Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

A kind of preparation method of 2,4,4-trichloro-1,1,1-trifluorobutane

A technology of trifluorobutane and trifluoroethane, which is applied in the field of preparation of hydrofluorochloroalkanes, can solve the problems of difficult availability and high price of trifluoropropene, and achieves the effects of high price and mature industrial production technology

Active Publication Date: 2016-08-17
XIAN MODERN CHEM RES INST
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of the above method is that the used raw material trifluoropropene is expensive and not easy to obtain

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of preparation method of 2,4,4-trichloro-1,1,1-trifluorobutane
  • A kind of preparation method of 2,4,4-trichloro-1,1,1-trifluorobutane
  • A kind of preparation method of 2,4,4-trichloro-1,1,1-trifluorobutane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 1.4 grams of copper chloride and 3.2 grams of 2,2-bipyridine to a 500 mL titanium alloy belt stirred autoclave, dissolve them in 20 mL of dimethyl sulfoxide, replace the air in the kettle with nitrogen, and inject 312 grams of R123 with nitrogen gas and 63 grams of vinyl chloride, the reaction temperature is 120°C, the reaction pressure is 1.2MPa, and the reaction time is 12 hours. After the reaction, the crude product is removed by atmospheric distillation to remove R123, R123 is recycled, and the vacuum distillation is continued to collect 2,4,4-trichloro- 1,1,1-Trifluorobutane, the conversion rate is 91.3%, and the selectivity is 87.6%.

[0017] Product structure characterization:

[0018] 1 H-NMR (500MHz, CDCl 3 ): δ2.66(m,1H), δ2.82(m,1H), δ4.37(m,1H), δ5.92(q,1H)

[0019] 13 C-NMR (500MHz, CDCl 3 ): δ44.52(s,1C), δ54.31(q,1C), δ68.53(s,1C), δ124.48(q,1C)

[0020] 19 F-NMR (500MHz, CDCl 3 ): δ-74.66(s,3F)

Embodiment 2～6

[0022] Examples 2-6 Prepare 2,4,4-trichloro-1,1,1-trifluorobutane according to the same preparation method as in Example 1, except that the reaction 2,2-difluorobutane in Example 1 Chlorine 1,1,1-trifluoroethane: vinyl chloride ratio is 2:1, while the telomerization ratios in Examples 2-6 are 1:1, 3:1, 5:1, 7:1, 10: 1. The reaction results of Examples 2-6 are shown in Table 1.

[0023] Table 1 Effect of telomerization ratio

[0024] Example

Embodiment 7～18

[0026] Examples 7-18 Prepare 2,4,4-trichloro-1,1,1-trifluorobutane according to the same preparation method as in Example 1, except that the reaction catalyst in Example 1 is copper chloride , and respectively ferric chloride, ferrous chloride, cupric chloride or cuprous chloride in the embodiment 7~18, the reaction can be carried out without adding solvent. The reaction results of Examples 7-18 are shown in Table 2.

[0027] Table 2 Catalyst and Catalytic Auxiliary Effect

[0028]

[0029]

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a preparation method of 2,4,4-trichloro-1,1,1-trifluorobutane. The 2,4,4-trichloro-1,1,1-trifluorobutane is synthesized from raw materials 2,2-dichloro-1,1,1-trifluoroethane and chloroethylene in the presence of a telomerization catalyst, a catalytic addictive and a solvent, wherein the telomerization catalyst is copper chloride or cuprous chloride; and the catalytic addictive is 2,2-dipyridyl, pentamethyldiethylenetriamine, tri(2-pyridylmethyl)amine or tri(2-dimethylaminoethyl)amine; the solvent is acetonitrile, methanol or dimethyl sulfoxide. The invention provides a new synthesis route which is cheap and easily available in raw materials, and the synthesis route is mainly used for preparing the 2,4,4-trichloro-1,1,1-trifluorobutane.

Description

technical field [0001] The invention relates to a preparation method of hydrofluorochloroalkane, in particular to a preparation method of 2,4,4-trichloro-1,1,1-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 room te...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C19/10C07C17/278
Inventor 赵波吕剑韩升唐晓博郝志军马辉曾纪珺毛伟张伟王博李凤仙
Owner XIAN MODERN CHEM RES INST
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com