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A kind of preparation method of hexafluoro-2-butyne

A technology of butyne and hexachlorobutadiene is applied in the field of preparation of hexafluoro-2-butyne, and can solve the problems of difficulty in obtaining 2-butyne diacid, high raw material price of sulfur tetrafluoride, unsuitability for industrialization and the like , to achieve the effect of low cost, less three waste emissions, and easy availability of raw materials

Active Publication Date: 2021-03-16
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] The main problem of this technology is that the raw material 2-butynedioic acid used is not easy to obtain, and the raw material price of sulfur tetrafluoride is high. This synthetic route is not suitable for industrialization

Method used

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  • A kind of preparation method of hexafluoro-2-butyne
  • A kind of preparation method of hexafluoro-2-butyne
  • A kind of preparation method of hexafluoro-2-butyne

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] In a 2L stainless steel reaction kettle with a condenser, add 260g of hexachlorobutadiene, 780g of sulfolane, and 348g of potassium fluoride, raise the temperature to 100°C for reaction, collect the gas phase reaction products, wash with water, wash with alkali, and rectify to obtain hexafluoro- 2-butyne product, the product is sampled and analyzed by gas chromatography, the conversion rate of raw material hexachlorobutadiene is 99%, and the product selectivity is 96%.

Embodiment 2

[0036] Add 260g of hexachlorobutadiene, 1,300g of diethylene glycol dimethyl ether, and 710g of chromium fluoride into a 2L stainless steel reaction kettle with a condenser, heat up to 250°C for reaction, and collect the gaseous reaction products and wash them with water and alkali 1. The hexafluoro-2-butyne product was obtained by rectification, and the product was sampled for gas chromatography analysis. The conversion rate of raw material hexachlorobutadiene was 99%, and the product selectivity was 95%.

Embodiment 3

[0038] Add 260g of hexachlorobutadiene, 800g of N-methylpyrrolidone, and 610g of zinc fluoride into a 2L stainless steel reaction kettle with a condenser, heat up to 150°C for reaction, collect the gas phase reaction products and wash with water, alkali, and rectify The hexafluoro-2-butyne product was obtained, and the product was sampled for gas chromatography analysis. The conversion rate of raw material hexachlorobutadiene was 99%, and the product selectivity was 98.5%.

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Abstract

The invention discloses a hexafluoro-2-butyne preparation method which is characterized by subjecting hexachlorobutadiene and fluoride salt to reaction in solvents. The hexafluoro-2-butyne preparationmethod is simple in processing, low in cost, green and environmentally friendly and easy to achieve industrialization.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of hexafluoro-2-butyne. Background technique [0002] 1,1,1,4,4,4-Hexafluoro-2-butene (HFO-1336) is a substance with zero ODP and low GWP value. Z-HFO-1336 (cis-isomer of 1,1,1,4,4,4-hexafluoro-2-butene), considered to be one of the ideal substitutes for blowing agent HCFC-141b, belongs to The fourth-generation blowing agent can completely replace HCFC-141b and HFC-245fa in the future, and has broad market prospects. [0003] Hexafluoro-2-butyne is the key compound for the synthesis of 1,1,1,4,4,4-hexafluorobutene, and hexafluoro-2-butyne is also an important fluorine-containing fine chemical raw material, which can be used in the synthesis Key intermediates containing bis-trifluoromethyl building blocks, ODS substitutes, and monomers for fluoropolymers, such as key intermediates that can be used to synthesize ortho bis-trifluoromethyl benzene r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/00C07C17/20C07C21/18C07C17/358C07C21/22
CPCC07C17/00C07C17/20C07C17/358C07C21/22C07C21/18
Inventor 王宗令方伟李宏峰耿为利吴庆
Owner JUHUA GROUP TECH CENT
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