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Preparation method of 1,2-bis(3-methyl phenoxy) ethane

A technology of methylphenoxy and ethane is applied in the field of preparation of 1,2-diethane heat-sensitive sensitizer, which can solve the problems of low yield, hydrolysis of dichloroethane, difficulty in post-processing, etc. High yield, improve conversion rate, avoid the effect of hydrolysis side reaction

Active Publication Date: 2019-02-22
沈阳感光化工研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the deficiencies in the prior art, the object of the present invention is to provide a method for preparing 1,2-bis(3-methylphenoxy)ethane with high yield, simple post-treatment, and suitable for large-scale production , to solve the problems of dichloroethane hydrolysis, low yield and post-processing difficulties in the prior art

Method used

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  • Preparation method of 1,2-bis(3-methyl phenoxy) ethane

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[0020] In a specific embodiment, the preparation method of 1,2-bis(3-methylphenoxy)ethane thermal sensitizer of the present invention comprises the following steps: (1) adding m-cresol and Potassium hydroxide, stir and heat up to 130-150°C, completely dissolve, cool down to below 80°C, add dichloroethane; (2) After adding, close the autoclave, replace with nitrogen for 3 times, and pass in a small amount of nitrogen , to make the pressure reach 0.1-0.2Mpa, raise the temperature to 130-150°C, and keep the heat for 15-20 hours; (3) cool down to 70-80°C, add water, heat up to 80-100°C and stir for 1-2 hours, then cool down to Precipitate at room temperature for more than 3 hours, filter, wash with water, and dry to obtain a white product. in,

[0021] The reaction formula in the process of preparing 1,2-bis(3-methylphenoxy)ethane thermal sensitizer is as follows:

[0022]

[0023] The molar ratio of m-cresol, dichloroethane and potassium hydroxide in the present invention is...

Embodiment 1

[0027] Add 400 grams of m-cresol and 254 grams of potassium hydroxide with a content of 90% in a 2-liter autoclave, heat up to 130-150°C, stir to dissolve, cool down to below 80°C, and then add 184 grams of 1,2-dichloroethane, After filling the closed autoclave, replace it with nitrogen for three times, then feed a small amount of nitrogen, raise the temperature to 130°C, keep the temperature for 15 hours, and lower it to below 80°C, add water, and keep the temperature at 80-100°C for 1 hour. The temperature was lowered to 5-25° C. to precipitate for more than 3 hours, filtered, rinsed with a small amount of water, and the filter cake was dried to obtain 419.0 g of a white solid product with a content of 99.3% and a yield of 93.5%.

Embodiment 2

[0029] Add 400 grams of m-cresol and 276 grams of potassium hydroxide with a content of 90% in a 2-liter autoclave, heat up to 130-150°C, stir and dissolve, cool down to 80°C, and then add 184 grams of 1,2-dichloroethane, After filling the closed autoclave, replace it with nitrogen for three times, then feed a small amount of nitrogen, raise the temperature to 150°C, keep it warm for 15 hours, then lower it to 70°C, add 1200 ml of water, and keep it at 80-100°C for 1.5 hours. The temperature was lowered to 5-25° C. to precipitate for more than 3 hours, filtered, rinsed with a small amount of water, and the filter cake was dried to obtain 423.5 g of a white solid product with a content of 99.5% and a yield of 94.5%.

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Abstract

The invention relates to the field of thermal sensitizers, in particular to a preparation method of a 1,2-bis(3-methyl phenoxy) ethane thermal sensitizer. The preparation method comprises the following steps: (1) adding m-cresol and potassium hydroxide into a high pressure reaction container, stirring the mixture to raise the temperature to 130-150 DEG C, fully dissolving the mixture, cooling themixture to 70-80 DEG C, and adding dichloroethane; (2) after addition, closing the high pressure kettle, introducing nitrogen to replace three times, introducing a small amount of nitrogen, heating the mixture to 130-150 DEG C, and keeping the temperature to react for 15 hours; and (3) reducing the temperature to 70-80 DEG C, adding water, raising the temperature to 80-100 DEG C and stirring the mixture for 1 hour, reducing the temperature to room temperature, separating out for more than 3 hours, and carrying out filtration, washing and drying to obtain the white 1,2-bis(3-methyl phenoxy) ethane thermal sensitizer product. The method provided by the invention is simple in process and suitable for industrial production on a large scale, and the product is widely applied to producing thermal sensitive paper.

Description

technical field [0001] The invention relates to the field of heat-sensitive sensitizers, in particular to a preparation method of a 1,2-bis(3-methylphenoxy)ethane heat-sensitive sensitizer. Background technique [0002] The structural formula of 1,2-bis(3-methylphenoxy)ethane thermal sensitizer is: [0003] [0004] This compound is usually generated by the reaction of m-cresol and dichloroethane under the action of lye. Among them, the hydrolysis side reaction of dichloroethane under alkaline conditions is the main reason affecting the reaction yield. In the previous synthetic method reports, the main research direction is how to avoid the side reaction and improve the yield. There are mainly the following methods: [0005] At the beginning, use the method of excessive m-cresol, the method m-cresol consumption is more, the cost is higher, contain excessive m-cresol post-processing difficulties, the yield can reach 72%; It needs long-term monitoring and control of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/16C07C43/205
CPCC07C41/16C07C43/2055
Inventor 李昌德马思聪许锦凤王越王思萌
Owner 沈阳感光化工研究院有限公司
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