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

Preparation method of 2-chloro-1,1,1,2-tetrafluoropropane

A technology of tetrafluoropropane and fluoropropene, which is applied in the field of 2-chloro-1, can solve the problems of difficult separation and high temperature of gas-phase fluorination reaction, and achieve the effect of saving energy and mild reaction conditions

Active Publication Date: 2012-07-25
山东华安近代环保科技有限公司
View PDF4 Cites 11 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following disadvantages: (1) the gas phase fluorination reaction temperature is high; (2) the boiling points of HCFC-1233xf and HCFC-244bb in the liquid phase fluorination product are close (15°C and 17°C respectively), making it difficult to separate

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
  • Preparation method of 2-chloro-1,1,1,2-tetrafluoropropane
  • Preparation method of 2-chloro-1,1,1,2-tetrafluoropropane
  • Preparation method of 2-chloro-1,1,1,2-tetrafluoropropane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1,1,2,3-Tetrachloropropene undergoes a nucleophilic substitution reaction with a nucleophilic fluorinating reagent to obtain 1,1,2-trichloro-3-fluoropropene, and the nucleophilic fluorinating reagent is potassium fluoride.

[0022] Add 1,1,2,3-tetrachloropropene (5.0g, 0.028mol) and 30mL of diethylene glycol successively into a 50mL dry there-necked flask equipped with a magnetic stirrer, a thermometer, and a condensing device, and heat up under constant stirring To 120°C, add potassium fluoride (4.87g, 0.084mol) under constant stirring, the molar ratio of potassium fluoride to 1,1,2,3-tetrachloropropene is 3, and react at 120°C for 2h . The reaction product was analyzed by gas chromatography, and the results showed that the conversion rate of 1,1,2,3-tetrachloropropene was 98%, and the selectivity of 1,1,2-trichloro-3-fluoropropene was 90%.

Embodiment 2～6

[0024] The operating process of Examples 2-6 is similar to that of Example 1, except that the nucleophilic fluorinating reagents used are different, and the reaction results are shown in Table 1.

[0025] Table 1

[0026] Example Nucleophilic fluorinating reagents Conversion rates(%) selectivity (%) 2 sodium fluoride 54 85 3 cesium fluoride 99 92 4 Potassium bifluoride 85 95 5 Potassium bifluoride 45 98 6 cesium hydrogen fluoride 90 94

Embodiment 7

[0028] 1,1,2,3-Tetrachloropropene undergoes a nucleophilic substitution reaction with a nucleophilic fluorinating reagent to obtain 1,1,2-trichloro-3-fluoropropene, and the nucleophilic fluorinating reagent is triethylamine dihydrofluoric acid Salt.

[0029] Add the nucleophilic fluorinating agent triethylamine dihydrofluoride (NEt 3 2HF) (10.8g, 0.084mol), then add 1,1,2,3-tetrachloropropene (5.0g, 0.028mol), triethylamine dihydrofluoride and 1,1,2,3-tetrachloropropene The molar ratio of allyl chloride was 3, and the reaction was carried out at a reaction temperature of 110°C for 2 hours. The reaction product was analyzed by gas chromatography, and the results showed that the conversion rate of 1,1,2,3-tetrachloropropene was 90%, and the selectivity of 1,1,2-trichloro-3-fluoropropene was 95%.

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-chloro-1,1,1,2-tetrafluoropropane, which comprises the following three steps: (a) a nucleophilic substitution reaction between 1,1,2,3-tetrachloropropene and a nucleophilic fluorinating reagent is conducted to obtain 1,1,2-trichloro-3-fluoropropene; (b) isomerization of the 1,1,2- trichloro-3-fluoropropene is conducted to obtain 3-fluoro-2,3,3-trichloropropene; and (c) a liquid fluorination reaction between 3-fluoro-2,3,3-trichloropropene and hydrogen fluoride is conducted to obtain 2-chloro-1,1,1,2-tetrafluoropropane. The preparation method of 2-chloro-1,1,1,2-tetrafluoropropane provided by the invention has the characteristics of mild reaction conditions and high conversion rate and selectivity. The preparation method provided by the invention is mainly used for preparing 2-chloro-1,1,1,2-tetrafluoropropane.

Description

technical field [0001] The present invention relates to a kind of preparation method of 2-chloro-1,1,1,2-tetrafluoropropane, in particular to using 1,1,2,3-tetrachloropropene as raw material, through nucleophilic substitution, isomerization and A preparation method for synthesizing 2-chloro-1,1,1,2-tetrafluoropropane by liquid-phase fluorination in three steps. Background technique [0002] 2-Chloro-1,1,1,2-tetrafluoropropane (HCFC-244bb) is the starting material for the synthesis of 2,3,3,3-tetrafluoropropene (HFO-1234yf). HFO-1234yf has zero ozone depletion potential and 4 greenhouse effect potential, and has excellent environmental performance. It is considered as an ideal substitute for HFC-134a. [0003] Chinese patent CN101395108A discloses a method for preparing HCFC-244bb, which uses 1,1,2,3-tetrachloropropene as a raw material, and gas phase fluorination to synthesize 2-chloro-3,3,3-trifluoropropene (HCFC -1233xf), followed by liquid-phase fluorination of HCFC-12...

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
IPC IPC(8): C07C19/10C07C17/21C07C17/087
Inventor 曾纪珺吕剑张伟马辉韩升郝志军杜咏梅亢建平杨志强
Owner 山东华安近代环保科技有限公司
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