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Preparation method of hexafluorobenzene

A technology of hexafluorobenzene and hexachlorobenzene, which is applied in the field of preparing hexafluorobenzene by using hexachlorobenzene and fluorine gas by direct reaction, can solve the problems of high raw material price, high requirement on reaction conditions, low product yield, etc. The effect of low cost, mild reaction and easy control, and high product yield

Active Publication Date: 2020-05-08
洛阳森蓝化工材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, the above traditional hexafluorobenzene synthesis methods all have the disadvantages of high raw material prices, high requirements for reaction conditions, and low product yields.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1) Perform dehumidification, dust removal and purification treatment on the reactor;

[0038] 2) Add 1.5L (mass of 1422g) of dimethylformamide solvent into the reactor, then add 2848g of hexachlorobenzene, close the reactor and vacuumize it, and replace the air in the reactor with nitrogen;

[0039] 3) Cool down the reactor, control the temperature in the reactor at -40°C, and stir for 1 hour to promote complete dissolution;

[0040] 4) Feed fluorine gas into the reactor, calculate the intake air amount according to the ratio of the fluorine intake amount and the theoretical intake amount of fluorine gas, and control the intake air volume of pure fluorine gas (that is, the concentration of fluorine gas is 100%) through a rotameter, Keep the temperature in the reactor at -40°C, the reaction pressure is 0MPa, the tail gas generated by the reaction is absorbed by alkali solution, then adsorbed by dry adsorbent and then vented;

[0041] 5) Calculate the amount of fluorine ...

Embodiment 2

[0044] 1) Perform dehumidification, dust removal and purification treatment on the reactor;

[0045] 2) Add 1.5L (mass 1185g) of acetonitrile solvent into the reactor, then add 2848g of hexachlorobenzene, close the reactor, and vacuumize it, and then replace the air in the reactor with nitrogen;

[0046] 3) Cool down the reactor, control the temperature in the reactor at -20°C, and stir for 1 hour to promote complete dissolution;

[0047] 4) Feed fluorine gas into the reactor, and control the intake of pure fluorine gas (that is, the concentration of fluorine gas is 100%) through a rotameter, so that the temperature in the reactor is maintained at -20 ° C, and the reaction pressure is 0.3 MPa, the tail gas produced by the reaction is absorbed by the alkali solution, then absorbed by the dry adsorbent and then emptied;

[0048] 5) Calculate the amount of fluorine fed into the reaction according to the theoretical amount of fluorine fed into the fluorine gas. When the amount of...

Embodiment 3

[0051] 1) Perform dehumidification and dust removal purification treatment on the reactor;

[0052] 2) Add 1.5L (mass 1185g) of acetonitrile solvent into the reactor, then add 2848g of hexachlorobenzene, close the reactor, and vacuumize it, and then replace the air in the reactor with nitrogen;

[0053] 3) Lower the temperature of the reactor, control the temperature at -20°C, and stir for 1 hour to promote complete dissolution;

[0054]4) Feed fluorine gas into the reactor, and control the concentration of 10% fluorine gas intake through the rotameter, so that the temperature in the reactor is maintained at -20°C, and the reaction pressure in the reactor is 0.8MPa, The tail gas produced by the reaction is absorbed by the alkali solution, then absorbed by the dry adsorbent and then emptied;

[0055] 5) Calculate the amount of fluorine entering the reaction according to the theoretical amount of fluorine entering the fluorine gas. When the amount of fluorine entering is 1254g,...

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Abstract

A preparation method of hexafluorobenzene comprises the following steps: dehumidifying, dedusting and purifying a reactor; adding a hexachlorobenzene solid into the reactor filled with a solvent, mixing uniformly, and sealing the reactor; vacuumizing the sealed reactor for replacement, and completely discharging air in a container; cooling the reactor, controlling the temperature in the reactor tobe not more than -10 DEG C, and then stirring the solvent added with the hexachlorobenzene solid to completely dissolve the hexachlorobenzene solid; introducing fluorine gas into the reactor in a slow bubbling manner, controlling the gas inflow of the fluorine gas, controlling the temperature in the reaction container to be not more than -10 DEG C, and controlling the reaction pressure in the reaction container to be 0-1MPa; and obtaining a hexafluorobenzene mother liquor after the reaction is finished, and purifying the hexafluorobenzene mother liquor to obtain the hexafluorobenzene product.The method has the advantages of simple reaction conditions, low raw material cost, mild and easily-controlled reaction, low operation requirements and high product yield.

Description

technical field [0001] The invention belongs to the field of chemical production technology, in particular to a method for preparing hexafluorobenzene by direct reaction of hexachlorobenzene and fluorine gas. Background technique [0002] Hexafluorobenzene, also known as perfluorobenzene, can be used as an important intermediate for the synthesis of perfluorinated aromatic compounds. Hexafluorobenzene can not only be used in the field of anesthetics in medicine, but also be used as an excellent solvent for various organic substances. In recent years, in the research on the development of new liquid crystal materials, it has been found that liquid crystal compounds derived from perfluorobenzene have good properties. [0003] The preparation method of existing hexafluorobenzene has: [0004] 1. Direct fluorination method: Vorozhtsov N.N., Platonov V.E., Yakobson G.G. proposed to use anhydrous KF to replace the chlorine atoms on hexachlorobenzene to prepare hexafluorobenzene i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/20C07C25/13
CPCC07C17/204C07C25/13Y02P20/582
Inventor 韩保国阎晓冬崔武孝李博文
Owner 洛阳森蓝化工材料科技有限公司
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