Method for preparing ultra-high purity difluoromono-chloroethane

A difluoro-monochloroethane, ultra-high-purity technology, applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, halogenated hydrocarbon disproportionation separation/purification, etc., can solve the problem of incomplete absorption of HCl and chlorine gas and incomplete reaction of raw materials , the problem of low product purity, to achieve the effect of inhibiting the formation of by-products, saving raw materials, and high reaction temperature

Inactive Publication Date: 2013-04-03
TAIXING MEILAN CHEM
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  • Abstract
  • Description
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Problems solved by technology

[0004] At present, the preparation method of difluorochloroethane in China is mainly the photochlorination method to prepare difluorochloroethane. Due to the constraints of production equipment and other factors, the prepared The difluorochloroethane can only meet the requirements of high-grade products, and the production cost is high, the pollution is heavy, and it cannot meet the requirements of most manufacturers today.
For example, Chinese patent 201010108206.8 discloses a method for the preparation of difluorochloroethane, the method is through raw material gasification preheating, photochlorination reaction, compression, multi-stage delight separation, liquid phase water washing, liquid phase neutralization, refining Difluorochloroethane with a purity ≥ 99.9% is obtained by distilling and drying, which has the disadvantages of incomplete reaction of raw materials, incomplete absorption of HCl and chlorine, and low product purity; Chinese patent 200410015778.6 discloses a preparation of difluorochloroethane The method is to obtain difluorochloroethane with a purity ≥ 99.9% by mixing raw materials, reacting in a photochemical reactor, reacting in a secondary reactor, and separating and processing, but there are complicated operation techniques, waste of raw materials, large energy consumption, and heavy pollution. , low product purity and high cost

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  • Method for preparing ultra-high purity difluoromono-chloroethane

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Embodiment 1

[0045] The present invention prepares the method for ultrahigh-purity difluoro-chloroethane comprising the following steps:

[0046] (1) Reaction: After the raw materials difluoroethane and liquid chlorine are gasified, they are mixed at a molar ratio of 1.15:1, and then enter the photochlorination reactor 1 for photochlorination reaction. The reaction temperature is 40°C, the reaction pressure is 0.05MPa, and the reaction residence time is 60S, the feeding amount of difluoroethane for a single photochlorination reactor is 100-150Kg / h;

[0047] (2) Water washing: The gas reacted in the photochlorination reactor absorbs hydrogen chloride through the two-stage water absorption HCl tower 2, and the working pressure in the tower is 1.5MPa, the temperature in the tower is 40°C, and the absorbed HCl is dissolved in water Converted into hydrochloric acid with a concentration of 25-30%;

[0048] (3) Alkali washing: the gas after removing HCl is removed through the two-stage alkali li...

Embodiment 2

[0054] The present invention prepares the method for ultrahigh-purity difluoro-chloroethane comprising the following steps:

[0055] (1) Reaction: After the raw materials difluoroethane and liquid chlorine are vaporized, they are mixed at a molar ratio of 1.15:1, and enter the photochlorination reactor 1 for photochlorination reaction. The reaction temperature is 80°C, the reaction pressure is 0.1MPa, and the reaction residence time is 90S, the feed rate of difluoroethane for a single photochlorination reactor is 100-150Kg / h;

[0056] (2) Water washing: The gas reacted in the photochlorination reactor absorbs hydrogen chloride through the two-stage water absorption HCl tower 2, and the working pressure in the tower is 2.0MPa, the temperature in the tower is 80°C, and the absorbed HCl is dissolved in water Converted into hydrochloric acid with a concentration of 25-30%;

[0057] (3) Alkali washing: the gas after removing HCl is removed through the two-stage alkali liquid absor...

Embodiment 3

[0063] The present invention prepares the method for ultrahigh-purity difluoro-chloroethane comprising the following steps:

[0064] (1) Reaction: After the raw materials difluoroethane and liquid chlorine are vaporized, they are mixed at a molar ratio of 1.15:1, and then enter the photochlorination reactor 1 for photochlorination reaction. The reaction temperature is 60°C, the reaction pressure is 0.07MPa, and the reaction residence time is 70S, the feed rate of difluoroethane for a single photochlorination reactor is 100-150Kg / h;

[0065] (2) Water washing: The gas reacted in the photochlorination reactor absorbs hydrogen chloride through the two-stage water absorption HCl tower 2, and the working pressure in the tower is 1.7MPa, the temperature in the tower is 60°C, and the absorbed HCl is dissolved in water Converted into hydrochloric acid with a concentration of 25-30%;

[0066] (3) Alkali washing: the gas after removing HCl is removed through the two-stage alkali liquid...

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Abstract

The invention provides a method for preparing ultra-high purity difluoromono-chloroethane, which comprises the following steps: mixing raw materials at a mole ratio of 1.15:1 and feeding the mixture into a photochlorination reactor for reaction, feeding the reactant into a two-stage water absorption HCL tower and a two-stage alkali liquor absorption chlorine gas tower to remove HCL and chlorine; feeding the obtained product into a dry buffer tank; compressing the gas from the dry buffer tank with a single-stage oil-free compressor and feeding the compressed gas into a degassing tower and a rectifying tower for degassing and rectifying to obtain difluoromono-chloroethane with moisture; and then removing the moisture with a molecular sieve drier to obtain a pure difluoromono-chloroethane product. According to the method, the production flow of the difluoromono-chloroethane is shortened, the reaction conversion rate is high, the by-products are few, the rectifying efficiency is high, the raw materials and the energy consumption are reduced, the purity of the product is high and the production of the whole set of device is safe and economic.

Description

technical field [0001] The invention belongs to the field of fluorine chemical industry, and in particular relates to a method for preparing ultra-high-purity difluoro-chloroethane. technical background [0002] As the requirements of domestic and foreign manufacturers continue to increase, the original high-grade difluorochloroethane can no longer meet the market demand, especially for some small indicators that are extremely strict, and only high-purity difluorochloroethane can meet the requirements According to market requirements, the following table shows the comparison of difluorochloroethane quality indicators: [0003] [0004] At present, the preparation method of difluoro-chloroethane in China is mainly the preparation of difluoro-chloro-ethane by the photochlorination method. Due to the constraints of production equipment and other factors, the prepared difluoro-chloro-ethane can only meet the requirements of high-grade products. , and the production cost is h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/12C07C17/10C07C17/38
Inventor 全文德陈明张龙
Owner TAIXING MEILAN CHEM
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