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Method for synthesizing ether oxygen bond-containing linear dimethyl dicarbonate

A technology of dimethyl dicarbonate and synthesis method, which is applied in the preparation of organic carbonate, chemical instruments and methods, organic chemistry, etc., can solve the problems of deactivation, large amount of calcium oxide, etc., and achieve the effect of excellent catalytic performance

Active Publication Date: 2019-02-22
ANHUI UNIVERSITY OF TECHNOLOGY AND SCIENCE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the amount of calcium oxide is large, 10wt%, and it is easy to absorb water and carbon dioxide in the air and deactivate

Method used

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  • Method for synthesizing ether oxygen bond-containing linear dimethyl dicarbonate
  • Method for synthesizing ether oxygen bond-containing linear dimethyl dicarbonate
  • Method for synthesizing ether oxygen bond-containing linear dimethyl dicarbonate

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Effect test

Embodiment 1

[0030] Such as Figure 1 to Figure 2 Shown, a kind of synthetic method containing ether oxygen bond linear dimethyl dicarbonate comprises:

[0031] Step 1: preparing the catalyst magnesium aluminum hydrotalcite, specifically including:

[0032] 1) Taking magnesium nitrate and aluminum nitrate as raw materials, preparing a salt solution with a total metal concentration of 1.6mol / L, wherein the Mg / Al molar ratio is 3;

[0033] 2) Precipitating agent is prepared with a mixed aqueous solution of sodium hydroxide and sodium carbonate, wherein the concentration of sodium hydroxide is 3.7mol / L, and the concentration of sodium carbonate is 0.3mol / L;

[0034] 3) Under the conditions of 40°C and PH=9.0, magnesium aluminum hydrotalcite was prepared by co-precipitation method, aged at 90°C for 4 hours, filtered, washed, and finally dried at 120°C for 12 hours;

[0035] Step 2: preparing a mixed reaction liquid of diethylene glycol, dimethyl carbonate, and magnesium aluminum hydrotalcite...

Embodiment 2

[0040] Such as Figure 1 to Figure 2 Shown, a kind of synthetic method containing ether oxygen bond linear dimethyl dicarbonate comprises:

[0041] Step 1: preparing the catalyst magnesium aluminum hydrotalcite, specifically including:

[0042] 1) Taking magnesium nitrate and aluminum nitrate as raw materials, preparing a salt solution with a total metal concentration of 1.6mol / L, wherein the Mg / Al molar ratio is 3;

[0043] 2) Precipitating agent is prepared with a mixed aqueous solution of sodium hydroxide and sodium carbonate, wherein the concentration of sodium hydroxide is 3.7mol / L, and the concentration of sodium carbonate is 0.3mol / L;

[0044] 3) At 40°C and pH=9.0, magnesium aluminum hydrotalcite was prepared by co-precipitation method, aged at 90°C for 4 hours, filtered, washed, and finally dried at 120°C for 12 hours;

[0045] Step 2: preparing a mixed reaction liquid of triethylene glycol, dimethyl carbonate, and magnesium aluminum hydrotalcite, wherein the mass r...

Embodiment 3

[0050] Such as Figure 1 to Figure 2 Shown, a kind of synthetic method containing ether oxygen bond linear dimethyl dicarbonate comprises:

[0051] Step 1: preparing the catalyst magnesium aluminum hydrotalcite, specifically including:

[0052]1) Taking magnesium nitrate and aluminum nitrate as raw materials, preparing a salt solution with a total metal concentration of 1.6mol / L, wherein the Mg / Al molar ratio is 3;

[0053] 2) Precipitating agent is prepared with a mixed aqueous solution of sodium hydroxide and sodium carbonate, wherein the concentration of sodium hydroxide is 3.7mol / L, and the concentration of sodium carbonate is 0.3mol / L;

[0054] 3) Under the conditions of 40°C and PH=9.0, magnesium aluminum hydrotalcite was prepared by co-precipitation method, aged at 90°C for 4 hours, filtered, washed, and finally dried at 120°C for 12 hours;

[0055] Step 2: preparing a mixed reaction liquid of tetraethylene glycol, dimethyl carbonate, and magnesium aluminum hydrotalci...

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Abstract

The invention relates to a method for synthesizing ether oxygen bond-containing linear dimethyl dicarbonate. The method comprises the following steps: 1, preparing a catalyst magnesite hydrotalcite; 2, preparing a mixed reaction solution of glycol, dimethyl carbonate and magnesite hydrotalcite; 3, stirring the reaction solution, raising the temperature to 90 DEG C, and recording the reaction time;and 4, cooling to a room temperature after the reaction is ended, filtering, performing rotary evaporation, and purifying, thereby obtaining the ether oxygen bond-containing linear dimethyl dicarbonate. The catalyst prepared by the method disclosed by the invention has an obvious magnesite hydrotalcite characteristic peak, and the synthesized ether oxygen bond-containing linear dimethyl dicarbonate has high rotary evaporation purity.

Description

technical field [0001] The invention relates to the technical field of synthesizing straight-chain dimethyl dicarbonate containing ether oxygen bonds, in particular to a method for synthesizing straight-chain dimethyl dicarbonate containing ether oxygen bonds. Background technique [0002] Organic carbonate is non-toxic and non-polluting. It is an important chemical intermediate and is widely used in the fields of drugs, cosmetics, fragrances, electrolytes, polymers, and biomedicine. The transesterification method is considered to be the most promising non-optical Carbonate synthesis route. As a green solvent, DMC is chemically stable, non-toxic, non-corrosive, can be miscible with alcohol in any proportion, and has mild reaction conditions with alcohol, so it is often used as a raw material for transesterification. Its relevant transesterification studies mainly focus on the transesterification reaction of DMC and monohydroxy compound to synthesize monocarbonate, especiall...

Claims

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Application Information

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IPC IPC(8): C07C68/06C07C69/96B01J27/232
CPCB01J27/232C07C68/06C07C69/96
Inventor 刘欢陈瑞洋
Owner ANHUI UNIVERSITY OF TECHNOLOGY AND SCIENCE
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