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A kind of synthetic method containing ether oxygen bond linear dimethyl dicarbonate

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

Active Publication Date: 2021-11-23
ANHUI POLYTECHNIC UNIV
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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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  • A kind of synthetic method containing ether oxygen bond linear dimethyl dicarbonate
  • A kind of synthetic method containing ether oxygen bond linear dimethyl dicarbonate
  • A kind of synthetic method containing ether oxygen bond linear dimethyl dicarbonate

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Comparison scheme
Effect test

Embodiment 1

[0030] like 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, w...

Embodiment 2

[0040] like 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) 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;

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

Embodiment 3

[0050] like 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 hydrotalcite,...

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Abstract

The invention relates to a synthesis method of ether oxygen bond-containing linear dimethyl dicarbonate, which comprises one step: preparing a catalyst magnesium aluminum hydrotalcite; second step: preparing a mixed reaction solution of glycol, dimethyl carbonate and magnesium aluminum hydrotalcite 3: Stir the reaction solution, heat up to 90°C, and record the reaction time; 4: Cool to room temperature after the reaction, filter, and purify by rotary evaporation to obtain a linear dimethyl dicarbonate containing ether oxygen bonds. The catalyst prepared by the method of the invention has obvious characteristic peaks of magnesium aluminum hydrotalcite, and the synthesized ether-oxygen bond straight-chain dimethyl dicarbonate has high rotary distillation 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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Patent Type & Authority Patents(China)
IPC IPC(8): C07C68/06C07C69/96B01J27/232
CPCB01J27/232C07C68/06C07C69/96
Inventor 刘欢陈瑞洋
Owner ANHUI POLYTECHNIC UNIV
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