Novel synthetic process of thymol

A synthesis process, technology of thymol, applied in the field of synthesis process of thymol, can solve problems such as increased cost of raw materials, high equipment requirements, and many wastes

Active Publication Date: 2014-07-30
SUQIAN COSMOS CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, in U.S. Patent No. 1892990 and U.S. Pat. No. 1,886,311, the process conditions of using propylene as an alkylating agent are disclosed, but the yield is only 50%. In addition, U.S. Pat. conditions, which will bring difficulties to the promotion of production and is not conducive to large-scale production
[0005] As can be seen from the analysis of existing patented technologies, there are many problems in the existing thymol synthesis process. For example, the use of propylene as an alkylating agent reduces the production cost, but the yield is low, often only 50%, and the process Harsh conditions and high requirements for equipment
In addition, adopt other reagents, for example with isopropyl chloride, isopropanol and isopropyl ether as alkylating reagent, although yield can be improved to 60~70%, but the cost of raw material improves greatly, and simultaneously produces " three wastes "more

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Add 11g of anhydrous aluminum trichloride, 6.6g of concentrated sulfuric acid and 120g of m-cresol into the reaction kettle, mix and stir evenly;

[0044] Then the reaction kettle was heated to 80°C, and then propylene gas was continuously fed in for the isopropylation reaction. The gas flow per hour was such that the molar ratio of propylene to m-cresol was 0.1:1, and the reaction was terminated after 10 hours of ventilation;

[0045] Cool the reaction kettle to 20°C, add 3% dilute hydrochloric acid to quench, then separate liquids at 80-90°C, wash the organic phase after liquid separation once with 10% salt water, and then distill under reduced pressure. The degree of vacuum is controlled between 10-15 mmHg, and the fraction of the target product thymol is obtained at 80-85° C., and the yield reaches 76%.

[0046] GC detection showed that the content of thymol was 99.3%.

Embodiment 2

[0048] 5g of zinc chloride, 3g of concentrated sulfuric acid with a mass percent concentration of 98% and 100g of m-cresol were added to the reactor, mixed and stirred evenly;

[0049] Then the temperature of the reactor was raised to 125°C, and then the isopropylation reaction was continuously fed with propylene gas, and the gas flow per hour was such that the molar ratio of propylene to m-cresol was 0.3:1, and the reaction was terminated after 14 hours of ventilation;

[0050] Cool the reaction kettle to 30°C, add 8% dilute hydrochloric acid to quench, then separate liquids at 75-80°C, wash the organic phase after liquid separation once with 10% salt water, and then distill under reduced pressure. The degree of vacuum is controlled between 10-15 mmHg, and the fraction of the target product thymol is obtained at 80-85° C., and the yield reaches 75%.

[0051] GC detection showed that the content of thymol was 99.1%.

Embodiment 3

[0053] Add 7.5g of anhydrous aluminum chloride, 5g of polyphosphoric acid and 100g of m-cresol into the reaction kettle, mix and stir evenly;

[0054] Then the reaction kettle was heated to 150°C, and then propylene gas was continuously fed in for isopropylation reaction. The gas flow per hour was such that the molar ratio of propylene to m-cresol was 0.5:1, and the reaction was terminated after 8 hours of ventilation;

[0055] Cool the reaction kettle to 30°C, add 2% dilute hydrochloric acid to quench, then separate liquids at 85-90°C, wash the organic phase after liquid separation once with 10% salt water, and then distill under reduced pressure. The degree of vacuum is controlled between 10-15 mmHg, and the fraction of the target product thymol is obtained at 80-85° C., and the yield reaches 80%.

[0056] GC detection showed that the content of thymol was 99.5%.

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PUM

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Abstract

The invention discloses a novel synthetic process of thymol. The novel synthetic process is as follows: in the presence of a catalyst which is a composition of concentrated sulfuric acid and aluminum trichloride, a composition of polyphosphoric acid and aluminum chloride, a composition of concentrated sulfuric acid and zinc chloride or a composition of the polyphosphoric acid and the zinc chloride, continuously introducing a propylene gas in a reaction system containing m-cresol by controlling the reaction temperature to carry out isopropylation reaction of the m-cresol, so that the thymol with content of 98%-99.5% and yield of 75%-80% is finally prepared. And moreover, the novel synthetic process is low in cost, simple in process condition and easy to operate.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a synthesis process of thymol. Background technique [0002] Thymol is also called thymol, and its chemical name is 5-methyl-2-isopropylphenol. It has a special aroma and a sweet and spicy flavor. It is often used to prepare gummies, peppermint, citrus, and mushroom aromas. and spices and other flavors. [0003] Thymol can not only be used as a spice, but also because of its antiseptic properties, it can also be used as a medical drug, often appearing in some oral hygiene products with medicinal value, and can also be used to treat wounds and store anatomical specimens; Phenol has a phenolic smell and is also commonly used as an insect repellant. In addition, thymol can also be used as an antioxidant, a special reagent for testing titanium nitride, a benchmark for comparison of thymol blue indicator, and a primary raw material for the synthesis of many chemicals. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/06C07C37/14
CPCC07C37/14C07C39/06
Inventor 杨正浩任静唐梁平杨东生顾国
Owner SUQIAN COSMOS CHEM
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