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Method for synthesizing perfluoro(2-methyl-3-pentanone)

A technology for the synthesis of perfluorohexanone and its application in chemical instruments and methods, preparation of heterocyclic compounds, chemical/physical/physicochemical processes, etc., which can solve the problem of low formula conversion rate, easy deactivation of composite catalysts, and low reaction yield. Instability and other problems, to achieve the effects of less three wastes, easy automatic control and scale-up production, and shorten synthesis reaction time

Pending Publication Date: 2020-04-14
XIAN ORIGIN CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The composite catalyst used in this patent is easily deactivated, resulting in unstable reaction yield, and the conversion rate of some formulations is lower than 70%.

Method used

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  • Method for synthesizing perfluoro(2-methyl-3-pentanone)
  • Method for synthesizing perfluoro(2-methyl-3-pentanone)
  • Method for synthesizing perfluoro(2-methyl-3-pentanone)

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Experimental program
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Effect test

Embodiment 1

[0033] This embodiment includes the following steps:

[0034] Step 1, isomerization synthesis reaction: Dissolve 0.01mol perfluoro-2,3-epoxy-2-methylpentane in 10mL acetonitrile to obtain perfluoro-2,3-epoxy-2-methylpentane solution, and then perfluoro-2,3-epoxy-2-methylpentane solution and catalyst triethylamine are sent into the microchannel reactor through a micro-injection pump, and then stay at a temperature of 10°C for 600s for isomerization Combination reaction to obtain reaction product; the amount of the substance of the catalyst triethylamine is 2.5% of the amount of the substance of perfluoro-2,3-epoxy-2-methylpentane, and the microchannel reactor of the microchannel reactor The channel aperture is 100μm and the depth is 40μm;

[0035] Step 2. Separation and purification: Cool the reaction product obtained in step 1 to 0°C to 5°C and then let it stand for stratification, then collect the lower layer after standing and stratification for rectification treatment, and...

Embodiment 2

[0042] The difference between the synthesis method of embodiment 2 and embodiment 3 and embodiment 1 is: the temperature of the isomerization synthesis reaction is different, the reaction temperature and the corresponding conversion rate and yield of embodiment 1 to embodiment 3 are shown in the following table 1 Show.

[0043] The temperature of reaction of table 1 embodiment 1~embodiment 3 and corresponding conversion rate and productive rate

[0044]

[0045] As can be seen from Table 1, the optimal reaction temperature for the synthesis of perfluorohexanone by the isomerization reaction of the present invention is 30° C., and when the reaction temperature is lower than 30° C., the degree of reaction progress is low, and the conversion rate and the productive rate are all low. When the reaction temperature exceeds 30°C, the by-products generated by the reaction begin to increase, and both the conversion rate and the yield begin to decrease. Therefore, the temperature of...

Embodiment 4～ Embodiment 10

[0047] Embodiment 4~Example 10 differs from the synthetic method of Example 2 in that: the type of catalyst used is different. The catalyst used in Example 4~Example 10 and Example 2 and the corresponding conversion rate and yield are as follows Table 2 shown.

[0048] The catalyst that table 2 embodiment 4~embodiment 10 and embodiment 2 adopts and corresponding conversion ratio and productive rate

[0049]

[0050] As can be seen from Table 2, various metal fluorides and organic amine catalysts have a certain catalytic effect on the isomerization reaction, and the catalytic effect of organic amine catalysts is better than that of metal fluorides, and among them triethylamine best catalytic effect. Therefore, the isomerization reaction catalyst is preferably triethylamine.

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Abstract

The invention discloses a method for synthesizing perfluoro(2-methyl-3-pentanone). The method comprises the following steps: in the presence of a polar aprotic solvent, carrying out an isomerization synthesis reaction in a micro-channel reactor by taking perfluoro-2,3-epoxy-2-methylpentane as a raw material and using an organic amine or metal fluoride as a catalyst to obtain a reaction product, and sequentially carrying out standing separation and rectification treatment on the reaction product to obtain perfluoro(2-methyl-3-pentanone). According to the invention, a reaction is performed by using a micro-channel reactor, so that the whole isomerization synthesis reaction cannot contact water or water vapor so as to avoid the generation of by-products and improve the conversion rate and theyield of the perfluoro(2-methyl-3-pentanone); and raw materials and a catalyst are subjected to high-speed uniform mixing and heat and mass transfer in the micro-channel reactor, so that the rate ofthe synthesis reaction is increased, the continuous and efficient synthesis of perfluoro(2-methyl-3-pentanone) is realized, and the method is good in repeatability, rapid in system response, easy forautomatic control and amplified production, almost free of amplification effect, high in safety, less in three wastes and easy for industrial production.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, and in particular relates to a method for synthesizing perfluorohexanone. Background technique [0002] Halon belongs to a class of halon chemicals, mainly used in fire extinguishing agents. Halons contain chlorine and bromine, which combine with ozone under solar radiation, causing massive damage to the ozone layer. With the continuous elimination of halon products, halon substitutes for fire extinguishing agents continue to appear, among which the more prominent product is Novec1230 developed by the American 3M company. TM Fireproof liquid, commonly known as perfluorohexanone, its chemical formula is CF 3 CF 2 COCF (CF 3 ) 2 , ASHRAE chemical code is FK-5-1-12, English name Dodecafluoro-2-Methylpentan-3-one. Perfluorohexanone is an important fluorine-containing chemical, which can be used as fire extinguishing agent, cleaning agent, protective gas and solvent for magnes...

Claims

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Application Information

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IPC IPC(8): C07C45/58C07C49/167B01J19/00
CPCC07C45/58B01J19/0093
Inventor 王宪沛张立龙闫俊雷东卫赵志利
Owner XIAN ORIGIN CHEM TECH
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