Hexafluoro-2-butyne preparation method

A technology of butyne and hexachlorobutadiene, which is applied in the field of preparation of hexafluoro-2-butyne, can solve the problems that it is not suitable for industrialization, 2-butynedioic acid is not easy to obtain, and the raw material price of sulfur tetrafluoride is high. Achieve the effects of easy availability of raw materials, low cost, and less discharge of three wastes

Active Publication Date: 2018-09-14
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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  • Hexafluoro-2-butyne preparation method
  • Hexafluoro-2-butyne preparation method
  • Hexafluoro-2-butyne preparation method

Examples

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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 Applications(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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