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Preparation method for thymol

A technology of thymol and cresol, which is applied in the field of preparation of thymol, can solve the problems of laborious, time-consuming catalyst loading and replacement, long reaction time, etc., and achieve good economic and social benefits, less side reactions, and high selectivity high effect

Active Publication Date: 2015-07-01
JIANGSU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the above method is prepared, a fixed bed reactor needs to be used. The loading and replacement of the fixed bed catalyst is time-consuming and laborious, and an inert gas is also required as a carrier. The most important point is that the reaction still needs to be carried out at high temperature, and the reaction time is long.

Method used

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  • Preparation method for thymol

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Effect test

Embodiment 1）

[0020] The preparation method of the thymol of the present embodiment is as follows:

[0021] Add 0.1 mol m-cresol and 0.1 mol isopropanol to a 50mL round-bottomed flask, stir well, then add 1g of Al-Cu / HAP catalyst to the mixture of m-cresol and isopropanol, stir again to obtain the reaction mass . The reaction materials were reacted for 5 min at a reaction temperature of 150° C. under microwave radiation with a power of 400 W to obtain 7.38 g of the target product thymol. The conversion rate of m-cresol is 50.36%, and the selectivity of the reaction is 97.57%.

[0022] The preparation method of the above-mentioned Al-Cu / HAP catalyst is as follows: 0.1 molAl(NO 3 ) 3· 9H 2 O, 0.01 mol CuSO 4· 5H 2 O was dissolved in 100mL of 0.05 mol / L dilute hydrochloric acid to obtain a mixed solution; 5 g of hydroxyapatite (HAP) as a carrier was added to the above mixed solution to obtain a solid-liquid mixture; 400mL of 1 mol / L NaOH solution was stirred evenly, and the above materi...

Embodiment 2）

[0024] The preparation method of the thymol of the present embodiment is as follows:

[0025] Add 0.1 mol m-cresol and 0.3 mol isopropanol to a 50mL round-bottomed flask, stir well, then add 1g of Al-Cu / HAP catalyst to the mixture of m-cresol and isopropanol, stir well again to obtain the reaction mass . The reaction materials were reacted for 5 min at a reaction temperature of 150° C. under microwave radiation with a power of 400 W to obtain 13.34 g of the target product thymol. The conversion rate of m-cresol is 91.48%, and the selectivity of the reaction is 97.12%.

[0026] The catalyst used in this example is the same as that in Example 1.

Embodiment 3）

[0028] All the other preparation methods of the thymol of the present embodiment are the same as in Example 1, except that the reaction material reacts for 10 min at a reaction temperature of 150° C. under microwave radiation of 400 W to obtain the target product Thymol Phenol 9.51g. The conversion rate of m-cresol is 65.34%, and the selectivity of the reaction is 96.98%.

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Abstract

The invention discloses a preparation method for thymol. Metacresol and isopropanol are used as reaction raw materials. The preparation method comprises the following preparation steps of stirring the metacresol and the isopropanol to be uniform; adding a catalyst in a mixture of the metacresol and the isopropanol and stirring to be uniform again to obtain a reaction mass; reacting the reaction mass at the reaction temperature of 100-200DEG C under the radiation of microwave with the power of 200 to 1,000W for 0.1 to 60 minutes to obtain the thymol as a target product, wherein the amount ratio of the metacresol to the isopropanol is 1:(0.01-10), and the dose of the catalyst is 1 to 30 percent of the mass sum of the metacresol and the isopropanol. According to the preparation method for the thymol, disclosed by the invention, the reaction temperature is 100 to 200DEG C and is greatly lower than the preparation temperature of the thymol by using an existing friedel-crafts alkylation reaction; the reaction time is shorter, and is only 0.1 to 60 minutes.

Description

technical field [0001] The invention relates to a preparation method of thymol. Background technique [0002] Thymol (also known as thymol, thymol), the chemical name is 5-methyl-2-isopropylphenol, it is white crystal or colorless translucent crystal at room temperature. Thymol has a wide range of uses. It is a commonly used food flavoring, preservative, bactericide and antioxidant. It is also the primary raw material for the synthesis of many chemicals, such as the synthesis of menthol by hydrogenation of thymol. [0003] There are two main sources of thymol: one is extracted from natural products (thyme oil, oregano oil, basil oil), and the other is obtained artificially. Due to the limited natural resources and the high extraction cost and environmental pressure, thymol is mainly artificially synthesized at present. [0004] The methods for artificially synthesizing thymol mainly include the following: (1) using fuming sulfuric acid as a catalyst to catalyze m-cresol an...

Claims

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Application Information

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IPC IPC(8): C07C39/06C07C37/16
CPCB01J23/72B01J27/1817B01J37/03B01J37/088C07C37/16C07C39/06
Inventor 张春勇周全法汪斌程洁红文颖频舒莉姚鹏飞孔峰
Owner JIANGSU UNIV OF TECH
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