Method for preparing hexafluoroisobutene through environment-friendly visual light catalysis
A technology for the preparation of hexafluoroisobutene and catalysis, which is applied in the fields of chemical instruments and methods, preparation of halogenated hydrocarbons, organic chemistry, etc., can solve the problems of complex synthesis, unenvironmental protection of the process and process, high requirements for synthesis process and equipment, and achieve technological progress Simple, simplified preparation route and process, short preparation route
Active Publication Date: 2019-05-24
浙江诺诚技术发展有限公司
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Problems solved by technology
[0008] Most of the above methods use uncommercialized starting fluorine-containing compounds. In addition, the synthesis is relatively complicated, and the requirements for the synthesis process and equipment are high, and the process and process are not environmentally friendly.
Method used
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Experimental program
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Effect test
Embodiment
[0026] In a dry 50ml three-necked flask, add 0.0001mol of photocatalyst tris (2-phenylpyridine) iridium (tris-fac-Ir(ppy)3), and remove oxygen in the three-necked flask by vacuum-nitrogen-vacuum three cycles And place the three-neck flask in a dry ice-acetone bath. In a vacuum state, add 0.2 mol of ketene and 0.2 mol of hexafluoroacetone respectively, and stir to make the three reactants mix uniformly. Next, a 10W blue LED lamp was used to irradiate the reactants for 1 h under stirring conditions.
[0027] The conversion rate can reach 46% as detected by gas chromatography.
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The invention discloses a method for preparing hexafluoroisobutene through environment-friendly visual light catalysis. The method comprises the steps that 1, a photocatalyst is added into a transparent container, oxygen inside the transparent container is removed and placed into a low-temperature dry ice bath, and under the vacuum state, hexafluoroacetone and ketene are added and stirred to be uniform; 2, under the stirring condition, visual light is used for irradiating a reactant in step 1; 3, the hexafluoroisobutene product is obtained through rectification separation refining. The initiator hexafluoroacetone is a commercialized product, and is easy to obtain and low in cost; photocatalysis is adopted for preparation, and environment-friendliness is achieved; due to one-step preparation, the technological process is simple; adopted raw materials and reactants are easy to separate, and purification is easy.
Description
【Technical field】 [0001] The invention relates to the technical field of preparation of hexafluoroisobutene, in particular to the technical field of a method for preparing hexafluoroisobutene by green and environment-friendly visible light catalysis. 【Background technique】 [0002] Hexafluoroisobutylene (HFIB) is a known comonomer used in the preparation of polyvinylidene fluoride (PVDF) or other fluoropolymers that are useful in the preparation of piezoelectric materials, semiconductor photoresists, special fluorine Elastomers and fluorine coatings have a wide range of applications. [0003] The preparation methods of hexafluoroisobutene can be classified into the following three categories: [0004] First, eliminate the reaction. WO2001014294 reports that hexafluoroisobutene is catalyzed by defluorinating reagents such as Fe, C, Ni, and Cu using octafluoroisobutane to eliminate two F atoms at high temperature to obtain a yield of 57-72% hexafluoroisobutene. [0005] Sec...
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Login to View More IPC IPC(8): C07C17/26C07C21/18
Inventor 钟宝其张心悦
Owner 浙江诺诚技术发展有限公司