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Preparation method of 2,3,5,6-tetrachloro-terephthalaldehyde

A technology of tetrachloroterephthalaldehyde and tetrachloro-p-phenylene dichlorobenzyl, which is applied in two fields, can solve the problems of low yield and expensive raw materials, and achieve the effects of low production cost, easy operation, and no waste acid

Active Publication Date: 2013-06-05
SHANGHAI HETENG FINE CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There is also document DE2201251 showing that 2,3,5,6-tetrachloro-p-phenylene dichlorobenzyl benzyl can be used as raw material, and hydrolyzed in ice water after reacting with SO3 to obtain 2,3,5,6-tetrachloro-terephthalaldehyde, But the yield is not high, also produce a lot of waste acid
[0006] In summary, the above methods are either expensive in raw materials, or have great disadvantages, so it is necessary to find another preparation method

Method used

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  • Preparation method of 2,3,5,6-tetrachloro-terephthalaldehyde

Examples

Experimental program
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Embodiment 1

[0019] Add 31.3 grams of 2,3,5,6-tetrachloro-p-benzenedichlorobenzyl, 600 grams of dilute nitric acid with a weight concentration of 5% and 1.5 grams of vanadium pentoxide into the autoclave, and then put it at 150°C and 0.8MPa pressure The oxidation reaction is 20 hours. Cool, filter, then reconsolidate with acetone and water. After drying, 23 g of 2,3,5,6-tetrachloroterephthalaldehyde was obtained, and the yield was about 85%. The mother liquor can be recycled after removing HCL by adding nitric acid.

Embodiment 2

[0021] Add 31.3 grams of 2,3,5,6-tetrachloro-p-phenylenedichlorobenzyl, 400 grams of dilute nitric acid with a weight concentration of 10% and 1 gram of vanadium pentoxide into the autoclave, and then at 120°C and 0.25MPa pressure Oxidize for 20 hours. Cool, filter, then reconsolidate with acetone and water. After drying, 20.5 g of 2,3,5,6-tetrachloroterephthalaldehyde was obtained, and the yield was about 75%. The mother liquor can be recycled after removing HCL by adding nitric acid.

Embodiment 3

[0023] Add 31.3 grams of 2,3,5,6-tetrachloro-p-phenylene dichlorobenzyl, 600 grams of 8% dilute nitric acid by weight and 1.5 grams of vanadium pentoxide into the autoclave, and then oxidize it at 150°C and 0.5MPa pressure. hour. Cool, filter, then reconsolidate with acetone and water. After drying, 24 g of 2,3,5,6-tetrachloroterephthalaldehyde was obtained, and the yield was about 88%. The mother liquor can be recycled after removing HCL by adding nitric acid.

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Abstract

The invention discloses a preparation method of 2,3,5,6-tetrachloro-terephthalaldehyde, comprising the following steps: carrying out an oxidation reaction on 2,3,5,6-tetrachloro-p-dibenzyl chloride, nitric acid and vanadium pentoxide, and then collecting the target product from the reaction products. The method provided by the invention has high yield above 88%, is simple in operation, almost hasno waste acid, has low production cost, and is easy for industrialization.

Description

Technical field [0001] The invention relates to a preparation method of 2,3,5,6-tetrachloroterephthalaldehyde. Background technique [0002] 2,3,5,6-Tetrachloroterephthalaldehyde is a chemical intermediate of medicines and pesticides, and has a wide range of applications in the fields of medicine and pesticides. At present, there are mainly the following preparation methods: [0003] Documents Ger360414, Neth6408879, Us3146086, Russian chemicalBulletin, 46(1), 101, mention that a, a, à, à, 2, 3, 5, 6-octachloro-p-dimethylbenzene is hydrolyzed in concentrated sulfuric acid The target product 2,3,5,6-tetrachloroterephthalaldehyde is obtained, with a yield of about 60%, and a large amount of waste acid is generated. [0004] The document JOC, 48(5), 727, 1983 mentions the production of 2,3,5,6-tetrachloroterephthalaldehyde by oxidation with 2,3,5,6-tetrachloroterephthalaldehyde as a raw material. The yield is : 40.4%. [0005] There is also the document DE2201251 indicating that 2,3,5...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/55C07C45/27
Inventor 施冠成唐卫星滑国钰孟海成
Owner SHANGHAI HETENG FINE CHEM
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