Preparation method of 1, 3-dichloro-1, 1-difluoropropane

A technology of difluoropropane and tetrachloropropane, which is applied in the field of fluorine-containing chemicals, can solve the problem of low selectivity of difluoropropane, and achieve the effects of high selectivity, easy availability of raw materials, and high conversion rate

Active Publication Date: 2022-03-22
ZHEJIANG FLUORINE CHEM NEW MATERIAL
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006]Hasxeldine et al reported that using benzene trifluoride as a solvent, 1,1,1,3-tetrachloropropane and antimony trifluoride and trifluoroantimony dichloride (molar ratio 1:1.36:0.97) reaction, the products are mainly 1,3-dichloro-1,1-difluoropropane (10%) and 3-chloro-1,1,1-trifluoropropane (61% ), the selectivity of the product 1,3-dichloro-1,1-difluoropropane is low

Method used

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  • Preparation method of 1, 3-dichloro-1, 1-difluoropropane

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Add 5.4g of niobium pentachloride, 35.6g of antimony trifluoride, 30ml of 1-chloroethane and 52g of 1,1,1,3-tetrachloropropane into a 300mL stainless steel belt stirred autoclave, and start stirring. After the temperature was raised to 40°C, the reaction was carried out for 8 hours. After the reaction, the sample was washed with water, filtered, and deacidified, and then analyzed by gas chromatography. The conversion rate of 1,1,1,3-tetrachloropropane was 99.6%. 1,3-Dichloro- The selectivity to 1,1-difluoropropane was 93.3%.

Embodiment 2～7

[0022] Examples 2-7 Prepare 1,3-dichloro-1,1-difluoropropane according to the same method as in Example 1, the difference is that the catalyst, solvent and , reaction temperature and reaction time, reaction result is as shown in table 1.

[0023] Table 1

[0024]

[0025] Table 1 shows that the polarity of the solvent can affect the solubility and acidity of the catalyst and substrate, which in turn affects the selectivity of the target product.

Embodiment 8～12

[0027] Examples 8-12 Prepare 1,3-dichloro-1,1-difluoropropane according to the same method as in Example 1, except that antimony trifluoride and 1,1,1,3-tetrachloropropane The molar ratio, the molar ratio of the catalyst to 1,1,1,3-tetrachloropropane, and the reaction results are shown in Table 2.

[0028] Table 2

[0029]

[0030] Table 2 shows that the conversion rate of raw material 1,1,1,3-tetrachloropropane is all above 99.0% within the range of above-mentioned experimental conditions, and can effectively improve target product 1,3-dichloropropane along with the increase of fluorination reagent consumption - The selectivity of 1,1-difluoropropane, when the molar ratio of the catalyst, antimony trifluoride and 1,1,1,3-tetrachloropropane is 0.05:0.8:1, the reaction selectivity is better, as 93.1%.

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Abstract

The invention discloses a preparation method of 1, 3-dichloro-1, 1-difluoropropane, and belongs to the technical field of fluorine-containing chemicals. Under the action of a lewis acid catalyst, in the presence or absence of a solvent, 1, 1, 1, 3-tetrachloropropane reacts with antimony trifluoride to generate 1, 3-dichloro-1, 1-difluoropropane, and the lewis acid catalyst is niobium pentachloride, tantalum pentachloride or antimony pentachloride. According to the preparation method of the 1, 3-dichloro-1, 1-difluoropropane, the raw materials are easy to obtain, the conversion rate is high, the 1, 3-dichloro-1, 1-difluoropropane can be prepared with high selectivity, and the selectivity can reach 90% under better conditions.

Description

technical field [0001] The invention belongs to the technical field of fluorine-containing chemicals, in particular to a preparation method of 1,3-dichloro-1,1-difluoropropane. Background technique [0002] 1,3-dichloro-1,1-difluoropropane is a fluorine-containing chemical, which can be used as an intermediate of new refrigerants or blowing agents, and the research on its preparation method is of great value. [0003] Henne et al reported the synthesis of 1,3-dichloro-1,1-difluoropropane (55%) and 3- The method of chloro-1,1,1-trifluoropropane (45%), the raw material trifluoropropene of this method is relatively expensive, and the product selectivity is not high. [0004] McBee et al. reported a method of photochlorination of 1-chloro-1,1-difluoropropane at a temperature of 70-80°C, and the product is mainly 1,3-dichloro-1,1-difluoropropane (58%) , 1,2-dichloro-1,1-difluoropropane (33%) and 1,3,3-trichloro-1,1-difluoropropane (9%); in this method, the raw materials are not...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/20C07C19/10
CPCC07C17/208C07C19/10
Inventor 苗国祥李晓寿江晟孙培锋
Owner ZHEJIANG FLUORINE CHEM NEW MATERIAL
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