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Preparation method of 1,1,1,3,3-pentachloro-4,4,4-trifluorobutane

A technology for trifluorobutane and trifluoropropene, which is applied in the field of preparation of hydrofluorochloroalkanes, can solve the problems of large amount of metal, waste, loss of trifluoropropene, etc., and achieves high industrial application prospects and the effect of improving catalytic efficiency

Inactive Publication Date: 2019-10-25
XIAN MODERN CHEM RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The telomerization reaction of 2-chloro-3,3,3-trifluoropropene and carbon tetrachloride is a key step in the synthesis of a new blowing agent HFO-1336. Patent CN102884030B reports a 2-chloro-3,3,3 - The telomerization method of trifluoropropene and carbon tetrachloride, the amount of metal used is 1.5wt% to 2.5wt%, the amount of metal used is relatively large, and the telomerization method of carbon tetrachloride and 2-chloro-3,3,3-trifluoropropene Polymerization ratio is 50:50mol%. In fact, under this high concentration condition, 2-chloro-3,3,3-trifluoropropene cannot be completely dissolved in carbon tetrachloride, resulting in 2-chloro-3,3,3 - Loss and waste of trifluoropropene

Method used

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  • Preparation method of 1,1,1,3,3-pentachloro-4,4,4-trifluorobutane
  • Preparation method of 1,1,1,3,3-pentachloro-4,4,4-trifluorobutane
  • Preparation method of 1,1,1,3,3-pentachloro-4,4,4-trifluorobutane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 2.14 grams of ferric chloride, 13.16 grams of tributyl phosphate and 50 grams of carbon tetrachloride solution in the 1.5L stainless steel belt stirred autoclave, add 4.39 grams of iron powder and 450 grams of carbon tetrachloride at the solid feed port, pre- After 26 grams of 2-chloro-3,3,3-trifluoropropene was introduced, the temperature was raised to 115° C., and 2-chloro-3,3,3-trifluoropropene was continuously introduced into the gas phase until 2-chloro-3 , After the amount of 3,3-trifluoropropene feeding reaches 100 grams, stop feeding, continue to stir the reaction to a pressure of 0.3 MPa, cool down to stop the reaction, take a sample for GC analysis, and obtain the product after vacuum distillation.

[0018] The product is detected by NMR, and the data are as follows:

[0019] 1 H NMR (500MHz, CDCl 3 )δ3.72(s,2H);

[0020] 13 C NMR (500MHz, CDCl 3 )δ121.8(q, J=281.3Hz), 92.6, 79.7(q, J=34.8Hz), 59.1;

[0021] 19 F NMR (470MHz, CDCl 3 )δ-80.2(s, CF ...

Embodiment 2～6

[0024] Examples 2-6 Prepare 1,1,1,3,3-pentachloro-4,4,4-trifluorobutane according to the same preparation method in Example 1, the difference is that the reaction four in Example 1 The ratio of chlorinated carbon: 2-chloro-3,3,3-trifluoropropene is 2.5:1, while the telomerization ratios in Examples 2-6 are 1:1, 2:1, 5:1, 7:1 respectively , 10:1. The reaction results of Examples 2-6 are shown in Table 1.

[0025] Table 1 Screening of telomerization ratio

[0026] Example The molar ratio of Conversion rate(%) selectivity (%) 2 1:1 90.5 84.1 3 2:1 93.3 96.1 4 5:1 94.5 95.0 5 7:1 95.6 94.3 6 10:1 96.8 96.2

Embodiment 7～10

[0028] Examples 7-10 Prepare 1,1,1,3,3-pentachloro-4,4,4-trifluorobutane according to the same preparation method in Example 1, the difference is the reaction catalyst in Example 1 It is ferric chloride, and it is respectively ferric bromide, ferrous chloride, ferric sulfate or ferric acetylacetonate among the embodiments 7-10. The reaction results of Examples 7-10 are shown in Table 2.

[0029] Table 2 Catalyst screening

[0030]

[0031]

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Abstract

The invention discloses a preparation method of 1,1,1,3,3-pentachloro-4,4,4-trifluorobutane. The preparation method comprises the steps: adopting 2-chloro-3,3,3-trifluoropropene and carbon tetrachloride as raw materials, and synthesizing 1,1,1,3,3-pentachloro-4,4,4-trifluorobutane in the presence of a telomerization catalyst, a catalytic assistant and a reducing agent. The invention provides a synthetic route with high telomerization reaction efficiency, and the preparation method is mainly applied to preparation of 1,1,1,3,3-pentachloro-4,4,4-trifluorobutane.

Description

technical field [0001] The invention relates to a preparation method of hydrofluorochloroalkane, in particular to a preparation method of 1,1,1,3,3-pentachloro-4,4,4-trifluorobutane. Background technique [0002] Due to the destruction of the ozone layer by the first and second generation blowing agents (fluorotrichloromethane CFC-11, fluorodichloroethane HCFC-141b, etc.), the use of the third generation blowing agents (1,1, 1,3,3-pentafluoropropane (HFC-245fa, etc.) will have a strong greenhouse effect. With the increasing impact of global warming on the earth's ecology, it is urgent to find green and environmentally friendly blowing agents. [0003] 1,1,1,4,4,4-hexafluoro-2-butene (HFO-1336) can quickly add to OH radicals after being discharged into the atmosphere due to the double bond contained in the molecule, and through oxidation For degradation, the atmosphere has a short lifetime (20 days) and a low greenhouse effect value (GWP≈9). Its boiling point is close to r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/278C07C19/10B01J27/128B01J31/22B01J31/24B01J27/053
CPCB01J27/053B01J27/128B01J31/1805B01J31/1815B01J31/1875B01J31/2404B01J2531/842C07C17/278C07C19/10
Inventor 吕剑赵波曾纪珺韩升杨志强唐晓博郝志军亢建平李凤仙张伟
Owner XIAN MODERN CHEM RES INST
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