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Production method for synthesizing anthracene associated anthrone under catalysis of solid superacid

A technology of solid superacid and anthracenthrone, which is applied in chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc., can solve problems such as waste sulfuric acid pollution yield, and achieve the effect of solving pollution

Inactive Publication Date: 2021-08-24
鞍山市五色石新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the embodiments of the present invention is to provide a production method of solid superacid catalyzed synthesis of anthracene, which solves the problems caused by the production of anthracene with 1,1'-binaphthyl-8,8'-dicarboxylic acid as raw material Problems of waste sulfuric acid pollution and low yield

Method used

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  • Production method for synthesizing anthracene associated anthrone under catalysis of solid superacid
  • Production method for synthesizing anthracene associated anthrone under catalysis of solid superacid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Ingredients: Add 193 parts of 1,1ˊ-binaphthalene-8,8ˊ-dicarboxylic acid into a 3000L enamel reaction kettle, add 900 parts of glacial acetic acid, start stirring the material and stir evenly, add 350 parts of acetic anhydride and 5 parts of solid super acid ( HND-33).

[0022] Main reaction: heat the reactor to reflux with steam, the material dissolves first, and then a large amount of solids precipitate out. After the reaction is over, distill out glacial acetic acid under reduced pressure. After distilling about 900 parts of glacial acetic acid, stop stirring and continue distilling until there is no liquid flow out. Stop distilling.

[0023] Product purification: slowly add 5% sodium hydroxide aqueous solution to the reaction kettle, slowly start stirring, after stirring for 3 hours, raise the temperature to 95°C, continue stirring until there is no blocky solid in the reaction kettle, then cool down to 55°C , filtered, washed with water until neutral. Dry to obta...

Embodiment 2

[0025] Ingredients: Add 193 parts of 1,1′-binaphthalene-8,8′-dicarboxylic acid into a 3000L enamel reaction kettle, add 1500 parts of o-dichlorobenzene and 5 parts of solid superacid (HND-32).

[0026] Main reaction: heat the reactor to reflux with heat conduction oil, and slowly separate the generated water from the water separator. After the reaction is over, steam distillation is performed, and o-dichlorobenzene is recovered from the bottom of the water separator.

[0027] Product purification: After the distillation of o-dichlorobenzene, slowly add 5% sodium hydroxide aqueous solution to the reaction kettle, slowly start stirring, after stirring for 3 hours, raise the temperature to 95°C, and continue stirring until there is no lump in the reaction kettle Cool to 55° C., filter, and wash with water until neutral. Dry to obtain 116 parts of anthracenthone.

Embodiment 3

[0029] Ingredients: Add 193 parts of 1,1′-binaphthalene-8,8′-dicarboxylic acid into a 3000L enamel reaction kettle, add 1500 parts of chlorobenzene and 5 parts of solid superacid (HND-31).

[0030] Main reaction: Heat the reactor to reflux with steam, and slowly separate the generated water from the water separator. After the reaction is finished, cool down and filter.

[0031] Product purification: put the filter cake containing chlorobenzene back into the 3000L reactor, add 1000 parts of water and 5 parts of tributyl phosphate as defoamer, stir and distill, and separate the chlorobenzene from the water separator. After the chlorobenzene is distilled off, slowly add 5% aqueous sodium hydroxide solution to the reaction kettle to adjust the pH value to 11, stir while hot until there is no lumpy solid in the reaction kettle, cool down to 55°C, filter and wash with water to neutral. Dry to obtain 109 parts of anthracene.

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Abstract

The invention is applicable to the technical field of organic dyes, and provides a production method for synthesizing anthracene associated anthrone under the catalysis of solid superacid, which comprises the following steps of proportioning: adding 1, 1'-binaphthyl-8, 8'-dicarboxylic acid into a proper amount of solvent, and then adding a solid superacid catalyst, main reaction: heating to reflux, and dehydrating, cooling until the reaction is complete, product purification: after the main reaction is finished, filtering to remove a solvent in a filter cake, then putting the filter cake into a sodium hydroxide aqueous solution, heating, and stirring to dissolve 1, 1'-binaphthyl-8, 8'-dicarboxylic acid which is not completely reacted, impurities in the 1, 1'-binaphthyl-8, 8'-dicarboxylic acid and impurities generated by the reaction, and filtering and drying again to obtain a product; The solid superacid is used as a catalyst, and the 1, 1'-binaphthyl-8, 8'-dicarboxylic acid is subjected to catalytic dehydration condensation in the organic solvent, so that the anthraanthrone with higher yield and purity is obtained; and the pollution problem of waste sulfuric acid in the traditional process is solved.

Description

technical field [0001] The invention belongs to the technical field of organic dyes, in particular to a production method for catalyzed synthesis of anthracenthrone by a solid superacid. Background technique [0002] Anthracene is the main intermediate of high-grade colorants C.I. Vat Orange 3, C.I. Vat Orange 19, C.I. Vat Black 29, C.I. Vat Violet 6, C.I. Vat Violet 7, C.I. Vat Red 37 and C.I. Pigment Red 168. This intermediate was first reported by Germans and British. In addition, the synthesis of this compound is mentioned on pages 687 and 569 of "Principles of Intermediates and Dye Synthesis" written by H.H. Vorozhuzov in 1955. There are only two kinds of synthetic methods in these documents: one is to add 1,1′-binaphthyl-8,8′-dicarboxylic acid to 98% sulfuric acid to dehydrate and synthesize anthracenone; Add 1,1′-binaphthyl-8,8′-dicarboxylic acid slowly to low temperature in oleum, and use sulfur trioxide to dehydrate it to synthesize anthracenone. During the synth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C46/00C07C50/22B01J27/053
CPCC07C46/00B01J27/053C07C2603/54
Inventor 杨鹏
Owner 鞍山市五色石新材料科技有限公司
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