Method for preparing thymol through isopropyl m-cresols

A high-purity technology of thymol, which is applied in the field of preparation of thymol, can solve the problems that the purity needs to be improved and the yield of the final product is not high, and achieve great guidance and application value, good product purity, and controllable reactions

Inactive Publication Date: 2015-11-18
侯颖
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are also scientists such as H. Grabowska etc. who use iron containing Cr, Si, and K oxides as catalysts to optimize the reaction (Research on Chemistry Intermediates, 2001, 27 (3): 281-285), but the yield of the final product is not high, and the purity remains to be seen. to promote
As for how to use m-cresol and isopropanol to directly prepare thymol from molecular sieve catalyst Al-MCM-41, there are few reports

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] 1) Add 500g of molecular sieve catalyst Al-MCM-41 into a 5L reactor, and use electric heating to raise the overall temperature of the reactor to 300°C.

[0012] 2) After the reactor is heated to 300°C and the temperature is constant, mix isopropanol:m-cresol with a molar ratio of 1.2:1 and mix the raw materials with a total of 1000g. Put it into the reactor and seal it to start the reaction.

[0013] 3) After the reaction was carried out for 20 minutes, the reaction product was taken out and filtered, and 1000 g of ethyl acetate was added to the above product to extract once, and then 400 g of ethyl acetate was used to extract twice, and the three extractions were summed up.

[0014] 4) The extracted liquid was dried with anhydrous sodium sulfate and then concentrated to obtain 771 ml of thymol. Through instrument detection, the thymol selectivity yield of the final product reaches 98.3%.

Embodiment 2

[0016] 1) Add 500g of molecular sieve catalyst Al-MCM-41 into a 5L reactor, and use electric heating to raise the overall temperature of the reactor to 320°C.

[0017] 2) After the reactor is heated to 320°C and the temperature is constant, mix isopropanol: m-cresol with a molar ratio of 1.4:1 and mix the raw materials with a total of 1000g. Put it into the reactor and seal it to start the reaction.

[0018] 3) After the reaction was carried out for 30 minutes, the reaction product was taken out and filtered, and 1000 g of ethyl acetate was added to the above product to extract once, and then 400 g of ethyl acetate was used to extract twice, and the three extractions were summed up.

[0019] 4) The extracted liquid was dried with anhydrous sodium sulfate and then concentrated to obtain 739 ml of thymol. Through instrument detection, the selectivity yield of thymol of the final product reaches 98.0%.

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Abstract

The invention relates to a method for preparing thymol through isopropyl m-cresols, which adopts a molecular sieve as a catalyst, adds raw material metacresol and isopropyl reagent isopropyl alcohols into a reaction kettle according to certain proportion, generates the thymol and isomers thereof through a catalytic reaction in a given temperature, and can achieve above 98% selective yield of the thymol. The method for preparing the thymol through the isopropyl m-cresols has the advantages of high catalysis efficiency, wide source of raw materials, excellent product selective yield and easy operation of industrial production. The method for preparing the thymol through the isopropyl m-cresols has great guidance and application value in production preparation of the isopropyl m-cresols.

Description

field of invention [0001] The invention relates to a new method for preparing thymol by using Al-MCM-41 molecular sieve as a catalyst to catalyze the reaction between isopropanol as an isopropylating reagent raw material and m-cresol. Background technique [0002] Thymol is a white to light yellow translucent crystal, which was originally isolated from thyme, hence the name. Thymol is also known as thymol, the chemical name is 2-isopropyl-5-methylphenol, the English name is 2-isopropyl-5-methylphenol, and the chemical formula is C 10 h 14 O, the molecular weight is 150.22. Thymol is a crystalline powder at room temperature, with a boiling point of 233°C and a melting point of 48-51°C. Thymol has a special aroma of thyme or thyme, and is an important raw material for the preparation of menthol. It is antiseptic and less toxic than phenol, has medicinal value and can be used in oral hygiene products; it also has antifungal and parasitic functions and can be used to treat w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/11C07C39/06
CPCC07C37/11
Inventor 侯颖
Owner 侯颖
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