New method for preparing hexafluorobutadiene

A technology of perfluorobutadiene and a new method, applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., can solve the problems of high chemical reaction activity, harsh reaction conditions, and many by-products, etc. The effect of obtaining, good conversion rate and simple equipment

Active Publication Date: 2016-01-27
泉州宇极新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented technology describes methods for making certain chemical compounds that can be useful or harmful substances found naturally occurring worldwide at very small concentrations (<10 ppb). These processes involve reacting hydrogen fluoride with other metals like iron chlorine, copper oxides, calcium carbonate, etc., producing various products such as metal hydrides, organic peroxy acids, ammonium salts, nitro esters, carboxylates, sulfones, olefins, alcohols, ketons, alkenes, alkynies, epoxanes, pyridines, quinolines, pigments, dyes, pesticides, herbs, medicinal agents, explosives, fertilizers, polymerizable resists, plastic coatings, adhesive tapes, lubricating greases, paints, solvents, cleaning solutions, cosmetic compositions, electronic devices, sensors, batteries, fuel cells, catalyst carriers, biological samples, foodstuffs, healthcare supplies, and others.

Problems solved by technology

This patents describes processes for producing specific types of molecules called carbon hexasulfonate esters through condensations involving formaldehyde/tritoluene dichloromalefnirile(CTFEI)). These chemistries have several advantages over existing techniques like sulfoxidil acids and triphenols but they also require complex procedures and involve multiple stages. Additionally, these prior art systems suffer from poor efficiency when generating desired products.

Method used

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  • New method for preparing hexafluorobutadiene
  • New method for preparing hexafluorobutadiene
  • New method for preparing hexafluorobutadiene

Examples

Experimental program
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Effect test

Embodiment 1

[0044] The first step: (1) in the reactor of 60 centimeters in length, the ceramic tubing of diameter 1 / 2 inch, fill 30mlFeCl 3 / C (wt, 6%) as a catalyst, (2) under the protection of nitrogen, after heating to 500 ° C in an electric furnace, HFC-134a and Br 2 Mixed and introduced into the reactor at a rate of 1:2 with a molar ratio, (3) The contact time between the reactant and the catalyst was 18 seconds. According to gas chromatography analysis, the conversion rate of HFC-134a reached 97%, CF 3 CFBr 2 The selectivity reached 62.2%; the crude product was separated and purified to obtain CF with a purity of 99.9%. 3 CFBr 2 .

[0045] Step 2: Under nitrogen protection, in a 250ml three-necked flask equipped with a thermometer and a stirrer, add 20g of activated zinc powder and 40ml of dried DMF (moisture content below 50ppm), heat to 60°C, and stir Slowly add CF under the condition 3 CFBr 2 27g, adjust the rate of addition, keep the reaction temperature below 90°C during ...

Embodiment 2

[0048] The first step: (1) in the reactor of 60 centimeters in length, the ceramic tubing of diameter 1 / 2 inch, fill 30mlCuCl 2 / C (wt, 6%) as a catalyst, (2) under the protection of nitrogen, after heating to 550 ° C in an electric furnace, HFC-134a and Br 2 Mixed and introduced into the reactor at a rate of 1:3 in molar ratio, (3) The reaction contact time between the reactant and the catalyst was 18 seconds. According to gas chromatography analysis, the conversion rate of HFC-134a reached 99%, CF 3 CFBr 2 The selectivity reached 70.5%; the crude product was separated and purified to obtain CF with a purity of 99.9%. 3 CFBr 2 .

[0049] Step 2: Under nitrogen protection, in a 250ml three-necked flask equipped with a thermometer and a stirrer, add 20g of activated zinc powder and 40ml of dried NMP (moisture content below 50ppm) respectively, heat to 60°C, and stir Slowly add CF under the condition 3 CFBr 2 27g, adjust the rate of addition, keep the reaction temperature ...

Embodiment 3

[0052] The first step: (1) in length 60 centimeters, in the reactor of internal helical stainless steel tubing of diameter 1 / 2 inch, fill 30mlFeBr 3 / C (wt, 6%) as a catalyst, (2) under the protection of nitrogen, after heating to 550 ° C in an electric furnace, HFC-134a and Br 2 Mixed and introduced into the reactor at a rate of 1:3 in molar ratio, (3) The reaction contact time between the reactant and the catalyst was 15 seconds. According to gas chromatography analysis, the conversion rate of HFC-134a reached 99.5%, CF 3 CFBr 2 The selectivity reached 75.5%; the crude product was separated and purified to obtain CF with a purity of 99.9%. 3 CFBr 2 .

[0053] The second step: under nitrogen protection, in a 250ml three-necked flask equipped with a thermometer and a stirrer, add 25g of activated zinc powder and 45ml of dried acetonitrile (water content below 50ppm) respectively, heat to 60°C, and Slowly add CF dropwise under stirring condition 3 CFBr 2 25g, adjust the r...

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Abstract

The invention relates to a new method for preparing hexafluorobutadiene. The new method is characterized by comprising the following steps that 1, HFC-134a and Br2 are subjected to a continuous gas phase catalysis reaction under the effect of a catalyst with metal chloride or bromide as an active component to prepare CF3CFBr2; 2, CF3CFBr2 is dripped into a reactor for aprotic polar solvent in which zinc powder is dissolved to prepare trifluoro vinyl zinc bromide; 3, with ferric salt and copper salt serving as catalysts, in the aprotic polar solvent, trifluoro vinyl zinc bromide is subjected to a telomerization reaction to generate a target product hexafluorobutadiene. The refrigerant HFC-134 a and Br2 which are used on a large scale at present and gradually obsoleted are used as starting raw materials, the materials are easy to obtain and low in price, the reaction is carried out under the gas phase condition, the reaction condition is easy to control, and the method is a C4F6 preparing method having a great market application prospect.

Description

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Claims

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Application Information

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Owner 泉州宇极新材料科技有限公司
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