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A kind of method for synthesizing hexafluoro-2-butyne

A technology for butyne and hydrogen fluoride, applied in the field of synthesizing hexafluoro-2-butyne, can solve the problems of limiting the industrial production of hexafluoro-2-butyne, expensive reaction yield of raw materials, high raw material price, etc., and achieves less industrial waste. , low price, and the effect of reducing risk

Active Publication Date: 2018-06-01
TIANJIN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method raw material is expensive, and reaction yield is low
[0004] As can be seen from the above, the preparation of hexafluoro-2-butyne in the prior art has the problems of harsh reaction conditions, expensive raw materials and low reaction yield, which largely limits the industrial production of hexafluoro-2-butyne

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Preparation of cyclization catalyst: adopt co-precipitation method, the steps are as follows, CrCl with a molar ratio of 95:2:3 3 ,, Zn(NO 3 ) 2 , Cu(NO 3 ) 2 Mix the solutions, add 30wt.% ammonia water dropwise to the mixed solution, adjust the pH=9.0, precipitate and filter, wash with deionized water, dry, press and form to obtain the cyclization catalyst Cr-Cu-Zn;

[0026] Drying of cyclization catalyst: fill 20ml of Cr-Cu-Zn catalyst in a tubular reactor made of Incon alloy with an inner diameter of 1 / 2 inch and a length of 30cm; Dry at 400°C for 10 hours, then lower the temperature to 200°C;

[0027] Activation of the cyclization catalyst: after the drying step, maintain the reactor temperature at 200°C, activate the catalyst with 100ml / min nitrogen and 20ml / min hydrogen fluoride for 4 hours; activate the catalyst with 100ml / min nitrogen and 50ml / min hydrogen fluoride for 4 hours; 50ml / min nitrogen Activate the catalyst with 100ml / min hydrogen fluoride for...

Embodiment 2

[0036] (1) Preparation of cyclization catalyst: adopt co-precipitation method, the steps are as follows, CrCl with a molar ratio of 95:2:3 3 ,, Zn(NO 3 ) 2 Ni(NO 3 ) 2 Mix the solutions, add 30wt.% ammonia water dropwise to the mixed solution, adjust the pH=9.0, precipitate and filter, wash with deionized water, dry, press and form to obtain the cyclization catalyst Cr-Ni-Zn;

[0037] Drying of cyclization catalyst: put 20ml Cr-Ni-Zn catalyst into a fixed-bed reactor, and the fixed-bed reactor is heated with an open tube heating furnace; the catalyst is first raised to 400 at 10°C / min under the protection of 50ml / min nitrogen ℃ for 10 hours, then lower the temperature to 200 ℃;

[0038] Activation of the cyclization catalyst: after the drying step, maintain the reactor temperature at 200°C, activate the catalyst with 100ml / min nitrogen and 20ml / min hydrogen fluoride for 4 hours; activate the catalyst with 100ml / min nitrogen and 50ml / min hydrogen fluoride for 4 hours; 50ml / ...

Embodiment 3

[0047] (1) Preparation of cyclization catalyst: adopt co-precipitation method, the steps are as follows, Cr(NO 3 ) 3 ,, ZnCl 2 , Co(NO 3 ) 2 ,In(NO 3 ) 3 The solutions are mixed, 40wt.% ammonia water is added dropwise to the mixed solution, the pH is adjusted to 7.5, the precipitate is filtered, washed with deionized water, dried, and press-molded to obtain the cyclization catalyst Cr-Zn-Co-In;

[0048] Drying of the cyclization catalyst: 20ml Cr-Zn-Co-In catalyst is packed into a fixed-bed reactor, and the fixed-bed reactor is heated with an open-type tube heating furnace; under the protection of 50ml / min nitrogen, first rise to Dry at 400°C for 10 hours, then lower the temperature to 200°C;

[0049] Activation of the cyclization catalyst: heat the reactor to 200°C, activate the catalyst with 100ml / min nitrogen and 20ml / min hydrogen fluoride for 4 hours; activate the catalyst with 100ml / min nitrogen and 50ml / min hydrogen fluoride for 4 hours; Hydrogen fluoride activate...

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Abstract

The invention discloses a hexafluoropropylene-2-butyne synthesizing method. Hexachlorobutadiene (CCl2=CCl-CCl=CCl2) is taken as the raw material to generate hexafluoropropylene-2-butyne under the action of a catalyst, the raw material hexachlorobutadiene is easy to obtain and low in cost. The gaseous-phase circulating fluorination method is adopted, the discharge level of three industrial wastes is low, the yield of products is high, and production cost is reduced greatly; the gaseous-phase circulating fluorination method is conducted at normal temperature, the traditional high-pressure telomerization process route is avoided, and risks in industrial safety production are reduced greatly; meanwhile, the method has the advantage that operation is easy and is totally suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and in particular relates to a method for synthesizing hexafluoro-2-butyne which is easy for industrial production. Background technique [0002] Hexafluoro-2-butyne has high industrial value and is a widely used industrial raw material. Its downstream products can be used in precision electronic circuit board cleaning agents, pesticides and insecticides, and fluorine-containing pharmaceutical intermediates, etc. It has high application value in the synthesis of fine chemicals. It has been reported that hexafluoro-2-butyne is widely used in the synthesis of bistrifluoromethyl stacking blocks, the synthesis of hexafluoro-2-butene, and the synthesis of new corrosion-resistant materials. [0003] There are few reports on the synthesis of hexafluoro-2-butyne. Patent (US20110288349) reports a kind of synthetic method, nonafluorobutane (molecular formula CF 3 -CF 2 -CFH-CF 3 ) and hydroge...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/358C07C21/22C07C17/20C07C23/06
CPCC07C17/20C07C17/358C07C21/22C07C23/06
Inventor 张美玲姚智周彪张苹丽孙传才
Owner TIANJIN MEDICAL UNIV
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