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
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[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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