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Method for preparing propargyl methyl carbonate

A technology of propargyl methyl carbonate and dimethyl carbonate, applied in the field of organic compound synthesis and purification, can solve the problems of long reaction synthesis route, high toxicity of methyl chloroformate, low production safety, etc. The effect of low production cost, high production safety and high preparation efficiency

Inactive Publication Date: 2018-05-11
HUIZHOU CAPCHEM CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Propargyl methyl carbonate is generated by the reaction of methyl chloroformate and propynyl alcohol. This method produces a large amount of hydrogen chloride. At the same time, the raw material methyl chloroformate is highly toxic, flammable, and corrosive. The vapor strongly irritates the eyes and respiratory tract. It can also cause poisoning through skin absorption, the maximum allowable concentration in the workplace is 0.005mg / L, the production safety is low, and the reaction synthesis route is long

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] S1, raw material premixing: take 224g propynyl alcohol and 672g dimethyl carbonate and mix according to the mass ratio of 1:3 to obtain the raw material mixed solution;

[0027] S2, heating reaction at normal pressure: add 786g dimethyl carbonate and 35g potassium carbonate to the raw material mixed solution, stir and heat and slowly raise the temperature, control the temperature in the range of 40°C to 115°C to carry out heating reaction at normal pressure and collect the fractions distilled by heating , when the reaction temperature reaches 115°C, stop the reaction to obtain the propargyl methyl carbonate reaction solution, and collect 672g fractions;

[0028] S3, filter the residue: filter the propargyl methyl carbonate reaction solution described in step S2, wash the filter residue with dimethyl carbonate, then suction filter, and combine the filtrates to obtain the propargyl methyl carbonate solution;

[0029] S4, vacuum rectification: the propargyl methyl carbonat...

Embodiment 2

[0031] S1, raw material premixing: take 112g of propynyl alcohol and 336g of dimethyl carbonate and mix according to the mass ratio of 1:3 to obtain the raw material mixed solution;

[0032] S2, heating reaction at normal pressure: add 1104g dimethyl carbonate and 15g potassium carbonate to the raw material mixed solution, stir and heat and slowly raise the temperature, control the temperature in the range of 40°C to 120°C to carry out heating reaction at normal pressure and collect the fractions distilled by heating , when the reaction temperature reaches 120°C, the reaction is stopped to obtain the propargyl methyl carbonate reaction solution, and 1072g fractions are collected;

[0033] S3, filter the residue: filter the propargyl methyl carbonate reaction solution described in step S2, wash the filter residue with dimethyl carbonate, then suction filter, and combine the filtrates to obtain the propargyl methyl carbonate solution;

[0034] S4, vacuum distillation: the propar...

Embodiment 3

[0036] S1, raw material premixing: take 112g of propynyl alcohol and 336g of dimethyl carbonate and mix according to the mass ratio of 1:3 to obtain the raw material mixed solution;

[0037] S2, heating reaction at normal pressure: add 747g dimethyl carbonate and 18g potassium carbonate to the raw material mixed solution, stir and heat and slowly raise the temperature, control the temperature in the range of 40°C to 120°C to carry out heating reaction at normal pressure and collect the fractions distilled by heating , when the reaction temperature reaches 120°C, stop the reaction to obtain the propargyl methyl carbonate reaction solution, and collect 770g fractions;

[0038] S3, filter the residue: filter the propargyl methyl carbonate reaction solution described in step S2, wash the filter residue with dimethyl carbonate, then suction filter, and combine the filtrates to obtain the propargyl methyl carbonate solution;

[0039] S4, vacuum distillation: the propargyl methyl car...

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Abstract

The invention discloses a method for preparing propargyl methyl carbonate. The method comprises the following steps: S1. raw material premixing; S2. normal-pressure heated reaction; S3. residue filtering; S4. rectification under vacuum, thereby obtaining the propargyl methyl carbonate. The method provided by the invention is safe, is low in cost and high in yield and can be used for extensively preparing the propargyl methyl carbonate.

Description

technical field [0001] The invention relates to the field of synthesis and purification methods of organic compounds, in particular to a preparation method of propargyl methyl carbonate. Background technique [0002] Propargyl methyl carbonate is a new type of non-aqueous lithium-ion battery electrolyte additive. Because the molecular structure of the additive contains unsaturated carbon-carbon triple bonds and ester groups at the same time, it can undergo polymerization on the electrode surface to form multiple Ester-based compounds, which can complex with metal ions on the surface of the positive electrode material to form a passivation film, reduce the catalytic oxidation of Co ions on the electrolyte, thereby inhibiting the decomposition of the electrolyte on the electrode surface and improving the high-temperature storage of the battery and cycle performance. [0003] The preparation method of propargyl methyl carbonate reported at present is as follows: [0004] Prop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/06C07C68/08C07C69/96
CPCC07C68/06C07C68/08C07C69/96
Inventor 陈群何舟
Owner HUIZHOU CAPCHEM CHEM CO LTD
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