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A kind of preparation method of chlorine trifluoride

A chlorine trifluoride and fluorine gas technology, applied in the direction of inter-halogen compounds, etc., can solve the problems of low reliability of equipment, large storage and transportation of raw material chlorine gas, complicated production process, etc., and achieves convenient feeding and discharging, cheap raw materials, The effect of the simple structure of the reactor

Active Publication Date: 2016-08-17
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] To sum up, the currently known preparation methods of chlorine trifluoride mainly have problems such as low equipment reliability, complex production process, and large safety risks in the storage and transportation of raw chlorine gas.

Method used

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  • A kind of preparation method of chlorine trifluoride
  • A kind of preparation method of chlorine trifluoride

Examples

Experimental program
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Effect test

Embodiment 1

[0052] (1) Firstly, the vacuum pump is used to vacuumize the various parts of the device; then use fluorine gas to purge and replace the residual air and moisture in the system; then excessive CCl 4 Add in the gas-liquid reactor, and feed fluorine gas from the bottom of the gas-liquid reactor at a flow rate of 0.1L / min, CCl 4 Bubble reaction with fluorine gas at 0.6MPa and 50°C to obtain product 1;

[0053] (2) Feed product 1, fluorine gas and nitrogen into the synthesis reactor with the flow velocity of 0.1L / min, 0.3L / min and 1.2L / min respectively, set the operating pressure of the synthesis reactor to be 0.6MPa, at 100 Reaction at ℃ to obtain product 2;

[0054] (3) Pass the product 2 into the cold trap, set the operating pressure of the cold trap to 0.6MPa, liquefy the product 2 at 0°C, and send the low-boiling point gas impurities to the tail gas treatment system through the exhaust pipeline. Empty after chemical treatment. After 20 hours, the feeding of raw gas was sto...

Embodiment 2

[0059] (1) First, the vacuum pump is used to pre-treat the various parts of the device; then nitrogen is used to purge and replace the residual air and moisture in the system; then the excess SiCl 4 Add in the gas-liquid reactor, and feed fluorine gas from the bottom of the gas-liquid reactor at a flow rate of 1L / min, SiCl 4 Bubble reaction with fluorine gas at 0.03MPa and 25°C to obtain product 1;

[0060] (2) Pass the product 1, fluorine gas and nitrogen gas into the synthesis reactor at a flow rate of 1L / min, 4L / min and 40L / min respectively, set the operating pressure of the synthesis reactor to 0.32MPa, and react at 380°C , to obtain the product 2;

[0061] (3) Pass the product 2 into the cold trap, set the operating pressure of the cold trap to 0.05MPa, liquefy the product 2 at -95°C, and send the low-boiling point gas impurities to the tail gas treatment system through the exhaust pipeline. Void after chemical treatment. After 3 hours, the feeding of raw material gas ...

Embodiment 3

[0066] (1) First, carry out vacuum pretreatment on each part of the device by a vacuum pump; then use nitrogen to purge and replace the residual air and moisture in the system; then excessive CCl 4 and SiCl 4 mixed solution (CCl 4 with SiCl 4 The volume ratio is 2:1) into the gas-liquid reactor, and fluorine gas, CCl 4 、SiCl 4 Bubble reaction with fluorine gas at -0.09MPa, -20°C to obtain product 1;

[0067] (2) Feed product 1, fluorine gas and nitrogen into the synthesis reactor with the flow rate of 0.5L / min, 1L / min and 0.51L / min respectively, set the operating pressure of the synthesis reactor to be-0.09MPa, at 400 Reaction at ℃ to obtain product 2;

[0068] (3) Pass the product 2 into the cold trap, set the operating pressure of the cold trap to -0.09MPa, liquefy the product 2 at -100°C, and send the low-boiling point gas impurities to the tail gas treatment system through the exhaust pipeline. Release it after harmless treatment. After 10 hours, the feeding of raw ...

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Abstract

The invention discloses a preparation method of chlorine trifluoride and belongs to the field of fine chemical engineering. The method comprises the following steps: carrying out a bubbling reaction on liquid-phase chloride and fluorine gas at a certain temperature to obtain a product 1; then charging the product 1, a diluent gas and fluorine gas in a synthesis reactor, and reacting at a certain temperature to obtain a product 2; finally carrying out liquidation, lightweight material discharge and vaporization treatments on the product 2 to obtain chlorine trifluoride. The raw materials in the preparation method are low in price and easily available, thus avoiding the adoption of chlorine with high corrosion and high toxicity, improving safety during production, transportation and storage processes; moreover, the reactor is simple in structure and convenient for material charging and discharging; the reaction conversion rate is high; by-products can be easily separated; and the preparation method can be put into industrial production easily.

Description

technical field [0001] The invention relates to a preparation method of chlorine trifluoride, in particular to a method for preparing chlorine trifluoride by using fluorine gas, carbon tetrachloride and / or silicon tetrachloride as raw materials, and belongs to the field of fine chemical industry. Background technique [0002] Chlorine trifluoride is the most active halogen fluoride known chemically, and is a powerful fluorinating agent. The boiling point of chlorine trifluoride is 11.5°C. It is a gas that is easy to condense under normal circumstances. It can be reacted in any state of gas or liquid as required, which is beyond the reach of general fluorinating agents. Many metal oxides and chlorides react with chlorine trifluoride to generate corresponding chlorides when heated. Using the characteristics of chlorine trifluoride, many important metal fluorides can be prepared, especially for the separation and purification of rare elements. . With the rapid development of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B7/24
CPCC01B7/24
Inventor 王新喜刘智慧丁成马卫东沙婷董云海郑秋艳郭绪涛
Owner PERIC SPECIAL GASES CO LTD
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