A green and environmentally friendly method for preparing hexafluoroisobutene by visible light catalysis
A technology for hexafluoroisobutene and catalytic preparation, which is applied in chemical instruments and methods, halogenated hydrocarbon preparation, organic chemistry and other directions, can solve the problems of complex synthesis, unenvironmentally friendly process and process, high requirements for synthesis process and equipment, and achieves the technological process. Simple, simplified preparation route and process, the effect of short preparation route
Active Publication Date: 2022-02-08
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 green and environment-friendly method for preparing hexafluoroisobutene by visible light catalysis. The steps include: a) adding photocatalyst into a transparent container, removing oxygen in the transparent container and placing it in a low-temperature dry ice bath; Fluoroacetone and vinyl ketone are stirred evenly; b) under stirring condition, irradiate the reactant in step a) with visible light and c) obtain hexafluoroisobutene product through rectification, separation and purification. The starting material hexafluoroacetone of the present invention is a commercial product, easy to obtain, and low in cost; it is prepared by photocatalysis, and is environmentally friendly; it is prepared by a one-step method, and the process is simple; the raw materials and reactants used are easy to separate, and the purification is simple.
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...
Claims
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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
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