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Preparation method of 1,1,1,2,4,4,4-heptafluoro-2-butene

A technology of butene and hexachlorobutadiene, which is applied in the field of synthesis of fluorine-containing organic compounds, can solve the problems of unfavorable industrial production, a large amount of waste, and large waste, and achieve the goal of less industrial waste, cheap raw materials, and convenient sources Effect

Active Publication Date: 2018-11-30
CIVIL AVIATION UNIV OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can reduce the consumption of solvent, it will also produce a large amount of waste, which is also unfavorable for industrial production;
[0005] It can be seen that the above method of synthesizing 1,1,1,2,4,4,4-heptafluoro-2-butene mainly adopts a liquid-phase catalytic method, and the liquid-phase catalytic method consumes a large amount of organic solvents , will also produce a large amount of waste, which is likely to cause environmental pollution and is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The preparation method of 1,1,1,2,4,4,4-heptafluoro-2-butene provided in this example comprises the following steps:

[0029] (1) Preparation of chromium-based catalyst precursor: adopt the co-precipitation method, the steps are as follows, the CrCl with a molar ratio of 85:5:10 3 , Zn(NO 3 ) 2 Mix evenly with the graphene solution, ultrasonically treat for 30 minutes at room temperature, slowly add 30wt.% ammonia water to the above mixed solution, adjust the pH of the solution to 9.0, and after 4 hours of precipitation and aging, filter the precipitate and wash it with deionized water Precipitates were calcined at 400°C and pressed into shape to obtain a chromium-based catalyst precursor.

[0030] Activation of chromium-based catalyst: 10ml of chromium-based catalyst precursor was loaded into a fixed-bed reactor, and the fixed-bed reactor was heated with an open tube heating furnace. Drying was carried out for 10 hours; then hydrogen fluoride was introduced at a rat...

Embodiment 2

[0033] The preparation method of 1,1,1,2,4,4,4-heptafluoro-2-butene provided in this example comprises the following steps:

[0034] (1) Preparation of chromium-based catalyst precursor: adopt the co-precipitation method, the steps are as follows, the CrCl with a molar ratio of 85:5:10 3 , Co(NO 3 ) 2 Mix evenly with activated carbon solution, ultrasonically treat for 30 minutes at room temperature, slowly add 30wt.% ammonia water to the above mixed solution, adjust the pH of the solution to 9.0, after 4 hours of precipitation and aging, filter the precipitate, and wash the precipitate with deionized water The product was calcined at 400°C and pressed into shape to obtain a chromium-based catalyst precursor.

[0035] Activation of chromium-based catalyst: 10ml of chromium-based catalyst precursor was loaded into a fixed-bed reactor, and the fixed-bed reactor was heated with an open tube heating furnace. Drying was carried out for 10 hours; then hydrogen fluoride was introdu...

Embodiment 3

[0038] The preparation method of 1,1,1,2,4,4,4-heptafluoro-2-butene provided in this example comprises the following steps:

[0039] (1) Preparation of chromium-based catalyst precursor: Co-precipitation method, the steps are as follows, the molar ratio of 82:5:13 Cr(NO 3 ) 3 , Ni(NO 3 ) 3 Mix evenly with the carbon nanotube solution, ultrasonically treat for 30 minutes at room temperature, slowly add 30wt.% ammonia water to the above mixed solution, adjust the pH of the solution to 9.0, after 4 hours of precipitation and aging, filter the precipitate, and use deionized water The precipitate was washed, calcined at 400° C., and pressed into shape to obtain a chromium-based catalyst precursor.

[0040] Activation of chromium-based catalyst: 10ml of chromium-based catalyst precursor was loaded into a fixed-bed reactor, and the fixed-bed reactor was heated with an open tube heating furnace. Drying was carried out for 10 hours; then hydrogen fluoride was introduced at a rate o...

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Abstract

The invention discloses a preparation method of 1,1,1,2,4,4,4-heptafluoro-2-butene. The method uses hexachlorobutadiene and hydrogen fluoride as raw materials and uses a chromium-based catalyst as a fluorine-chlorine exchange catalyst to form the 1,1,1,2,4,4,4-heptafluoro-2-butene under gas phase conditions through a plurality of gas-phase catalytic reactions. Compared with the prior art, the preparation method of the 1,1,1,2,4,4,4-heptafluoro-2-butene provided by the invention has the following advantages: 1, the gas phase fluorination method adopted in the method is a cycle fluorination method, has less three industrial wastes (waste water, waste gases and solid waste), and greatly reduces the production costs; 2, the method can realize rapid and multiple-cycle fluorination, improve a product yield, and have simple separation and purification of the product; and 3, the method has the advantages of cheap raw materials, convenient sources and simple operation, and is suitable for industrialized production.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, in particular to a method for synthesizing fluorine-containing organic compounds. Background technique [0002] Due to its excellent working performance and environmental performance, hydrofluoroolefin (HFO) has gradually become a substitute for a new generation of reversed-phase chromatographic columns (ODS), and has been widely used in refrigeration, fire extinguishing, foaming, etching, cleaning and other fields. a wide range of applications. And 1,1,1,2,4,4,4-heptafluoro-2-butene is an important compound in HFO, which can not only be used in the fields of refrigeration, foaming, drying or degreasing solvents, but also As an intermediate for the preparation of hexafluoro-2-butyne. However, there are still few methods for synthesizing 1,1,1,2,4,4,4-heptafluoro-2-butene. There are two main ways to synthesize butene: [0003] (1) John T.Maynard [Journal of Organic Chemistry...

Claims

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Application Information

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IPC IPC(8): C07C21/18C07C17/20C07C17/087B01J23/26B01J23/86B01J35/02B01J37/03B01J37/26
CPCC07C17/087C07C17/206B01J23/26B01J23/864B01J23/866B01J37/035B01J37/26B01J35/00B01J35/30C07C21/18
Inventor 周晓猛李秀涛罗星娜张青松
Owner CIVIL AVIATION UNIV OF CHINA
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