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Synthetic method for propylend glycol dimethyl ether

A technology of propylene glycol dimethyl ether and propylene glycol methyl ether, which is applied in the synthesis field of propylene glycol dimethyl ether, can solve problems such as poor safety, and achieve the effects of less side reactions, high product purity and simple process flow

Inactive Publication Date: 2004-12-15
NANJING FORESTRY UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] During the reaction process, gas is generated and discharged, which makes the reaction balance move to the right, which is beneficial to the generation of propylene glycol dimethyl ether, but due to the use of metal sodium, the safety of the reaction is poor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0030] In a 1000ml four-necked flask equipped with a mechanical stirrer with a mechanical seal, a reflux condenser and a thermometer, add 225g of propylene glycol monomethyl ether and 130g of sodium hydroxide respectively, turn on the stirrer, raise the temperature to 60°C for 1 hour, and introduce 139g Chloromethane gas is used for etherification reaction, the reaction temperature is controlled at 60-70°C, and the addition is completed within 6 hours. After stopping the circulation of chloromethane, continue the heat preservation reaction for 1 hour, and the reaction ends. After cooling to room temperature and filtering, 237 g of crude product was obtained, and the content of propylene glycol dimethyl ether was 81.3% according to gas chromatography analysis.

example 2

[0032] In a 1000ml four-neck flask equipped with a mechanical stirrer with a mechanical seal, a reflux condenser and a thermometer, add 225g of propylene glycol monomethyl ether and 145g of sodium methoxide respectively, turn on the stirrer, raise the temperature to 50°C for 1 hour, and introduce 139g of chlorine The etherification reaction is carried out with methane gas, the reaction temperature is controlled at 50-60°C, and the addition is completed within 6 hours. After stopping the flow of chloromethane, continue the heat preservation reaction for 1 hour, and the reaction ends. Cool to room temperature and filter to obtain 301 g of crude product, the content of propylene glycol dimethyl ether is 62.7% according to gas chromatography analysis.

example 3

[0034] In a 1000ml four-neck flask equipped with a mechanical stirrer with a mechanical seal, a reflux condenser and a thermometer, add 225g of propylene glycol monomethyl ether and 150g of sodium hydroxide respectively, turn on the stirrer, raise the temperature to 70°C for 1 hour, and add 315g of Carry out etherification reaction of dimethyl sulfate, control the reaction temperature at 70-80°C, complete the addition within 6 hours, stop the dropwise addition of dimethyl sulfate, continue the heat preservation reaction for 1 hour, and the reaction ends. After cooling to room temperature and filtering, 227 g of crude product was obtained, and the content of propylene glycol dimethyl ether was 76.5% according to gas chromatography analysis.

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Abstract

The synthesis process of propylene glycol dimethyl ether features that the materials including propylene glycol methyl ether, alkali and alkylation agent are reacted at 40-90 deg.c to prepare propylene glycol dimethyl ether product. Where, the alkali may be sodium hydroxide, sodium methoxide, potassium hydroxide or potassium methoxide; and the alkylation agent may be chloromethane, dimethyl sulfate or dimethyl carbonate. The present invention has the advantages of mild reaction condition, high production safety, high product selectivity, less side reactions, high product purity, simple technological process, and easy industrial application.

Description

1. Technical field: [0001] The invention relates to a synthesis method of propylene glycol dimethyl ether, which belongs to the technical field of organic chemical industry. 2. Background technology: [0002] The chemical name of propylene glycol dimethyl ether is 1,2-dimethoxypropane, and its structural formula is: CH 3 OCH 2 CH(CH 3 )OCH 3 . Propylene glycol dimethyl ether, as a new type of aprotic polar solvent with low toxicity and easy to solvate cationic substances, can be used in chemical technology fields such as electrochemistry, polar organic reactions, anionic polymerization, and coordination ion polymerization; for extraction It can also be used in industrial products such as lubricants, fabrics, pharmaceuticals, and pesticides; it can also be widely used in cleaning agents, extractants, stabilizers, co-solvents, organic synthesis reaction solvents, additives, and wetting solvents Wait. [0003] There are few reports on the synthesis of propylene glycol dim...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/01C07C43/04
Inventor 朱新宝王甫泉
Owner NANJING FORESTRY UNIV
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