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Method for preparing 4,4'-di(2,4-dinitro-phenoxy) sulfone

A technology of dinitrophenoxy and dihydroxydiphenyl sulfone, which is applied in 4 fields to achieve the effects of less waste, convenient recycling and environmental friendliness

Inactive Publication Date: 2008-07-30
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] But the preparation method of 4,4'-bis(2,4-dinitrophenoxy)diphenyl sulfone, there is no published patent or literature report at present

Method used

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  • Method for preparing 4,4'-di(2,4-dinitro-phenoxy) sulfone
  • Method for preparing 4,4'-di(2,4-dinitro-phenoxy) sulfone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 25.0 grams (0.10 moles) of 4,4'-dihydroxydiphenylsulfone, 44.6 grams (0.22 moles) of 2,4-dinitrochlorobenzene, 110.4 grams (0.80 moles) of potassium carbonate, 700 milliliters of N, N- Put dimethylformamide and 180 ml of toluene into the reaction kettle, stir, heat and reflux for water separation for 18 hours, concentrate the reaction solution, recover the solvent for recycling, cool the reactant system, add water, precipitate a solid product, wash and dry , obtain 54.6 grams of 4,4'-bis(2,4-dinitrophenoxy) diphenyl sulfone crystal product, the purity is 99.6%, according to the actual 4,4'-bis(2,4-dinitrophenoxy) According to the amount and theoretical amount (58.2 grams) of phenylphenoxy)diphenylsulfone, the yield of 4,4'-bis(2,4-dinitrophenoxy)diphenylsulfone was calculated to be 93.8%.

Embodiment 2

[0029] 25.0 grams (0.10 moles) of 4,4'-dihydroxydiphenylsulfone, 54.4 grams (0.22 moles) of 2,4-dinitrobromobenzene, 55.2 grams (0.40 moles) of potassium carbonate, 150 milliliters of N, N- Dimethylacetamide and 15 milliliters of xylene were put into the reaction kettle, stirred, heated to reflux and separated from water for 6 hours, concentrated the reaction solution, recovered the solvent for recycling, cooled the reactant system, added water, precipitated a solid product, washed, Dry to obtain 47.5 grams of 4,4'-bis(2,4-dinitrophenoxy)diphenyl sulfone crystal product with a purity of 99.1%. Obtain 4,4'-bis(2,4-dinitrophenoxy) According to the amount and theoretical amount (58.2 grams) of 4,4'-bis(2,4-dinitrophenoxy)diphenyl sulfone, the yield was 81.7%.

Embodiment 3

[0031] 25.0 grams (0.10 moles) of 4,4'-dihydroxydiphenyl sulfone, 40.5 grams (0.20 moles) of 2,4-dinitrochlorobenzene, 10.6 grams (0.10 moles) of sodium carbonate, 90 milliliters of N-methyl - Put 2-pyrrolidone and 50 ml of dichlorobenzene into the reaction kettle, stir, heat to reflux and divide water for 16 hours, concentrate the reaction solution, recover the solvent for recycling, cool the reactant system, add water, precipitate the solid product, and wash , dried to obtain 42.8 grams of 4,4'-bis(2,4-dinitrophenoxy) diphenyl sulfone crystal product with a purity of 97.0%. According to the actual obtained 4,4'-bis(2,4- The amount of nitrophenoxy)diphenyl sulfone and the theoretical yield (58.2 g), the calculated yield of 4,4'-bis(2,4-dinitrophenoxy)diphenyl sulfone was 73.5%.

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Abstract

The invention relates to a method for preparing 4, 4'-double (2, 4- dinitrophenoxy) sulfone, which comprises the steps that: (1) 4, 4'-dihydroxy diphenyl sulfone and 2, 4- dinitrohalobenzenes with a molar ratio ranging from 1.0 : 2.0 to 1.0 : 2.2 are subject to a heat refluxing and water diversion reaction for 6 to 18 hours in a system comprising salt forming agents and organic solvents; (2) the reaction solution is concentrated, the reactant system is cooled, and the water is added in the reactant system so as to precipitate the solid product; the obtained product is filtered, washed and dried so as to obtain 4, 4'-double (2, 4- dinitrophenoxy) sulfone. The invention has simple operations and high product yield and purity, the solvents can be conveniently recycled and can be repeatedly used with few wastes, and the invention is environmentally friendly and suitable for industrialized production.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic organic compounds, in particular to a preparation method of 4,4'-bis(2,4-dinitrophenoxy)diphenylsulfone. Background technique [0002] Aromatic polyimide has excellent thermal stability, chemical stability, nuclear radiation resistance, excellent mechanical properties, electrical properties and resistance to organic solvents, and has been widely used in aerospace, electronic microelectronics, electrical and other fields . Because of its high temperature resistance, high strength, corrosion resistance, good insulation, and simple film forming process, it is an excellent functional material that can meet the performance requirements of LCD (liquid crystal display). [0003] 4,4'-bis(2,4-dinitrophenoxy)diphenyl sulfone is one of the important raw materials for the synthesis of highly branched aromatic polyimide monomers, that is, an important raw material for aromatic polyvalent primary amines...

Claims

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Application Information

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IPC IPC(8): C07C317/22C07C315/04C07C205/38C07C201/12
CPCY02P20/582
Inventor 虞鑫海
Owner DONGHUA UNIV
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