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Preparation method of perfluoropropane

A technology of octafluoropropane and hexafluoropropene, which is applied in the field of preparation of octafluoropropane, which can solve the problems of equipment corrosion, increase equipment cost, and high equipment material requirements, and achieve the effects of reducing the severity, reducing material requirements, and inhibiting cracking

Inactive Publication Date: 2014-01-08
FOSHAN HUATE GASES +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, in the above method, tetrafluoromethane (CF 4 ) and hexafluoroethane (C 2 f 6 ), and addition yields C 4 f 8 and C 6 f 12 , and cycloaddition produces by-products such as 4 rings. At the same time, the fluorinating agent (advanced metal fluoride) is not treated in depth, which reduces the selectivity of the target product and the yield of octafluoropropane
In addition, some compounds in the impurities are difficult to separate by rectification, so it is almost impossible to obtain high-purity octafluoropropane
In particular, in the implementation process of the above method, the feasibility of the method is demonstrated experimentally, and the industrial production process is not mentioned.
Moreover, these methods are carried out at relatively high temperatures, and the diluent hydrogen fluoride (HF) added to the reactants during the reaction is very corrosive to the equipment. Therefore, the requirements for the material of the equipment are also very high, which aggravates the industrialization of this product. The cost of equipment seriously restricts the industrial production of octafluoropropane

Method used

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preparation example Construction

[0020] figure 1 It is a flowchart of the preparation method of octafluoropropane of the present invention.

[0021] Such as figure 1 As shown, the steps of the preparation method of octafluoropropane include in turn: electrolysis, dust removal, condensation, adsorption; mixing; reaction of mixed gas with cobalt difluoride; purging, vacuuming inert gas replacement; Cobalt reaction; cooling, adsorption; rectification.

[0022] Combine below figure 1 Specifically introduce the detailed steps of the preparation method of octafluoropropane:

[0023] S101. Potassium bifluoride is electrolytically treated in an electrolytic cell to obtain a fluorine gas mixture, and the fluorine gas mixture is sequentially subjected to dedusting, condensation, and adsorption treatments to purify the fluorine gas mixture as a raw material.

[0024] Electrolytic reaction formula: 2KHF 2 →2KF+H 2 +F 2

[0025] What needs to be explained here is that potassium bifluoride is electrolytically treat...

Embodiment 1

[0053] The reactor is a fixed bed reactor with internal heating and 8 temperature control points. In the mixed gas, the concentration of fluorine gas is 20%, and its production method is as follows:

[0054] A. Turn on the electrolytic cell, control the pressure of the electrolytic cell to a slight negative pressure, and obtain a fluorine gas mixture after electrolytic treatment of potassium bifluoride in the electrolytic cell, and then process the fluorine gas mixture in turn through dust removal, condensation, and adsorption treatments to purify it into fluorine gas as a raw material .

[0055] B. After the raw material fluorine gas is pressurized by a compressor, it is uniformly mixed with an inert gas to obtain a mixed gas, and the concentration of fluorine gas in the mixed gas is 20%.

[0056] C. Raise the temperature of the reactor to 300°C in advance, with 12.5Nm 3 The mixed gas is passed into the reactor at a flow rate of / h, and the pressure in the reactor is contro...

Embodiment 2

[0062] In this embodiment, the concentration of fluorine in the mixed gas is 40%, and the rest are the same as the method of Embodiment 1.

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Abstract

The invention discloses a preparation method of perfluoropropane. The preparation method sequentially comprises the following steps: (1) electrolyzing potassium bifluoride to obtain a mixed fluorine gas, and sequentially carrying out dust extraction, condensation and adsorption treatments on the mixed fluorine gas to purify the mixed fluorine gas to raw material fluoride; (2) pressurizing the raw material fluoride and uniformly mixing the raw material fluoride with an inert gas to obtain a mixed gas; (3) introducing the mixed gas into a reactor filled with cobaltous fluoride to react to obtain cobaltic oxide; (4) carrying out purging and vacuumizing replacement treatments on the reactor and related pipelines and pipe fittings after the reaction; (5) introducing hexafluoropropylene into the reactor to react with the cobaltic oxide to obtain perfluoropropane containing impurities; (6) cooling and adsorbing the perfluoropropane; and (7) introducing the perfluoropropane into a rectifying column through a compressor to be rectified. By adopting the preparation method disclosed by the invention, the corrosion of impurities on the reactor can be reduced, such unfavorable side reactions as hexafluoropropylene pyrolysis, self polymerization, addition, and the like, are inhibited, and perfluoropropane with high purity is prepared.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of octafluoropropane. Background technique [0002] Octafluoropropane is often used as an etching or cleaning gas in the process of preparing semiconductor devices. There are multiple methods for the direct preparation of octafluoropropane using hexafluoropropylene as a raw material: [0003] Japanese patent JP-B-62-61572 pointed out that a direct fluorination reaction between hexafluoropropylene and fluorine gas was used to prepare octafluoropropane; Japanese patent JP-B-1-45455 pointed out that in the presence of a catalyst, hexafluoropropylene React with fluorine to prepare octafluoropropane; Japanese patent JP-B-62-54777 pointed out that hexafluoropropylene was reacted with high-order metal fluorides to prepare octafluoropropane; Japanese patent JP-B-62-61682 pointed out that, In the case of dilution with inert gas and reaction product gas, react hexafl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/08C07C17/04C07C17/383
Inventor 唐忠福马建修陈艳珊
Owner FOSHAN HUATE GASES
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