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

Method for preparing 2,3,3,3-tetrafluoropropene

A technology of tetrafluoropropene and tetrafluoropropanol, which is applied in the field of preparation of 2,3,3,3-tetrafluoropropene, can solve the problems of waste of fluorine element and low utilization rate of fluorine element, and achieves low equipment requirements and conditions. Mild, easy-to-industrial effect

Inactive Publication Date: 2018-05-04
HANGZHOU NORMAL UNIVERSITY +1
View PDF6 Cites 9 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The mainstream production process of florfenicol in China uses Ishikawa reagent (N,N-diethyl-1,1,2,3,3,3-hexafluoropropylamine) for fluorination, and the utilization rate of fluorine is relatively low. Low, the produced by-product N,N-diethyl-2,3,3,3-tetrafluoropropionamide reaches more than 1,000 tons / year, which not only causes waste of fluorine, but also brings huge environmental pressure to the production of enterprises

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
  • Method for preparing 2,3,3,3-tetrafluoropropene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Hydrolysis reaction:

[0039] Add 603.5g (3.0mol) of N,N-diethyl-2,3,3,3-tetrafluoropropionamide and 440.6g (5.0mol) of 1,4-dioxane into a 3000mL three-necked glass reaction flask, mechanically Add dropwise 85% sulfuric acid solution 691.8g (H 2 SO 4 6.0mol), after the drop, the temperature rose to 100°C, and the temperature was maintained for 10 hours. Fluoropropionic acid, the gas chromatography analysis purity is 98.5%, the yield is 87.1%.

[0040] Reduction reaction:

[0041] Add NaBH to 1000mL three-necked glass reaction flask 3 CN 31.4g (0.5mol), tetrahydrofuran 200g (4.35mol), heated up to 40°C under magnetic stirring, added 73.0g (0.5mol) of 2,3,3,3-tetrafluoropropionic acid dropwise, and kept the reaction at 50°C after dropping 3 hours. After the reaction is complete, lower the temperature to 10°C, add 200g of deionized water dropwise, extract the reaction solution with ethyl acetate (100mL×3 times), combine the extracts, carry out atmospheric distillatio...

Embodiment 2

[0047] Hydrolysis reaction:

[0048] Add 603.5g (3.0mol) of N,N-diethyl-2,3,3,3-tetrafluoropropionamide and 440.6g (5.0mol) of 1,4-dioxane into a 3000mL three-necked glass reaction flask, mechanically Add 608g of concentrated hydrochloric acid (HCl6.0mol) dropwise under stirring, the internal temperature rises to 80°C after dropping, and keep it warm for 12 hours. 2,3,3,3-Tetrafluoropropionic acid has a gas chromatography purity of 97.7% and a yield of 73.0%.

[0049] Reduction reaction:

[0050] Add LiAlH to a 1000mL three-necked glass reaction flask 4 19g (0.5mol), 200g (4.35mol) of absolute ethanol, heated to 40°C under magnetic stirring, slowly added 73.0g (0.5mol) of 2,3,3,3-tetrafluoropropionic acid dropwise, and kept at 50°C after dropping React for 3 hours. After the reaction is complete, lower the temperature to 10°C, add 200g of deionized water dropwise, extract the reaction solution with ethyl acetate (100mL×3 times), combine the extracts, carry out atmospheric...

Embodiment 3

[0056] Hydrolysis reaction:

[0057] Add 603.5g (3.0mol) of N,N-diethyl-2,3,3,3-tetrafluoropropionamide and 54.0g (3.0mol) of deionized water into a 3000mL three-necked glass reaction flask, add 85 % sulfuric acid solution 691.8g (H 2 SO 4 6.0mol), the temperature rose to 100°C after dripping, and kept for 10 hours. After the reaction was completed, rectification at atmospheric pressure collected 119.5-120.5°C fractions to obtain 377.3g of colorless liquid, which was 2,3,3,3-tetra Fluoropropionic acid, the gas chromatography analysis purity is 99.0%, the yield is 85.3%.

[0058] Reduction reaction:

[0059] Add NaBH to 1000mL three-necked glass reaction flask 4 18.9g (0.5mol), 34.1g (0.25mol) of zinc chloride, 200g (4.35mol) of absolute ethanol, heated to 40°C under magnetic stirring, slowly added dropwise 73.0 g of 2,3,3,3-tetrafluoropropionic acid g (0.5 mol), after the dropwise reaction at 60°C for 3 hours. After the reaction is complete, lower the temperature to 10...

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 relates to a method for preparing 2,3,3,3-tetrafluoropropene. The method comprises the following steps: (1) by taking a by-product N,N-diethyl-2,3,3,3-tetrafluoropropylamide of an Ishikawa's reagent as a raw material, hydrolyzing under acidic or alkaline conditions to obtain 2,3,3,3-tetrafluoropropionic acid; (2) contacting the 2,3,3,3-tetrafluoropropionic acid with a reducing agentin the presence of a catalyst or in a catalyst-free system so as to obtain 2,3,3,3-tetrafluoropropanol; and (3) reacting the 2,3,3,3-tetrafluoropropanol in the presence of a dehydrating agent, therebyobtaining the 2,3,3,3-tetrafluoropropene. The method disclosed by the invention is simple in operation, mild in conditions and low in equipment requirements, recycling of the by-product is realized,and industrialized application is easily realized.

Description

technical field [0001] The invention relates to a preparation method of refrigerant, in particular to a preparation method of 2,3,3,3-tetrafluoropropene. Background technique [0002] In the vapor compression refrigeration system, the refrigerant is vividly called "blood". 1,1,1,2-tetrafluoroethane (HFC-134a), does not damage the ozone layer, has good safety performance (non-flammable, non-explosive, non-toxic, non-irritating, non-corrosive), making It has become a very effective and safe substitute for R12 (dichlorodifluoromethane), and is the most widely used third-generation automotive refrigerant. However, HFC-134a is a greenhouse gas with a GWP value of 1340 (relative to CO 2 In terms of), according to the provisions of the Montreal Protocol, will be phased out and banned. In the search for a replacement for HFC-134a, 2,3,3,3-tetrafluoropropene (HFO-1234yf) has zero ozone depletion potential (ODP=0), very low greenhouse effect potential (GWP=4 ), stand out among man...

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 Applications(China)
IPC IPC(8): C07C17/35C07C21/18
CPCC07C17/35C07C29/149C07C51/06C07C21/18C07C31/38C07C53/21
Inventor 章鹏飞吴海锋赵国标叶盛徐龙
Owner HANGZHOU NORMAL UNIVERSITY
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