steps of: in an inert gas environment, taking the alkaline ionic liquid as a catalyst, after carrying out ester exchange reaction on normal propyl alcohol and dimethyl carbonate, removing methanol and the catalyst in the obtained product, and then collecting colorless liquid fractions (85-90 oC) so as to obtain the dipropyl carbonate, wherein the adopted catalyst is green, environmental-friendly and reusable alkaline ionic liquid which is a 1-butyl-3-methylimidazolium imidazole salt, a 1-butyl-3-methylimidazolium hydroxide or a 1-butyl-3-methylimidazolium acetate. In the method for preparing dipropyl carbonate through catalytic synthesis by using alkaline ionic liquid disclosed by the invention, a product dipropyl carbonate is relatively easy to separate from the catalyst alkaline ionic liquid, the operation process is simple, the reaction conditions are mild, the purity of the product dipropyl carbonate reaches 96-98%, and the yield reaches 46-51%.

Description

technical field [0001] The invention relates to a preparation method for catalytically synthesizing dipropyl carbonate with an alkaline ionic liquid. Background technique [0002] Dipropyl carbonate is a widely used organic chemical product, often used as an intermediate in the synthesis of drugs, pesticides, polycarbonate, etc. At the same time, it is also an excellent lithium battery electrolyte solution or electrolyte additive, which can greatly improve various performances of lithium batteries. With the vigorous development of the lithium-ion battery industry, the requirements for battery performance are getting higher and higher. As an excellent solvent or additive, the demand for dipropyl carbonate also increases accordingly. [0003] At present, the methods for preparing dipropyl carbonate mainly include phosgene method and transesterification method. The industrial synthesis method of dipropyl carbonate mainly adopts the phosgene method, but the phosgene method ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/96C07C68/06
Inventor 韩生骆铭吴志桥
Owner SHANGHAI INST OF TECH
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