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A kind of preparation method of 1,1,1,2,4,4,4-heptafluoro-2-butene

A technology of butene and hexachlorobutadiene, applied in the field of synthesis of fluorine-containing organic compounds, can solve problems such as a large amount of waste, environmental pollution, large waste and the like

Active Publication Date: 2021-11-02
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. In the method, hexachlorobutadiene and hydrogen fluoride are used as raw materials, and under gas-phase conditions, a chromium-based catalyst is used as a fluorine-chlorine exchange catalyst, and 1, 1, 1, 2, 4, 4, 4- Heptafluoro-2-butene. Compared with the prior art, the preparation method of 1,1,1,2,4,4,4-heptafluoro-2-butene provided by the present invention has the following advantages: 1. The gas-phase fluorination method adopted in the present invention is Cyclic fluorination has fewer industrial three wastes and greatly reduces production costs; 2. The present invention can realize rapid multiple cycle fluorination, improve product yield, and simple product separation and purification; 3. It has cheap raw materials, convenient sources and simple operation. Advantages, suitable for industrial 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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Patent Type & Authority Patents(China)
IPC IPC(8): C07C21/18C07C17/20C07C17/087B01J23/26B01J23/86B01J35/02B01J37/03B01J37/26B01J35/00
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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