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Synthesis method of 1, 1, 1-trichloroethane

A technology of trifluoroethane and difluoroethane, which is applied in the field of synthesizing 1,1,1-trifluoroethane, which can solve the problems of failure to meet the requirements of anti-corrosion or low-corrosion use, reliability and safety hazards, etc.

Inactive Publication Date: 2018-05-18
东阳市巍华制冷材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] It is well known that in the liquid phase catalyst Sbcl 5 In the presence of organic substances such as chloroalkanes, chlorofluoroalkanes, chlorofluoroalkenes or chloroalkenes, and hydrogen fluoride to prepare various CFC, HCFC or HFC compounds, there is Sbcl 5 The catalyst system is highly corrosive to the reactor material, especially when there is liquid-phase hydrogen fluoride under the reaction conditions, the fluorination reactor corrodes faster, even if the reactor material is Hastelloy, inconel, Monel, NAR-25-50MTi, etc. The alloy material of nickel cannot meet the requirements of anti-corrosion or low-corrosion use, which poses a major hidden danger to the reliability and safety of the pressurized fluorination reaction

Method used

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  • Synthesis method of 1, 1, 1-trichloroethane

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Effect test

Embodiment 1

[0027] Sncl 4 As a catalyst to synthesize 1,1,1-trifluoroethane. The implementation process is as follows: add the Monel and Q345R steel of the pre-cleaned and dried scraper test sample to the bottom of the fluorination reactor 1, and after the fluorination reactor 1 is sealed, add 0.55kg of hydrogen fluoride and 2kg of Sncl 4Sequentially add to 15 liters of fluorination reactor 1 made of RQ345R steel, heat fluorination reactor 1 with water vapor, and make its internal temperature rise to 85 ° C, at this time, a certain amount of hydrogen chloride gas is produced by the catalyst activation reaction, from It is released from the discharge port, and then emptied after washing with water and alkali. The hydrogen chloride gas in the fluorination reactor 1 was exhausted, and the temperature was lowered to 50° C. with cooling water to obtain an active catalyst. Control the internal temperature of fluorination reactor 1 at 50°C, and add HCFC-142b at 1.6kg / hr and hydrogen fluoride a...

Embodiment 2

[0029] The present embodiment adopts the same operating method as in Example 1, and the catalyst and reaction conditions during the operation are listed below.

[0030] Add 2kg fluorosulfonic acid FS0 3 H as a catalyst. The results of this example are: the content of HFC-143a in the reaction product is 53.2%, the unreacted HCFC-142b is 46.8%, no high boiler tar and other by-products are detected, the annual corrosion rate of Monel alloy is 0.01mm, and the Q345R steel The annual corrosion rate is 0.1mm.

Embodiment 3

[0032] The present embodiment adopts the same operating method as in Example 1, and the addition and product conditions during the operation are listed below.

[0033] Add 1.5kgSncl 4 And 0.5kg fluorosulfonic acid as catalyst. The results of this example are: the content of HFC-143a in the reaction product is 99.8%, the unreacted HCFC-142b is 0.2%, no high boiler tar and other by-products are detected, the annual corrosion rate of Monel alloy is 0.01mm, and 16MnR is ordinary The annual corrosion rate of carbon steel is 0.15mm.

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Abstract

The invention discloses a synthesis method of 1, 1, 1-trichloroethane and belongs to the technical field of chemical synthesis. The synthesis method includes following steps: using 1-chloro-1, 1-difluoroethane and hydrogen fluoride as raw materials for liquid-phase fluoridation, wherein a liquid-phase fluoridation catalyst is one of or a mixture of tetravalent tin compound and halogenosulfonic acid. Before feeding, a mixture of a liquid-phase catalyst and hydrogen fluoride is heated to obtain an active catalyst; a fluoridation separation process is adopted, so that side reaction can be controlled effectively, reaction conditions are mild, conversion rate and selectivity are high, the conversion rate reaches higher than 99.6%, and the selectivity reaches 99.9%. A liquid-phase fluoridation catalyst system is adopted, so that corrosion speed of a reactor material can be controlled effectively, service life is long, and operation is safe and reliable.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a method for synthesizing 1,1,1-trifluoroethane. Background technique [0002] 1-Chloro-1,1-difluoroethane (HCFC-142b for short) is a transitional CFC substitute, ODP is not zero, and has a destructive effect on atmospheric ozone. Internationally, HCFC-142b and other HCFC substances have been regarded as final banned chemicals. The Chinese government has also stipulated that starting from January 1, 2009, the approval of new construction and expansion projects of HCFC transitional CFC substitutes will be stopped. In the process of producing HCFC-141b and HFC-143a with vinylidene chloride or methyl chloroform as raw materials, a certain amount of HCFC-142b will always be produced, and the HCFC-142b produced in the production process or replaced from refrigeration equipment , converted into 1,1,1-trifluoroethane (HFC-143a for short) with zero ODP and reducing the impact...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/08C07C17/20
CPCC07C17/206C07C19/08
Inventor 潘敏楼晓权单利锋俞慧
Owner 东阳市巍华制冷材料有限公司
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