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Preparation methods of acetate alpha-phenethyl alcohol and acetate styrene

A technology of acetoxyacetophenone and phenethyl alcohol, applied in the field of preparation of benzene ring derivatives, can solve the problems of increasing solvent separation and recovery procedures, low reaction selectivity and conversion rate, difficulty in separation and purification of dehydration products, etc. The effect of improving the property, reducing the content, and inhibiting the reaction speed

Active Publication Date: 2013-10-23
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] In summary, there are following deficiencies in the known preparation method of p-acetoxy α-phenylethanol: (1) adopt palladium / carbon catalyst to carry out hydrogenation reaction, and reaction selectivity and conversion rate are all low, it is the separation of dehydration product Purification has brought difficulties; (2) the use of solvent in the hydrogenation reaction process increases the volume of the reactor and increases the separation and recovery process of the solvent

Method used

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  • Preparation methods of acetate alpha-phenethyl alcohol and acetate styrene
  • Preparation methods of acetate alpha-phenethyl alcohol and acetate styrene

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Experimental program
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Effect test

Embodiment 1

[0052] The test is carried out in a 500ml high-pressure reactor with stirring, 178g p-acetoxyacetophenone, 0.28g sodium hydroxide and 14g palladium / carbon catalyst (containing 5% palladium) are packed in the reactor, and then with 1.2MPa The hydrogen replaces the air in the reactor twice. Keep the hydrogen pressure in the reactor at 1.2 MPa, stir and heat. The reaction temperature was 75° C., and after 6 hours, the hydrogen gas was discharged, and the reaction was completed. Analyze the reaction solution composition with gas chromatography, the result shows, p-acetoxy group α-phenethyl alcohol content is 96.5%, p-acetoxy ethylbenzene 0.5%, unreacted p-acetoxy acetophenone 0.4%, ethylbenzene 1.1%, the rest for other components. The conversion of p-acetoxyacetophenone was 99.7%.

Embodiment 2

[0054] 215g p-acetoxyacetophenone, 0.6g sodium hydroxide and 2.15g palladium / carbon catalyst (containing 5% palladium) are packed in the reactor of 500ml with stirring, then in the hydrogen displacement reactor with 1.5MPa of air twice. Keep the hydrogen pressure in the reactor at 1.5 MPa, and heat the material in the reactor to 90° C., and discharge the hydrogen after reacting for 4 hours. The product is analyzed by gas chromatography, and the results show that the p-acetoxy α-phenylethanol content is 97%, p-acetoxy ethylbenzene 0.4%, unreacted p-acetoxy acetophenone 0.9%, ethylbenzene 1.0%, and the rest is other components. The conversion rate of p-acetoxyacetophenone was 99.1%.

Embodiment 3

[0056] 267g p-acetoxyacetophenone, 1.3g diethanolamine and 16g palladium / carbon catalyst (containing 5% palladium) are packed in the 500ml reactor with stirring, then use the hydrogen displacement reactor of 1.5MPa Second-rate. Keep the hydrogen pressure in the reactor at 1.5 MPa, and heat the material in the reactor to 80° C., and discharge the hydrogen after reacting for 6 hours. The product is analyzed by gas chromatography, and the results show that the p-acetoxy α-phenylethanol content is 96%, p-acetoxy ethylbenzene 1.2%, unreacted p-acetoxy acetophenone 0.7%, ethylbenzene 0.7%, and the rest is other components. The conversion of p-acetoxyacetophenone was 99.4%.

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Abstract

The invention discloses preparation methods of acetate alpha-phenethyl alcohol and acetate styrene, and belongs to the technical field of preparation of benzene derivatives. The preparation method is characterized by comprising the following processing steps of: enabling acetate acetophenone to react with at least stoichiometric amount of hydrogen to prepare the acetate alpha-phenethyl alcohol under existence of a stopping agent and a catalyst, wherein the used stopping agent is alkali metal hydroxide or alcohol amine compound or more than two mixed components thereof; and carrying out dehydration reaction on the acetate alpha-phenethyl alcohol to generate the acetate styrene. By adopting the method provided by the invention, the reaction speed of side reaction to generate hydrocarbon is effectively inhibited; the reaction selectivity is high; and the percent conversion on the acetate acetophenone can be up to over 99%.

Description

technical field [0001] The preparation method of p-acetoxy α-phenylethyl alcohol and p-acetoxy styrene belongs to the technical field of preparation of benzene ring derivatives. Background technique [0002] P-acetoxy α-phenylethyl alcohol and its dehydration product are the raw materials for synthesizing p-acetoxy styrene monomer, and its target product is used as the bonding resin of photoresist. In the high-resolution photoresist series technology, the monomer used to replace the styrene copolymer DUV photoresist is p-acetoxystyrene. [0003] In the electronic information industry, photoresist is the key basic processing material of microfabrication technology. There are many manufacturers of photoresist in the world, but there are less than ten manufacturers that can produce photoresist with resolution below 0.25-0.18μm. This high-resolution photoresist produced with p-acetoxystyrene as a monomer will fill the gap in China. At present, the preparation process of this ...

Claims

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Application Information

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IPC IPC(8): C07C69/157C07C67/29C07C67/297
Inventor 菅秀君王申军潘清
Owner CHINA PETROLEUM & CHEM CORP
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