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Preparation method of 2-chloro-1, 1, 1, 2-tetrafluoropropane and 2, 3, 3, 3-tetrafluoropropene

A technology of tetrafluoropropane and tetrafluoropropene, applied in chemical instruments and methods, preparation of halogenated hydrocarbons, preparation of halogen substitution, etc., can solve problems such as harsh reaction conditions, difficulty in control, and rising costs, and achieve simple and direct process routes, Efficient and low-cost manufacturing, the effect of high industrial production costs

Pending Publication Date: 2021-05-11
ZHEJIANG HUANXIN FLUORO MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Although there are many methods for preparing 2-chloro-1,1,1,2-tetrafluoropropane (HCFC-244bb) disclosed at present, there are some problems such as harsh reaction conditions, difficult control, unfriendly catalysts to the environment, intermediate reactions The energy consumption and cost increase caused by the difficult separation of the body and the low selectivity of the target product are insufficient. Therefore, there is continuous improvement and demand for more effective preparation methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Preparation of 2-chloro-1,1,1,2-tetrafluoropropane:

[0043] Inject 2,3-dichloro-1,1,1-trifluoropropane and HF (containing tin tetrachloride 0.1‰) in a molar ratio of 1:22 into a cylindrical Hastelloy through two injection ports In the nickel-based alloy mixer, the mixed material enters the helical tube gasifier (inner diameter 25mm, Inconel625) in the way of upper and lower outlets. The temperature of the material at the outlet of the gasifier is controlled at 150°C. The material enters the fixed bed reactor continuously, the inner diameter of the reaction tube is 38mm, and 800ml of the supported catalyst mixed with chromium base is loaded. The temperature of the reactor is 350°C, the reaction pressure is 0.8Mpa, and the reaction contact time is 20s. After the stream was washed with water, it was detected and analyzed by gas chromatography. 243db was 25.117%, 1233xf was 12.078%, 244bb was 60.341%, 1234yf was 1.011% and other unknown organic substances were 1.453%.

Embodiment 2

[0045] Preparation of 2-chloro-1,1,1,2-tetrafluoropropane:

[0046] The operation is basically the same as in Example 1, except that the stream leaving the reactor is condensed and liquefied into the phase separator, the upper layer of the phase separator is rich in HF layer and returns to the mixer through the metering pump to re-enter the reactor for recycling, and the lower layer for the organic layer. The organic layer is transported to the crude fractionation tower by a metering pump for fractionation and purification. The high boiling point is 243db, and it returns to the mixer and re-enters the reactor for recycling. The components collected from the top of the tower go through a photochlorination reactor (Φ12×300) to remove unsaturated hydrocarbon compounds. , The stream that removes unsaturated hydrocarbons enters the rectification column for purification to obtain more than 99.5% of 244bb.

Embodiment 3

[0048] Preparation of 2-chloro-1,1,1,2-tetrafluoropropane:

[0049] Inject 2,3-dichloro-1,1,1-trifluoropropane to HF (containing antimony pentachloride 0.1‰) in a molar ratio of 1:22 into a cylindrical Hastelloy corrosion-resistant In the nickel-based alloy mixer, the mixed material enters the spiral tube gasifier (inner diameter is 25mm, Inconel625) in the way of upper and lower outlets. The temperature of the material at the outlet of the gasifier is controlled at 180°C. The material enters the fixed bed reactor continuously, the inner diameter of the reaction tube is 38mm, and it carries 800ml of supported catalyst mixed with chromium base as the carrier. The temperature of the reactor is 350°C, the reaction pressure is 0.8Mpa, and the reaction contact time is 20s. After washing with water, it was detected and analyzed by gas chromatography, 243db was 10.334%, 1233xf was 10.556%, 244bb was 75.365%, 1234yf was 1.778% and other unknown organic substances were 1.967%.

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Abstract

The invention relates to the technical field of halogenated hydrocarbon, in particular to a preparation method of 2-chloro-1, 1, 1, 2-tetrafluoropropane and 2, 3, 3, 3-tetrafluoropropene. The method comprises the following steps of: mixing 2, 3-dichloro-1, 1, 1-trifluoropropane and a fluorinating agent, feeding the mixed material into a gasifier, performing gasifying in the gasifier, conducting heating to 150-180DEG C, feeding the material into a fixed bed reactor loaded with a fluorinating catalyst, and carrying out continuous reaction to obtain a 2-chloro-1, 1, 1, 2-tetrafluoropropane product. And dehydrochlorination is carried out on the 2-chloro-1, 1, 1, 2-tetrafluoropropane, so that the 2, 3, 3, 3-tetrafluoropropene can be prepared. The method has the characteristics of continuous and stable reaction process, easy control, high efficiency and low cost.

Description

technical field [0001] The invention relates to the technical field of halogenated hydrocarbons, especially the field of preparation of alkanes and alkenes with three carbon atoms substituted by polyfluorine. Background technique [0002] Chlorofluorocarbons (HFCs) have extremely high global warming potential (GWP), are the most concerned greenhouse gases in the Kyoto Protocol, and are one of the main hidden dangers of global warming in the future. Automobile air-conditioning system is the most important industry for HFCs emissions, accounting for 65% of the total HFCs emissions. 1,1,1,2-Tetrafluoroethane (HFC-134a) is widely used as a refrigerant in automotive air conditioners. Because of its GWP of 1430, it has become the first HFCs to be phased out. The European Union has banned the use of HFC-134a in newly produced air conditioners since January 1, 2011, and will completely ban HFC-134a on January 1, 2017. The United States has also phased out HFC-134a since 2012. 2,3,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/20C07C19/10C07C17/25C07C21/18
CPCC07C17/206C07C17/25
Inventor 方海滔应永安吕洁吴志筐杨新华王志强陈伟
Owner ZHEJIANG HUANXIN FLUORO MATERIAL
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