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Three-stage rectification method of electronic-grade CHF3

An electronic grade, rectification technology, applied in chemical instruments and methods, organic chemistry, preparation of halogenated hydrocarbons, etc., can solve the problems of failure to meet the requirements of semiconductor use, difficult separation of various impurities deep removal technology, low purity, etc.

Active Publication Date: 2021-06-04
FUJIAN DEER TECH CORP
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  • Description
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Problems solved by technology

[0003]The purity of general electronic-grade trifluoromethane is 99.9999%, and its purification involves the deep removal technology of various impurities, which is difficult to separate
At present, the purity of the existing industrial trifluoromethane in my country is relatively low, and there are few reports. Patent 201110423419.4 adopts a low-temperature batch rectification process to prepare high-purity trifluoromethane, with a purity of 99.99%, which does not meet the use requirements of the semiconductor industry (electronic grade).

Method used

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  • Three-stage rectification method of electronic-grade CHF3
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  • Three-stage rectification method of electronic-grade CHF3

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preparation example Construction

[0041] Please also see Figure 4 , the present invention further provides a kind of electronic grade CHF The novel preparation method comprises: the following steps:

[0042] S7, feed a reaction gas mixed with HF and chlorodifluoromethane from top to bottom into the catalyst tube 105, wherein the ratio of HF to chlorodifluoromethane is 1.05-1.1:1 and HF will be partially dissolved in The water formed is non-reactive, so an excess is required; the catalyst column 105 includes activated catalyst particles;

[0043] S8, controlling the upper temperature of the catalyst tube 105 to 220-230°C, the middle temperature to 245-255°C, the lower temperature to 230-240°C, the reaction pressure to 0.05-0.2Mpa, and the residence time to 40-80s to obtain the catalyst with a purity of 98% or more. Trifluoromethane crude product;

[0044] S9, after the crude trifluoromethane product is washed with water, washed with alkali, dried and rectified, electronic-grade CHF with a purity of 99.9999% ...

Embodiment 1

[0058] The chromium trichloride / activated carbon composite of 8 parts by weight, the aluminum trichloride of 60 parts by weight, the nickel chloride of 3 parts by weight, the magnesium chloride of 5 parts by weight are mixed wherein, chromium trichloride is in said chromium trichloride The content in the activated carbon composite is 20wt%, and it is filled into the catalyst column tube 105 and assembled on the device for activation; N 2 The flow rate is 300ml / min, the catalyst bed temperature is raised to 100°C at a heating rate of 10°C / min, and dried at a constant temperature for 4 hours; the temperature of the catalyst tube 105 is raised to 200°C at a heating rate of 10°C / min, and dried at a constant temperature for 6 hours; 200°C After drying, start fluorination with HF at this temperature; N 2 The flow rate is maintained at 300ml / min, and the HF flow rate is gradually increased from 10ml / min to 300ml / min, which can be adjusted by 20ml / min each time, once every hour. 5°C,...

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Abstract

The invention provides a novel preparation method of electronic-grade CHF3, which comprises the following steps: S1, reaction gas formed by mixing HF and monochlorodifluoromethane is introduced into a catalyst tube nest (105) from top to bottom, and the ratio of HF to monochlorodifluoromethane is (1.05-1.1):1, wherein the catalyst tube nest (105) comprises activated catalyst particles, the catalyst particles are formed by mixing 8-10 parts by weight of chromium trichloride / activated carbon compound, 50-70 parts by weight of aluminum trichloride, 2-5 parts by weight of nickel chloride and 2-5 parts by weight of magnesium chloride, and the content of chromium trichloride in the chromium trichloride / activated carbon compound is 15-25 wt%; s2, controlling the upper temperature of the catalyst tube nest (105) to be 220-230 DEG C, the middle temperature of same to be 245-255 DEG C, the lower temperature of same to be 230-240 DEG C, the reaction pressure to be 0.05-0.2 Mpa and the retention time to be 40-80 s, so as to obtain a trifluoromethane crude product with the purity of 98% or above; s3, carrying out water washing, alkali washing, drying and rectification on the trifluoromethane crude product to obtain the electronic-grade CHF3 with the purity of 99.9999%.

Description

technical field [0001] The present invention relates to an electronic grade CHF 3 three-stage distillation method. Background technique [0002] Trifluoromethane is a versatile and chemically stable fluoroalkane. In the semiconductor process, the demand for high-purity trifluoromethane as an etchant in the manufacturing process of 8-12 inch chips continues to increase with the rapid development of the semiconductor industry. [0003] The purity of general electronic-grade trifluoromethane is 99.9999%, and its purification involves the deep removal of various impurities, which is difficult to separate. At present, the purity of the existing industrial trifluoromethane in my country is relatively low, and there are few reports. Patent 201110423419.4 adopts a low-temperature batch rectification process to prepare high-purity trifluoromethane, with a purity of 99.99%, which does not meet the use requirements of the semiconductor industry (electronic grade). . Contents of the...

Claims

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Application Information

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IPC IPC(8): C07C17/383C07C19/08
CPCC07C17/383C07C19/08
Inventor 张奎华祥斌黄雨迪杨青黄荣保阙祥育
Owner FUJIAN DEER TECH CORP
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