The preparation method of 1,2-bis(3-methylphenoxy)ethane

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

Active Publication Date: 2021-08-03
沈阳感光化工研究院有限公司
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  • Abstract
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  • 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

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  • The preparation method of 1,2-bis(3-methylphenoxy)ethane

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preparation example Construction

[0020] In a specific embodiment, the method of preparation of 1,2-bis (3-methylphenoxy) ethane thermosensitive agent, including the following steps: (1) adding megres in a high pressure reaction vessel and Potassium hydroxide, stir up to 130 ~ 150 ° C, all dissolve, cool down to 80 ° C, add dichloroethane; (2) incorporate the autoclave, access nitrogen replacement 3 times, and pass a small amount of nitrogen , The pressure reaches 0.1 to 0.2 MPa, warmed to 130 ~ 150 ° C, and the insulation reaction is 15-20 hours; (3) cool down to 70-80 ° C, add water, stir up to 80 to 100 ° C for 1-2 hours, cool down to Room temperature, precipitation for more than 3 hours, filtration, washing, drying, and white products. in,

[0021] The reaction formula in the preparation of 1,2-bis (3-methylphenoxy) ethane thermosensitive "is as follows:

[0022]

[0023] In the present invention, cresol, dichloroethane and potassium hydroxide molar ratio of 2: 1: 2.2 ~ 2.5.

[0024] The above step (3) is su...

Embodiment 1

[0027] In a 2-raised hyperthermine, 400 g of 1,54 g of potassium hydroxide was added, and 254 g of potassium hydroxide was added, and the temperature was 10 to 150 ° C, stirred, and the temperature was dissolved to 80 ° C or less. 1,2-dichloroethane 184 grams, The complex collision was added three times with nitrogen, and then a small amount of nitrogen was transferred, heated to 130 ° C, the insulation reaction was 15 hours, drown to 80 ° C, and water was added at 80 to 100 ° C for 1 hour. Ciparateing to 5 ~ 25 ° C for more than 3 hours, filtered, washed with a small amount of water, and the filter cake was dried to give 419.0 g of a white solid product, the content was 99.3%, and the yield was 93.5%.

Embodiment 2

[0029] At 2-liter pressure, 400 g of 1,90% hydroxide was added to 276 grams of potassium hydroxide, and the temperature was tapered to 130 to 150 ° C, stirred and dissolved, cooled to 80 ° C, then add 1,2-dichloroethane 184 grams, The bridge was closed, the autoclave was added three times with nitrogen, and then a small amount of nitrogen was transferred, heated to 150 ° C, and the insulation reaction was 15 hours, drown to 70 ° C, add 1200 ml of water, heat insulation at 80 to 100 ° C for 1.5 hours. Covered to 5 to 25 ° C for more than 3 hours, filtered, dried with a small amount of water, and the filter cake was dried to give 423.5 g of a white solid product, the content was 99.5%, and the yield was 94.5%.

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Abstract

The invention relates to the field of heat-sensitive sensitizers, in particular to a preparation method of 1,2-bis(3-methylphenoxy)ethane heat-sensitive sensitizers. The method comprises the following steps: (1) adding m-cresol and potassium hydroxide into a high-pressure reaction vessel, stirring and raising the temperature to 130-150° C., dissolving them all, cooling down to 70-80° C., and adding dichloroethane; (2) After the addition is complete, close the autoclave, replace it with nitrogen for 3 times, and feed a small amount of nitrogen, raise the temperature to 130-150°C, and keep the temperature for 15 hours; (3) cool down to 70-80°C, add water, and heat up to 80-80°C Stir at 100°C for 1 hour, cool down to room temperature, precipitate for more than 3 hours, filter, wash with water, and dry to obtain a white 1,2-bis(3-methylphenoxy)ethane thermal sensitizer product. The method of the invention has simple process and is suitable for large-scale industrial production, and the product is widely used in the production of thermal paper.

Description

Technical field [0001] The present invention relates to the field of thermal tanks, and more particularly to a method of preparation of 1,2-bis (3-methylphenoxy) ethane thermosensitive intensive agent. Background technique [0002] The structural formula of 1,2-bis (3-methylphenoxy) ethane thermistory is: [0003] [0004] The compound is usually reacted with EtOAc EtOAc EtOAc. Among them, the hydrolysis side reaction in alkaline conditions is the main cause of the reaction yield. The previous synthetic method reported that how the research direction mainly avoids the generation of the side, improve the yield. There is mainly the following methods: [0005] The method of interstitial mtechanol is started at the beginning, the amount of cresol in this method is much more cost, and the cost is difficult to treat after having excess of methanol, and the yield can reach 72%; then adopt a batch of alkaline method, this method It takes long-term monitoring and controlling the concent...

Claims

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Application Information

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Patent Type & Authority Patents(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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