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Preparation method of polynitrostyrene

A technology of nitrostyrene and fuming nitric acid, applied in the field of organic polymers, can solve the problems of low nitration rate, small reaction interface, insoluble final product, etc., achieve high nitro group introduction rate, short reaction time, and simple method Effect

Inactive Publication Date: 2017-06-09
FOSHAN SHANGHAO DOOR & WINDOW CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The synthesis of this type of polynitrostyrene uses a cross-linked PS matrix, the reaction interface is small, the nitration rate is not high, and the final product is insoluble, which affects the functionalization reaction yield and limits their application in terms of solubility.
[0003] Zhang Jing et al. improved the NRDC reaction route, and used m-nitrotoluene as solvent to nitrate non-crosslinked PS to obtain a higher nitration rate, but the high price of m-nitrotoluene affected the industrial application of this research

Method used

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  • Preparation method of polynitrostyrene

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Experimental program
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Effect test

Embodiment 1

[0015] Add 20 parts by weight of a mixture of fuming nitric acid and concentrated sulfuric acid (ratio: 1:1), 40 parts by weight of dichloromethane into the dried mixing tank, then start stirring for 1 hour, cool to 0°C, and slowly drop in quantitative 100 parts by weight of styrene monomer were stirred for 3 hours, and absolute ethanol was added dropwise to terminate the reaction, and the product was filtered to obtain a product of colorless crystals. The product was washed with deionized water and dried to constant weight.

[0016] The yield calculated by weighing method was 87%, and the nitro group introduction rate was 96%.

Embodiment 2

[0018] Add 30 parts by weight of a mixture of fuming nitric acid and concentrated sulfuric acid (ratio: 1:2) and 30 parts by weight of dichloromethane into the dried mixing tank, then start stirring for 1 hour, cool to 0°C, and slowly drop in quantitative 100 parts by weight of styrene monomer were stirred for 3 hours, and absolute ethanol was added dropwise to terminate the reaction, and the product was filtered to obtain a product of colorless crystals. The product was washed with deionized water and dried to constant weight.

[0019] The yield calculated by weighing method was 92%, and the nitro introduction rate was 98%.

Embodiment 3

[0021] Add 30 parts by weight of a mixture of fuming nitric acid and concentrated sulfuric acid (ratio: 1:3) and 30 parts by weight of dichloromethane into the dried mixing tank, then start stirring for 1 hour, cool to 0°C, and slowly drop in quantitative 100 parts by weight of styrene monomer were stirred for 3 hours, and absolute ethanol was added dropwise to terminate the reaction, and the product was filtered to obtain a product of colorless crystals. The product was washed with deionized water and dried to constant weight.

[0022] The yield calculated by the weighing method was 96%, and the nitro group introduction rate was 98%.

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Abstract

The invention relates to the field of organic polymers, particularly a polynitrostyrene. Fuming nitric acid is utilized to perform one-step synthesis of the polynitrostyrene. The consumption of concentrated sulfuric acid is increased, the relative molecular mass of the polynitrostyrene is increased, and the yield is enhanced. The preparation method has the advantages of short reaction time, high nitro introduction rate, simple process, low cost and the like, and can be used for industrial production.

Description

technical field [0001] The invention relates to the field of organic polymers, in particular to a polynitrostyrene. Background technique [0002] The benzene ring of polystyrene (PS) is prone to functionalization reactions (such as nitration, sulfonation, etc.), the hydrogen atoms on the benzene ring are replaced by nitro groups to form polynitrostyrene, and the reduction of nitro groups produces polyaminobenzene vinyl. Such functional polymers have broad application prospects in the fields of self-assembly, biomedical polymers, water treatment, ion exchange resins, chelating agents, immobilized catalysts and dyes. Bachman et al. were the first to prepare azo polymers from PS through the four-step reaction of nitration, reduction, diazotization, and coupling (referred to as the NRDC reaction route). The synthesis of this kind of polynitrostyrene adopts cross-linked PS matrix, the reaction interface is small, the nitration rate is not high, and the final product is inso...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F8/30C08F112/08C08F112/14
CPCC08F8/30C08F112/14C08F112/08
Inventor 刘正英
Owner FOSHAN SHANGHAO DOOR & WINDOW CO LTD
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