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Preparation method of 1,1,1,3,3,3-hexafluoro-2-(4-styrene)propanol

A preparation process and technology of styrene, applied in 1 field, can solve the problems of high protection and equipment requirements for operators, difficult disposal of magnesium bromide, a by-product of the three wastes, difficulty in using hexafluoroacetone, etc., and achieve low protection and equipment requirements , easy storage, good market prospects

Inactive Publication Date: 2015-12-09
CHANGSHU XINHUA CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] At present, the preparation of 1,1,1,3,3,3-hexafluoro-2-(4-styrene) propanol generally adopts styrene magnesium bromide and hexafluoroacetone as raw materials for production, and its The disadvantages are: raw materials are expensive; hexafluoroacetone is relatively difficult to use and store, and requires relatively high protection and equipment requirements for operators. Hexafluoroacetone still belongs to 2.3 types of toxic gases, and the risk of poisoning is high; the final three wastes By-products such as magnesium bromide and bromine-containing wastewater are not easy to treat, and have a great impact on the environment

Method used

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  • Preparation method of 1,1,1,3,3,3-hexafluoro-2-(4-styrene)propanol

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Embodiment Construction

[0014] The specific implementation manners of the present invention will be further described below in conjunction with the drawings and examples. The following examples are only used to illustrate the technical solution of the present invention more clearly, but not to limit the protection scope of the present invention.

[0015] The technical scheme of concrete implementation of the present invention is:

[0016] A preparation process for 1,1,1,3,3,3-hexafluoro-2-(4-styrene) propanol, comprising the steps of:

[0017] 214.5 grams of hexafluoroacetone trihydrate (specific gravity ≥ 1.59) is dehydrated with 500 grams of 98% sulfuric acid (at a constant temperature of 110-135 degrees) (controlling the concentration of sulfuric acid to not less than 85%) to generate hexafluoroacetone gas;

[0018] Pre-cool the hexafluoroacetone gas to -5~5°C, and then react with 500 grams of styrene magnesium chloride Grignard reagent (concentration: 1.3~1.5mol / kg) at -20~-40°C under normal pre...

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Abstract

The invention discloses a preparation method of 1,1,1,3,3,3-hexafluoro-2-(4-styrene)propanol. According to the preparation method, phenylethenyl magnesium chloride Grignard reagent is reacted with hexafluoroacetone at a low temperature, and an obtained product is subjected to washing and refining so as to obtain a finished product with a content of 99.0% or higher. Cheaper raw materials are adopted in the preparation method, the raw materials are safer for storage, transportation, and using, and requirement on operator protection and equipment is low; the preparation method is more reasonable, safe, simple, low in energy consumption, high in yield, and low in environmental pollution; the finished product is a high-activity organic intermediate with a fluorine double bond structure, augmented products of the finished product are more, application range is extremely wide, and market prospect is promising; an obtained three wastes byproduct is magnesium chloride which is an excellent flame-resistant material in the field of building material, and can be recycled; and three wastes processing of chlorine-containing waste water is convenient, and less pollution on the environment is caused.

Description

technical field [0001] The invention relates to an intermediate for synthesis of medicine, pesticide, rubber and the like, in particular to a preparation process of 1,1,1,3,3,3-hexafluoro-2-(4-styrene)propanol. Background technique [0002] At present, the preparation of 1,1,1,3,3,3-hexafluoro-2-(4-styrene) propanol generally adopts styrene magnesium bromide and hexafluoroacetone as raw materials for production, and its The disadvantages are: raw materials are expensive; hexafluoroacetone is relatively difficult to use and store, and requires relatively high protection and equipment requirements for operators. Hexafluoroacetone still belongs to 2.3 types of toxic gases, and the risk of poisoning is high; the final three wastes By-products such as magnesium bromide and bromine-containing waste water are also not easy to treat and have a great impact on the environment. Contents of the invention [0003] The object of the present invention is to provide a kind of preparatio...

Claims

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Application Information

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IPC IPC(8): C07C29/64C07C33/46
CPCC07C29/64C07C33/46
Inventor 陆志忠窦建华
Owner CHANGSHU XINHUA CHEM
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