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Method and device for removing water in microwave airtight reactor

A microwave reaction and reactor technology, applied in chemical instruments and methods, chemical/physical/physical-chemical processes using energy, preparation of organic compounds, etc., can solve problems such as inability to drain water

Inactive Publication Date: 2013-02-13
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at the problem of inability to drain water in a microwave closed reactor, and provides a water removal method equipped with a 3A molecular sieve water removal device

Method used

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  • Method and device for removing water in microwave airtight reactor
  • Method and device for removing water in microwave airtight reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 0.551mL of absolute ethanol, 0.300mL of acetic acid and 0.015g of p-toluenesulfonic acid into a 2-5mL microwave test tube, seal the upper end of the microwave test tube with a sealing cap, and put it into a microwave reactor for reaction. Set the temperature at 80°C, power at 90W, and react for 25 minutes. After the reaction, pour into saturated sodium carbonate solution, extract the organic layer, wash with saturated brine and saturated calcium chloride solution, and dry over anhydrous magnesium sulfate, collect fractions at 73-78°C with a yield of 74.54%.

Embodiment 2

[0036] Add 0.551mL of absolute ethanol, 0.300mL of acetic acid and 0.015g of p-toluenesulfonic acid into a 2-5mL microwave test tube, then directly add 0.800g of molecular sieve into the reaction liquid, then seal the upper end of the microwave test tube with a sealing cap, and put it into the microwave reaction reaction in the vessel. Set the temperature at 80°C, power at 90W, and react for 25 minutes. After the reaction, pour into saturated sodium carbonate solution, extract the organic layer, wash with saturated brine and saturated calcium chloride solution, and dry with anhydrous magnesium sulfate, collect fractions at 73-78°C with a yield of 12.31%.

Embodiment 3

[0038] Add 0.551mL of absolute ethanol, 0.300mL of acetic acid and 0.015g of p-toluenesulfonic acid into a 2-5mL microwave test tube, then add 0.600g of molecular sieve into the glass net bag inside the microwave reaction test tube, and then seal the upper end of the microwave test tube with a sealing cap. Put it into a microwave reactor to react. Set the temperature at 80°C, power at 90W, and react for 25 minutes. After the reaction, pour into saturated sodium carbonate solution, extract the organic layer, wash with saturated brine and saturated calcium chloride solution respectively, and dry with anhydrous magnesium sulfate, collect the fraction at 73-78°C, the yield is 79.89% ( Molecular sieve absorbs water 0.030g).

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Abstract

The invention discloses a method for removing water in a microwave airtight reactor, relating to a method for removing water by using an adsorbent in an adsorption device in the microwave airtight reactor. According to the device, a glass net bag of which the diameter is slightly less than the inner diameter of a microwave test tube is inserted at the upper end in the microwave reaction test tube; and a 3A molecular sieve capable of absorbing water is added in the glass net bag. When an esterification reaction is performed, generated water is absorbed by the absorbent, a balance is broken, so that the reaction is promoted to be continuously performed towards right, and the yield of the esterification reaction is improved. The method can be promoted and applied to other airtight reactors to absorb some specific products, so that the reaction yield is improved.

Description

technical field [0001] The invention belongs to the field of organic synthesis and relates to a method for removing water in a microwave closed reactor, in particular to a method for removing water in a microwave closed reactor by using a glass net bag device equipped with 3A molecular sieves. Background technique [0002] In 1986, Gedye et al. found that the use of microwave heating technology in organic synthesis can significantly increase the reaction rate. In the following ten years, the research on microwave-assisted organic synthesis has developed into a new and exciting field. Compared with traditional heating, microwave heating can speed up the reaction rate, even thousands of times, and has the characteristics of convenient operation, high yield and easy purification of products. At the same time, because microwave is a strong electromagnetic field, microwave plasma generated can often There are high-energy atoms, molecules and ions that cannot be obtained by therm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/12C07B41/04C07B41/12C07C69/14C07C67/08C07D493/10
Inventor 杨扬殷乐张国君尹芳华孙小强
Owner CHANGZHOU UNIV