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

Continuous preparation method of high-purity perfluoro-2, 4-dimethyl-3-heptene

A dimethyl, high-purity technology, applied in the field of continuous microchannel preparation of high-purity hexafluoropropylene trimer, can solve the problems that the overall yield is only 50.7%, and it is difficult to realize continuous industrial production, so as to improve selectivity , The effect of improving product yield

Active Publication Date: 2021-10-26
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +1
View PDF9 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Chinese patent CN109072054A discloses a method for obtaining hexafluoropropylene trimer by reacting hexafluoropropylene with a catalyst in the presence of a solvent, and the proportion of hexafluoropropylene trimer isomer mixture in the reaction product of this method is about 87.6%. , the highest purity of 98.45% perfluoro-2,4-dimethyl-3-heptene can be obtained after distillation and purification, but the overall yield is only 50.7%
[0008] In summary, most of the mixtures prepared in the prior art are mixtures of three isomers of hexafluoropropylene trimer, and there is little mention of high-purity perfluoro-2,4-dimethyl-3-heptene Prepared
And the above-mentioned liquid-phase preparation is all batch reaction, it is difficult to realize continuous industrialized production

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
  • Continuous preparation method of high-purity perfluoro-2, 4-dimethyl-3-heptene
  • Continuous preparation method of high-purity perfluoro-2, 4-dimethyl-3-heptene
  • Continuous preparation method of high-purity perfluoro-2, 4-dimethyl-3-heptene

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0039] In a dry three-neck flask equipped with a reflux condenser and a magnetic stirrer, add 5.8g (0.1mol) of potassium fluoride, 26.4g (0.1mol) of 18-crown-6 and 500ml of N,N,-dimethylformaldehyde Amide solution (6.46mol), the oil bath temperature is set to 100°C, start stirring and heating, add 3.0g (0.01mol) perfluoro-4-methyl-2-pentene through a constant pressure dropping funnel, wait until the oil bath temperature After stabilization, keep it for 1 h, stop heating, and filter the mixed solution after cooling down to room temperature (25° C.). After filtration, a catalyst is obtained, which is designated as Cat1.

preparation example 2-7

[0041] Preparation example 2-7 is the preparation of Cat 2-3 and comparative Cat 1-3, the operation steps are the same as preparation example 1, the difference is that the types of component A, component B, component C and component D are changed during the preparation process Or dosage, see Table 1 below for details.

[0042] Table 1 Preparation of Cat 2-6 and comparative Cat 1-3

[0043]

Embodiment 1

[0045] The microchannel reaction module that adopts straight-through channel structure is used as preheating module 3 and quenching module 10, adopts attached figure 2 The corning "heart-shaped" microchannel reaction module shown in (e) is used as the reaction module, according to the attached figure 1 The reaction process shown constitutes a continuous flow microchannel reaction system. According to the principle of forced heat transfer in the microchannel reactor, only two temperature measuring points are set at the reactor inlet and outlet. Before the reaction, the microchannel reaction system and connecting pipelines were dehydrated and dried, and the air tightness was checked at 1.0MPa. The liquid phase catalyst is continuously and stably added to the microchannel reaction system through the liquid phase pump 1; the hexafluoropropylene gas is continuously quantitatively added to the microchannel reaction system through the gas mass flow meter 2.

[0046] Set the temper...

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 continuous preparation method of high-purity perfluoro-2, 4-dimethyl-3-heptene. The preparation method comprises the following step: in a micro-channel reactor, hexafluoropropylene and a liquid phase catalyst preheated by a preheating module react at 70-140 DEG C to obtain the perfluoro-2, 4-dimethyl-3-heptene. the liquid-phase catalyst is prepared from a component A, a component B, a component C and a component D, the component A is selected from at least one of potassium fluoride, cesium fluoride and potassium bifluoride; the component B is selected from at least one of crown ether, cyclodextrin, polyethylene glycol, calixarene or pillararene; the component C is an amide compound; and the component D is selected from at least one of perfluoro-4-methyl-2-pentene, perfluoro-2-methyl-2-pentene and perfluoro-2-ethyl-3, 3-dimethyl ethylene oxide. The method has the advantages of accurate temperature control, good selectivity, high product purity and the like.

Description

technical field [0001] The invention relates to the field of fluorine-containing intermediates, in particular to a microchannel continuous preparation method of high-purity hexafluoropropylene trimer. Background technique [0002] Hexafluoropropylene trimer is an important fluorine-containing organic intermediate, which can be used in the preparation of fluorine-containing surfactants for detergent, textile, leather and other fields, and can also be used as a reaction solvent and heat transfer medium. At present, the trimer of hexafluoropropylene is mainly obtained by telomerization of hexafluoropropylene through liquid phase method or gas phase method, but the trimer obtained by telomerization is mostly perfluoro-2,4-dimethyl-3-heptene, A mixture of perfluoro-2,4-dimethyl-3-ethyl-2-pentene and perfluoro-4-methyl-3-isopropyl-2-pentene, since the three are isomers solid, with similar boiling points, it is difficult to separate. [0003] U.S. Patent No. 4,296,265A discloses ...

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): C07C2/22B01J31/22C07C21/18B01J19/00
CPCC07C2/22B01J31/2213B01J2231/32B01J2531/13C07C2531/22B01J19/0093C07C21/18Y02P20/584
Inventor 王飞倪航
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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