Preparation method of hexafluorobutadiene

A technology for hexafluorobutadiene and butene, which is applied in the field of hexafluorobutadiene preparation, can solve the problems of not considering rearrangement reaction and how to remove it, and achieves the reduction of impurity content, small equipment investment, and reduced cost. effect of stress

Active Publication Date: 2021-07-02
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, this method uses X-type molecular sieves, A-type molecular sieves, activated carbon, etc. to adsorb impurities in hexafluorobutadiene after reactive distillation. There are some problems in this process, that is, X-type molecular sieves have a strong catalytic effect on hexafluorobutadiene. , A-type molecular sieves contain acid centers and will also catalyze the reaction
Therefore, this patent technology does not consider how to reduce the occurrence of rearrangement reactions during the preparation process, nor does it consider how to remove the generated hexafluoro-2-butyne

Method used

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  • Preparation method of hexafluorobutadiene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] use figure 1 In the process shown, the dechlorination reactor 1 used in the dechlorination reaction is a mechanically stirred vertical jacketed reactor with a volume of 250 liters. The starting material is R-1 in Table 1.

[0045] The organic solvent is ethanol, and the raw materials of ethanol and 3,4-dichlorohexafluoro-1-butene are dehydrated to 2ppm by using 3A molecular sieves. The dechlorination reactor 1 is continuously cleaned with dehydrated ethanol until the moisture content of the ethanol flowing out from the dechlorination reactor 1 is lower than 3 ppm.

[0046] Before the dechlorination reaction starts, add 150 liters of ethanol, 5 kilograms of zinc powder, and 0.25 kilograms of zinc chloride into the dechlorination reaction kettle 1 . The dechlorination reactor 1 was heated to 40° C., and the stirring speed was 250 rpm.

[0047] The 3,4-dichlorohexafluoro-1-butene raw material is continuously and slowly dripped into the dechlorination reaction kettle 1 a...

Embodiment 2

[0053] use figure 2 Product A in Example 1 is processed by the reactive distillation column in the arrangement shown. The reactive distillation column uses high-purity nitrogen to purge the moisture content in the nitrogen to the outlet below 1ppm.

[0054] The arrangement of the reactive distillation column from top to bottom is the reaction section 5, the first packing section 6, and the second packing section 6. The height of the first joint packing section 6 is 4 meters, the height of the second joint packing section 6 is 2 meters, and the height of the reaction section 5 is 0.5 meters. The extraction point of the side line is located between the first packing section 6 and the second packing section 6 . The tower still of the reactive distillation tower is connected with the dechlorination reactor 1 through a gas phase pipeline and a liquid phase pipeline. The liquid phase pipeline is provided with an overflow device, and the liquid phase descending from the bottom of...

Embodiment 3

[0057] use image 3 The reactive distillation column in the arrangement shown in the figure processes the product A in Example 1. The top-to-bottom arrangement of the reactive distillation column is the first packing section 6, the second packing section 6, the reaction section 5, and the third section Packing section 6. The height of the first packing section 6 is 3 meters, the height of the second packing section 6 is 1 meter, the height of the third packing section 6 is 2 meters, and the height of the reaction section 5 is 0.5 meters.

[0058] The operating pressure of the reactive distillation column is 160kPaA. At this time, the temperature of the reaction section 5 is 20°C, the temperature of the first packing section 6 is 16°C, the temperature of the second packing section 6 is 18°C, and the temperature of the third packing section The temperature of 6 is 80°C. Others are the same as embodiment 2. The obtained hexafluorobutadiene product was named product 3.

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Abstract

The invention relates to a preparation method of hexafluorobutadiene, which comprises the following steps: respectively dehydrating a 3, 4-dichlorohexafluoro-1-butene raw material and an organic solvent, adding the dehydrated 3, 4-dichlorohexafluoro-1-butene raw material and the dehydrated organic solvent into a dechlorination reaction kettle together with zinc powder, carrying out a dechlorination reaction to obtain a dechlorination product, and carrying out rectification and catalytic conversion on the dechlorination product to obtain a hexafluorobutadiene product. Compared with the prior art, the method has the advantages that the by-product is rearranged into hexafluorobutadiene by using a catalyst, and rectification purification is combined, so that the purity of the obtained hexafluorobutadiene product is high, the content of impurities such as hexafluoro-2-butyne and hexafluorocyclobutene in the hexafluorobutadiene product is remarkably reduced, the difficulty of downstream production of high-purity hexafluorobutadiene can be reduced, and the purity requirement on 3, 4-dichlorohexafluoro-1-butene raw material is reduced from 99.95% to 99%, the requirement on the purity of the 3, 4-dichlorohexafluoro-1-butene raw material is reduced, the pressure of upstream production and investment is greatly reduced, and the height of a rectifying tower for producing the 3, 4-dichlorohexafluoro-1-butene can be greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of hexafluorobutadiene preparation, and relates to a preparation method of hexafluorobutadiene using 3,4-dichlorohexafluoro-1-butene as a raw material. Background technique [0002] The electronic information industry is an important driving force for social and economic development in today's world, and the integrated circuit is the core of the electronic information industry. my country's integrated circuit related industries are developing rapidly, the scale is getting bigger and bigger, and the industrial technology innovation ability has also been significantly improved. In terms of pure electronic products, there is still a big gap with developed countries. [0003] Hexafluoro-1,3-butadiene (C 4 f 6 , referred to as hexafluorobutadiene) is a perfluorinated compound with a boiling point of about 6°C at atmospheric pressure, which was first used in the synthesis of fluorine-containing polymer compounds....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/23C07C17/383C07C21/20
CPCC07C17/23C07C17/383C07C21/20Y02P20/10
Inventor 李瑜哲吴高胜许保云艾波包春凤翟金国王世忠刘陈真
Owner SHANGHAI RES INST OF CHEM IND
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