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Method for synthesizing chlorine trifluoride with high yield

A chlorine trifluoride, high-yield technology, applied in the field of high-yield synthesis of chlorine trifluoride, can solve the problems of complex process, low raw material purity and reaction conversion rate, low chlorine trifluoride yield, etc. Reasonably effective, excellent catalysis, improved purity and conversion

Pending Publication Date: 2022-07-08
欧中电子材料(重庆)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Aiming at the problems of complex process, low raw material purity and reaction conversion rate, and low yield of chlorine trifluoride in the current method for preparing chlorine trifluoride, the present invention provides a method for synthesizing chlorine trifluoride with high yield. Using chlorine and fluorine as raw materials to produce chlorine trifluoride gas, using anhydrous NiF 2 The excellent catalytic effect in the temperature range of 150 ~ 400 ℃, through the effective control of the temperature in the reaction process, the reasonable and effective use of the heat generated in the reaction process, not only can inhibit the formation of ClF as a by-product of the disproportionation reaction, but also avoid the High temperature deep fluorination to generate ClF 5 and ClF 7 Wait for the occurrence of the reaction of fluorinated halogen compounds to finally obtain chlorine trifluoride with a high yield of 95%.

Method used

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  • Method for synthesizing chlorine trifluoride with high yield
  • Method for synthesizing chlorine trifluoride with high yield

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Experimental program
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Effect test

Embodiment 1

[0045]A method for synthesizing chlorine trifluoride in high yield, the specific steps of the method are as follows:

[0046] Step 1: Set the pressure of the reaction system to 0.01-0.02Mpa, chlorine gas is metered into the dryer to be preheated to remove moisture at a temperature of 100-130°C, and fluorine gas is metered into the dryer to be preheated at a temperature of 100-130°C to remove moisture. removal of hydrogen fluoride;

[0047] Step 2: The inert gas argon is introduced into the reactor to be F 2 Carrier gas, the reactor is charged with anhydrous NiF as a catalyst for synthesizing chlorine trifluoride 2 ;

[0048] Step 3: Control the temperature of chlorine gas and fluorine gas at 100-130 °C, and press chlorine gas and fluorine gas by Cl 2 / F 2 The ratio of = 1 / 1 is passed into the gas mixing chamber in the reactor, and the gas flow rate is reduced to 0.01-0.02m / s for buffer mixing to control the F in the mixed gas. 2 The concentration range of 20-40%;

[0049...

Embodiment 2

[0057] A method for synthesizing chlorine trifluoride in high yield, the specific steps of the method are as follows:

[0058] Step 1: Set the pressure of the reaction system to 0.01-0.02Mpa, chlorine gas is metered into the dryer to be preheated to remove moisture at a temperature of 100-130°C, and fluorine gas is metered into the dryer to be preheated at a temperature of 100-130°C to remove moisture. removal of hydrogen fluoride;

[0059] Step 2: The inert gas nitrogen introduced into the reactor is F 2 Carrier gas, the reactor is charged with anhydrous NiF as a catalyst for synthesizing chlorine trifluoride 2 ;

[0060] Step 3: Control the temperature of chlorine gas and fluorine gas at 100-130 °C, and press chlorine gas and fluorine gas by Cl 2 / F 2 The ratio of =1 / 2.5 is passed into the gas mixing chamber in the reactor, and the gas flow rate is reduced to 0.01-0.02m / s for buffer mixing, and the F in the mixed gas is controlled. 2 The concentration range of 20-40%; ...

Embodiment 3

[0069] A method for synthesizing chlorine trifluoride in high yield, the specific steps of the method are as follows:

[0070] Step 1: Set the pressure of the reaction system to 0.1~0.2Mpa, chlorine gas is metered into the dryer to be preheated to remove moisture at a temperature of 100~130℃, and fluorine gas is metered into the dryer to be preheated and removed at a temperature of 100~130℃. removal of hydrogen fluoride;

[0071] Step 2: The inert gas argon is introduced into the reactor to be F 2 Carrier gas, the reactor is charged with anhydrous NiF as a catalyst for synthesizing chlorine trifluoride 2 ;

[0072] Step 3: Control the temperature of chlorine gas and fluorine gas at 100-130 °C, and press chlorine gas and fluorine gas by Cl 2 / F 2 The ratio of = 1 / 3.2 is passed into the gas mixing chamber in the reactor, and the gas flow rate is reduced to 0.05-0.1m / s buffer mixing to control the F in the mixed gas. 2 The concentration range of 20-40%;

[0073] Step 4: Aft...

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Abstract

The invention provides a method for synthesizing chlorine trifluoride with high yield, which adopts chlorine and fluorine as raw materials to prepare chlorine trifluoride gas, utilizes the excellent catalytic action of anhydrous NiF2 in the temperature range of 150-400 DEG C, effectively controls the temperature in the reaction process, reasonably and effectively utilizes the heat generated in the reaction process, and improves the yield of chlorine trifluoride. According to the method, not only can the generation of a disproportionation reaction byproduct ClF be inhibited, but also the reaction of generating ClF5, ClF7 and other fluorinated halogen compounds due to high-temperature deep fluorination can be avoided, and finally, the chlorine trifluoride can be obtained at a high yield of 95%. According to the method for synthesizing chlorine trifluoride, the used raw materials are simple and easy to obtain, the operation process is convenient, the purity and conversion rate of the raw materials are high, the yield of the finally obtained product chlorine trifluoride is high, and industrial production is facilitated.

Description

technical field [0001] The invention relates to a method for synthesizing chlorine trifluoride in high yield, in particular to a method for synthesizing chlorine trifluoride by using fluorine gas and chlorine gas as raw materials, and belongs to the field of fine chemicals. Background technique [0002] Chlorine trifluoride is an important fluorinating agent that can replace elemental fluorine for many reactions. With the development of the electronics industry, CIF 3 It has become an important electronic gas for cleaning of CVD chambers and their piping. with other fluorine-containing gases (such as NF 3 and CF 4 Unlike chlorine trifluoride, which reacts with semiconductor materials at room temperature, it can clean cold-walled CVD chambers. Cleaning with chlorine trifluoride is a chemical etching process, and there is no high-energy ion bombardment process like plasma, and damage to equipment can be minimized. Compared with the cleaning process of plasma cracking to pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B7/24
CPCC01B7/24Y02P20/584
Inventor 雷海平苏·丹尼尔
Owner 欧中电子材料(重庆)有限公司
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