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Synthetic method of diallyl diethylene glycol carbonate

A technology of diallyl diethylene glycol and its synthesis method, which is applied in the preparation of organic carbonates and organic chemistry, etc., which can solve the problems of high temperature resistance of catalysts, easy deactivation production costs, complex synthesis processes, etc., and improve the utilization rate and conversion rate, reducing potential safety hazards, and the effect of simple synthesis method

Inactive Publication Date: 2013-05-22
山东鲁源化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] The purpose of the present invention is to provide a synthetic method of diallyl diglycol carbonate, aiming at solving the problems of complex existing synthetic process, the catalyst used is not resistant to high temperature, easy to deactivate and high production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add diethylene glycol, dimethyl carbonate, propenyl alcohol, catalyst ion exchange resin Amberlyst-15 to the reactor equipped with agitator, thermometer, wherein, the mol ratio of raw material diethylene glycol: dimethyl carbonate: propenyl alcohol is 1: 2: 2.5, the mass ratio of catalyst to diethylene glycol is 1: 0.005, the reaction mixture is stirred evenly, heated, when the temperature rises to 50 ° C, reflux for 2 to 3 hours, and then control the temperature at 65 ° C ~ 70 ℃, the above-mentioned reaction solution is distilled and the by-product methanol is collected, and when there is no more methanol to steam out, the transesterification reaction is completed, and the control temperature is at 95 ℃~100 ℃, and the propylene alcohol and the diallyl carbonate generated are recovered, and the recovery is completed. , the reaction solution is lowered to room temperature, and the catalyst ion exchange resin Amber lys t-15 is separated by filtration to obtain a diallyl di...

Embodiment 2

[0040]Add diethylene glycol, dimethyl carbonate, propylene alcohol, catalyzer ion exchange resin Amberlyst-15 in the reactor that agitator, thermometer are housed, wherein, raw material diethylene glycol: dimethyl carbonate: the mol ratio of propylene alcohol is 1:2:8, the mass ratio of catalyst to diethylene glycol is 1:0.008. Stir the reaction mixture evenly and heat it. When the temperature rises to 55°C, keep it under reflux for 2~3 hours, and then control the temperature at 60°C~70°C. ℃, distill the above reaction liquid and collect the by-product methanol. When no more methanol is distilled out, the transesterification reaction is completed. , down to room temperature, filter and separate the catalyst ion exchange resin Amberlyst-15 to obtain diallyl diglycol carbonate product, and the recovered catalyst can be reused.

Embodiment 3

[0042] Add diethylene glycol, dimethyl carbonate, propylene alcohol, catalyzer ion exchange resin Amberlyst-15 in the reactor that agitator, thermometer are housed, wherein, raw material diethylene glycol: dimethyl carbonate: the mol ratio of propylene alcohol is 1:4:2.5, the mass ratio of catalyst to diethylene glycol is 1:0.01, stir the reaction mixture evenly, heat, when the temperature rises to 60°C, keep it under reflux for 2~3 hours, then control the temperature at 65°C~75°C ℃, distill the above reaction liquid and collect the by-product methanol. When no more methanol is distilled out, the transesterification reaction is completed. , down to room temperature, filter and separate the catalyst ion exchange resin Amberlyst-15 to obtain diallyl diglycol carbonate product, and the recovered catalyst can be reused.

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PUM

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Abstract

The invention belongs to the technical field of synthesis of diallyl diethylene glycol carbonate, and particularly relates to a synthetic method of diallyl diethylene glycol carbonate. The synthetic method comprises the following steps of: (1) adding diethylene glycol, allyl alcohol, dimethyl carbonate and catalyst ion exchange resin Amberlyst-15 into a reaction still, reacting the dimethyl carbonate with the allyl alcohol to generate diallycarbonate and methanol, carrying out an ester exchange reaction on the diallycarbonate and the diethylene glycol at 50-140 degree centigrade, reflowing and thermally insulating for 2-3 hours; and (2) distilling the reaction liquid in the step (1), recovering methanol at 65-90 DEG C, recovering allyl alcohol and diallycarbonate at 95-140 DEG C, reducing to the room temperature of the catalyst-containing mixed liquor, filtering and separating the catalyst ion exchange resin Amberlyst-15 to obtain required products. The synthetic method of diallyl diethylene glycol carbonate disclosed by the invention has the advantages of simple method, heat-resisting catalyst and high purity of the obtained products, and is capable of saving the production cost.

Description

technical field [0001] The invention belongs to the technical field of synthesis of diallyl diethylene glycol carbonate, and particularly relates to a synthesis method of diallyl diethylene glycol carbonate. Background technique [0002] Dially glycol carbonates (Dially glycol carbonates), molecular weight 274.27, structural formula CH 2 CHCH 2 OCO 2 CH 2 CH 2 OCH 2 CH 2 OCO 2 CH 2 CHCH 2 , with a melting point of -4 °C, is the most widely used material for the production of ordinary resin lenses. It was discovered by chemists from Columbia Company in the United States in the 1940s. It is the No. 39 material in a series of polymers developed by the US Air Force. Therefore, known as CR-39 (Columbia Resin No. 39), CR-39 was used in the production of ophthalmic corrective lenses from 1955-1960 and was the first generation of ultra-light, impact-resistant resin lenses. In the prior art, the synthetic method of CR-39 can be divided into three categories: phosgene method...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/06
Inventor 冯仲善许明然李京东安国成王光平
Owner 山东鲁源化工科技有限公司
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