Continuous preparation method of hexafluoropropylene tripolymer

A technology of hexafluoropropylene trimer and hexafluoropropylene, which is applied in the field of continuous microchannel preparation of hexafluoropropylene trimer, and can solve the problem of high temperature required for reaction, existence of highly toxic compound carbonyl fluoride, and difficulty in realizing hexafluoropropylene Problems such as selective synthesis of propylene trimer isomers, to achieve the effect of highly selective preparation and improved selectivity

Active Publication Date: 2021-10-26
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +1
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chinese patent CN109734552A discloses a method for obtaining hexafluoropropylene trimer after gas-solid phase contact at high temperature using carriers loaded with metal fluorides such as KF, CsF, NaF, and AgF. This reaction does not require a solvent, but the required temperature for the reaction is High, and the highly toxic compound carbonyl fluoride exists in the reaction product
[0008] The hexafluoropropylene trimer prepared in the above-mentioned prior art is mostly a mixture of three isomers, and it is difficult to selectively synthesize one or two of the isomers of the hexafluoropropylene trimer
Moreover, the above-mentioned liquid phase preparations are all batch reactions, and it is difficult to realize continuous industrial production

Method used

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  • Continuous preparation method of hexafluoropropylene tripolymer
  • Continuous preparation method of hexafluoropropylene tripolymer
  • Continuous preparation method of hexafluoropropylene tripolymer

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0043] In a dry three-necked 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 acetonitrile solution (9.56mol) respectively. Set the bath temperature to 82°C, start stirring and heating, add 3.16g (0.01mol) perfluoro-2-ethyl-3,3-dimethyloxirane through a constant pressure dropping funnel, and wait until the temperature of the oil bath is stable Afterwards, keep for 1 h, stop heating, and filter the mixed solution after cooling down to room temperature (25° C.). After filtering, a catalyst is obtained, which is designated as Cat1.

preparation example 2-9

[0045] Preparation 2-9 is the preparation of Cat 2-6 and comparative Cat 1-3, the operation steps are the same as Preparation 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.

[0046] Table 1 Preparation of Cat 2-6 and comparative Cat 1-3

[0047]

Embodiment 1

[0049] The microchannel reaction module adopting direct-flow 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 forced heat transfer principle of 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.

[0050] Set the temperature of th...

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Abstract

The invention discloses a continuous preparation method of a hexafluoropropylene tripolymer. The continuous preparation method comprises the following step: in a micro-channel reactor, reacting hexafluoropropylene with a liquid-phase catalyst preheated by a preheating module at 70-140 DEG C to obtain the hexafluoropropylene tripolymer. 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 18-crown ether-6, beta-cyclodextrin and polyethylene glycol, the component C is selected from at least one of nitrile compounds, glycol ether compounds and amide compounds; 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 continuous preparation method has the advantages of accurate temperature control, good selectivity, continuous feeding, catalyst reutilization 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 for hexafluoropropylene trimer. Background technique [0002] Hexafluoropropylene trimer is an important fluorine-containing organic intermediate, which can be used to prepare 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 perfluoro-2,4-dimethyl-3-heptene (T1 ), a mixture of perfluoro-2,4-dimethyl-3-ethyl-2-pentene (T2) and perfluoro-4-methyl-3-isopropyl-2-pentene (T3), Since the three are isomers with similar boiling points, it is difficult to separate them. [0003] Chinese patent CN109734552A discloses a method for o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/18C07C17/281C09K5/10
CPCC07C17/281C09K5/10C07C21/18Y02P20/584
Inventor 王飞倪航
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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