Separation method of high-boiling matter in 1-chloro-1,1-difluoroethane production process

A difluoroethane, production process technology, applied in the field of separation, can solve the waste of fluorine resources and other problems, achieve the effect of improving economic benefits and promoting further development

Active Publication Date: 2017-08-18
SHANDONG DONGYUE CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the deficiencies in the prior art, the object of the present invention is to provide a method for separating high boilers of a 1-chloro-1,1-difluoroethane production process, from 1-chloro-1,1-difluoroethane (R142b) Separation of difluorodichloroethane and difluorotrichloroethane from high boilers in the production process to solve the problem of waste of fluorine resources and make a positive contribution to the protection of the environment

Method used

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  • Separation method of high-boiling matter in 1-chloro-1,1-difluoroethane production process

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] The high boilers in the 1-chloro-1,1-difluoroethane (R142b) production process enter the degasser 2 tons of material from the high boilers storage tank through the material delivery pump 1#, and the fluctuation range of the control degasser operating parameters is : The temperature of the tower kettle is 55-60℃, the pressure of the tower kettle is 0.10-0.20MPa, the temperature of the tower top is 10-18℃, and the pressure of the tower top is 0.05-0.15MPa.

[0052] Gas chromatography was used to analyze and detect the samples at the top and bottom of the degassing tower. According to the sampling analysis results, when the components of the degassing tower are balanced, the light component 1-chloro-1,1-difluoroethane (R142b) in the high boilers is intermittently recovered from the top of the tower; When there is no 1-chloro-1,1-difluoroethane (R142b), feed to rectification column 1# through material delivery pump 2#.

[0053] Control the fluctuation range of operation pa...

Embodiment 2

[0059] The whole process is controlled by a continuous operation mode, and the fluctuation range of the operation parameters of the degassing tower is controlled: the temperature of the tower bottom is 60-70 ° C, the pressure of the bottom of the tower is 0.20-0.30 MPa, the temperature of the top of the tower is 18-27 ° C, and the pressure of the top of the tower is 0.15-0.25 MPa The operating parameters of rectification tower 1# fluctuate in the range of: tower kettle temperature 95-108°C, tower kettle pressure 0.15-0.20MPa, tower top temperature 65-78°C, tower top pressure 0.10-0.15MPa; rectification tower 2# The fluctuation range of the operating parameters is: the temperature of the tower bottom is 120-128°C, the pressure of the tower bottom is 0.15-0.20MPa, the temperature of the top of the tower is 95-103°C, and the pressure of the top of the tower is 0.10-0.15MPa.

[0060] The purity of recovered stream 3 is: 95.78wt% 1-chloro-1,1-difluoroethane (R142b), 4.22wt% difluoro...

Embodiment 3

[0062] The whole process is controlled by a continuous operation mode, and the fluctuation range of the operating parameters of the degassing tower is controlled: the temperature of the tower bottom is 70-80 ° C, the pressure of the bottom of the tower is 0.30-0.40 MPa, the temperature of the top of the tower is 25-40 ° C, and the pressure of the top of the tower is 0.25-0.35 MPa ; The fluctuation range of operating parameters of rectification tower 1# is: tower kettle temperature 110-120°C, tower kettle pressure 0.20-0.25MPa, tower top temperature 78-85°C, tower top pressure 0.15-0.20MPa; rectification tower 2# The fluctuation range of operating parameters is: the temperature of the tower bottom is 128-135°C, the pressure of the tower bottom is 0.20-0.25MPa, the temperature of the top of the tower is 103-110°C, and the pressure of the top of the tower is 0.15-0.20MPa.

[0063] The purity of recovered stream 3 is: 94.39wt% 1-chloro-1,1-difluoroethane (R142b), 5.61wt% difluorodi...

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Abstract

The invention relates to a separation method, in particular to a separation method of a high-boiling matter in a 1-chloro-1,1-difluoroethane production process. The separation method comprises the following steps: performing pretreatment on the high-boiling matter in the 1-chloro-1,1-difluoroethane production process in a degassing tower and recovering a light component, namely 1-chloro-1,1-difluoroethane in the high-boiling matter from the top of the tower; enabling a heavy component in a tower kettle of the degassing tower to enter a rectifying tower 1# and rectifying out a finished product, namely difluoro dichloroethane through a condenser at the tower top of the rectifying tower 1#; enabling a heavy component in a tower kettle of the rectifying tower 1# to enter a rectifying tower 2# and rectifying out a finished product, namely difluoro trichloroethane through a condenser at the tower top of the rectifying tower 2#. The high-boiling matter mainly comprises the following components: 1-chloro-1,1-difluoroethane, difluoro dichloroethane, difluoro trichloroethane and isomers thereof. The separation method provided by the invention has the benefits that difluoro dichloroethane and difluoro trichloroethane are separated from the high-boiling matter in the 1-chloro-1,1-difluoroethane production process, the problem of fluorine resource waste is solved, the cost is reduced, the economic benefits are improved, and a positive contribution is made to environmental protection.

Description

technical field [0001] The invention relates to a separation method, in particular to a separation method of high boilers in a 1-chloro-1,1-difluoroethane production process. Background technique [0002] 1-Chloro-1,1-difluoroethane (R142b) is a commonly used high-temperature refrigerant, polymer (plastic) foaming agent, thermostatic control switch and intermediate of aviation propellant, and can also be used For the production of polyvinylidene fluoride. In recent years, with the rapid development of the domestic PVDF industry, the production capacity of 1-chloro-1,1-difluoroethane (R142b) in various enterprises has been expanding day by day. [0003] In the process of producing 1-chloro-1,1-difluoroethane (R142b) by dry photochlorination of 1,1-difluoroethane (R152a) and chlorine gas reported in CN 101781164 A, about 4- 7wt% high boiler {which mainly contains entrained 3-5wt% 1-chloro-1,1-difluoroethane (R142b), 30-40wt% difluorodichloroethane, 10-20wt% Difluorotrichlor...

Claims

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Application Information

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IPC IPC(8): C07C17/383C07C19/12
CPCC07C17/383C07C19/12
Inventor 游康丽史阿莹唐存国刘敬宋淑伟曾照民
Owner SHANDONG DONGYUE CHEM
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