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Controlled synthesizing method of propylene glycol monomethyl ether

A technology of propylene glycol monomethyl ether and a synthesis method, which is applied in the directions of ether preparation, alkylene oxide preparation of ether, etc., can solve the problems of complex preparation process, cumbersome steps, increase post-treatment process, etc., and achieves simple preparation process and good recyclability. , the effect of non-toxic side effects

Inactive Publication Date: 2017-08-11
HARBIN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its preparation process is quite complicated and the steps are cumbersome, and the synthesis reaction of this disclosed technology is carried out in organic solvents such as acetonitrile, acetone and acetic acid, which increases the post-treatment process after the reaction, and the volatilization of organic solvents will cause adverse effects on the environment.

Method used

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  • Controlled synthesizing method of propylene glycol monomethyl ether
  • Controlled synthesizing method of propylene glycol monomethyl ether
  • Controlled synthesizing method of propylene glycol monomethyl ether

Examples

Experimental program
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Effect test

specific Embodiment approach 1

[0030]This embodiment prepares propylene glycol monomethyl ether according to the following steps: select a 100mL stainless steel autoclave, add 0.05g of nano-iron oxide catalyst, 0.5mL of propylene oxide and 21mL of methanol into its polytetrafluoroethylene lining, put the lining into Put it into the reaction kettle, seal the reaction kettle, put it into an oil bath and heat it to 160 ° C, stir and react at this temperature for 8 hours, stop heating and stirring after the reaction is completed, and when the temperature of the reaction system drops to about room temperature, filter to obtain The mixed solution containing the product was analyzed by gas chromatography, and the result of the analysis was that the conversion rate of propylene oxide was 46.9%, and the selectivity of PM-2 was 73.6%.

[0031] The preparation method of the nano-iron oxide catalyst described in this embodiment is as follows: put 30 mL of 1 mol / L ferric chloride solution, 2 mL of polyethylene glycol, an...

specific Embodiment approach 2

[0034] The difference between this embodiment and the first embodiment is that the added amount of the nano-iron oxide catalyst is 0.1 g. Adopt gas chromatography to analyze: the conversion rate of propylene oxide is 97.7%, the selectivity of PM-2 is 82.6%, the total selectivity of propylene glycol monomethyl ether is about 100%, two kinds of isomer products PM-2 and PM- The ratio of 1 is 4.75.

specific Embodiment approach 3

[0036] The difference between this embodiment and specific embodiment 1 or 2 is that the addition amount of the nano-iron oxide catalyst is 0.15 g. Analyzed by gas chromatography: the conversion rate of propylene oxide was 92.3%, and the selectivity of PM-2 was 83.1%.

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Abstract

The invention relates to a controlled synthesizing method of propylene glycol monomethyl ether and belongs to the field of organic chemical synthesis. The synthesizing method includes: adding 0.05-0.3g of nano metal oxide catalyst, 0.5-1mL of propylene oxide and 21-50mL of methanol into a 100mL stainless steel high-pressure reaction kettle, sealing the reaction kettle, heating the reaction kettle to 110-160 DEG C, and performing reaction for 4-8 hours to obtain the propylene glycol monomethyl ether. The controlled synthesizing method has the advantages that the method is mild in reaction condition, easy to operate and high in efficiency, the reaction which is heterogeneous catalytic reaction is performed under a solvent-free condition, and the catalyst is easy to separate and good in recycling performance; the raw material conversion rate is 97.7%, the selectivity of the product PM-2 is 82.6%, and the total selectivity of the propylene glycol monomethyl ether is about 100%; the ratio of the isomer product PM-2 to the isomer product PM-1 is 4.75; the method can be used for oxidizing ethanol, propyl alcohol, butanol, isobutanol, amyl alcohol, isoamyl alcohol, n-octanol and the like.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and in particular relates to a control synthesis method of propylene glycol monomethyl ether. Background technique [0002] Propylene glycol methyl ether (PM) is a solvent with excellent performance and low toxicity. It has the characteristics of strong solvency, low volatility, high flash point and mild odor. It is one of the important products in the series of propylene glycol ether compounds. It is widely used in coatings, printing and dyeing and pesticide industries. At the same time, it can also be used as fuel antifreeze, detergent, extraction agent and organic synthesis intermediate. The molecular structure and physical and chemical properties of propylene glycol monomethyl ether are similar to those of ethylene glycol ethers, so it is considered to be an ideal substitute for more toxic ethylene glycol ethers. [0003] Synthesis of propylene glycol monomethyl ether by reaction of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/03C07C43/13
CPCC07C41/03C07C43/13
Inventor 路嫔何柏潼蔡清海
Owner HARBIN NORMAL UNIVERSITY