Preparing process of 4,4-dinitro diphenyl ether

A technology of dinitrodiphenyl ether and p-nitrochlorobenzene, which is applied in 4 fields, can solve the problems of large environmental pollution, large environmental pollution, complicated post-processing, etc., and achieves low environmental pollution, good product quality and low production cost. low effect

Inactive Publication Date: 2007-06-27
忻雪琴
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The diphenyl ether nitration method is to directly nitrate diphenyl ether with nitric acid to prepare 4,4'-dinitrodiphenyl ether. This method has many by-products and low yield, and uses a strong acid as a reactant and catalyst, and the post-treatment of the product is complicated. Lock, environmental pollution, has been eliminated
Its main disadvantage is that it generates NO and NO which are easy to form acid rain while generating the key intermediate p-nitrophenolate 2 (or N 2 o 3 ) gas, which pollutes the environment more

Method used

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  • Preparing process of 4,4-dinitro diphenyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Put 15.75Kg of p-nitrochlorobenzene, 860g of sodium benzoate, 6Kg of sodium carbonate and 10L of N-methylpyrrolidone into a 500L reactor with stirring device, and heat up to 190-210°C by passing steam into the interlayer of the reactor , the condensation reaction proceeds under the conditions. The reaction was finished after 8 hours, and the N-methylpyrrolidone solvent was distilled off. Cool to 85°C, add 300L of distilled water, precipitate the product, centrifuge and dry to obtain 11.0Kg of 4,4'-dinitrodiphenyl ether, yield 85.0%, melting point 143.2-144.3°C, content 99.5% (HPLC).

Embodiment 2

[0025] Other conditions are the same as in Example 1, and the solvent is recycled N-methylpyrrolidone. 11.6Kg of 4,4'-dinitrodiphenyl ether was obtained, with a yield of 89.6%, a melting point of 142.8-144.0°C, and a content of 99.3% (HPLC).

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Abstract

The present invention is preparation process of 4, 4'-dinitro diphenyl ether, and belongs to the field of fine chemical technology. P-nitro chlorobenzene produces condensation reaction inside polar non-protonic solvent at 190-210 deg.c in the presence of catalyst alkali metal carboxylate and alkali metal carbonate, and the reaction product is crystallized to obtain 4, 4'-dinitro diphenyl ether. The present invention features the green production process with less environmental pollution and no nitroxide release, low production cost, high product quality and high product yield.

Description

Technical field [0001] The invention relates to a preparation method of 4,4'-dinitrodiphenyl ether, which belongs to the technical field of fine chemicals. Background technique [0002] 4,4'-Dinitrodiphenyl ether is an important fine chemical product. It is a useful intermediate for the manufacture of medicine and pesticides. Its reduction product 4,4'-Diaminodiphenyl ether is a new type of special engineering plastic poly It is an important monomer of high temperature resistant resins such as imide and polyaramid, and also a crosslinking agent for polymer materials such as high performance heat resistant epoxy resin and polyurethane. With the continuous upgrading of my country's industrial technology, the performance requirements of corresponding polymer materials are getting higher and higher, which will greatly promote the development of 4,4'-dinitrodiphenyl ether as a key new material monomer raw material. Therefore, the preparation of 4,4'-dinitrodiphenyl ether has gre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/38C07C201/12
Inventor 忻雪琴
Owner 忻雪琴
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