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Purification method of chlorine trifluoride

A technology of chlorine trifluoride and purification method, which is applied in the direction of halogen compounds, etc., can solve the problems of material selection and use of purification equipment, and achieve the effects of reducing the content of impurities, high purification efficiency and simple operation

Active Publication Date: 2015-04-29
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The boiling point of hydrogen fluoride (19°C) is relatively close to that of chlorine trifluoride (11.5°C). It is difficult to separate and remove the impurities of hydrogen fluoride in chlorine trifluoride by distillation or freezing conventional purification methods, and they are all highly corrosive substances. There are strict requirements on the selection and use of materials for purification equipment. At present, there is no patent registration related to the purification of chlorine trifluoride at home and abroad.

Method used

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  • Purification method of chlorine trifluoride
  • Purification method of chlorine trifluoride

Examples

Experimental program
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Effect test

Embodiment 1

[0034] (1) The entire purification system is deoiled, dried and vacuumized, and replaced with high-purity nitrogen for 5 times to ensure that there are no impurities other than nitrogen in the system. Fill the adsorption tower with spherical sodium fluoride particles with a diameter of 1mm and a porosity of 10%, with a filling height of 450mm, and inject high-purity nitrogen to activate sodium fluoride at 500°C for 10h.

[0035] (2) vaporize the chlorine trifluoride solution (the content of chlorine trifluoride is 91%) in the crude product storage tank by a vaporizer, in the vaporizer, water is used as a heat-conducting agent, and the water temperature is 16°C, and the vaporized chlorine trifluoride (at a temperature of 15° C.) into an adsorption tower filled with fillers at a flow rate of 0.4 L / min, and stay in the adsorption tower for 0.1 min at 20° C. and 0.01 MPa to obtain a grade 1 crude product of chlorine trifluoride;

[0036] (3) pass the first-grade crude product of c...

Embodiment 2

[0041] (1) The entire purification system is deoiled, dried and vacuumized, and replaced with high-purity nitrogen for 5 times to ensure that there are no impurities other than nitrogen in the system. Fill the adsorption tower with spherical potassium fluoride particles with a diameter of 10 mm and a porosity of 30%, with a filling height of 700 mm, and inject high-purity nitrogen to activate potassium fluoride at 300 °C for 6 hours.

[0042] (2) the chlorine trifluoride solution (the content of chlorine trifluoride is 95%) in the crude product storage tank is vaporized by a vaporizer, and water is used as a heat conducting agent in the vaporizer, and the water temperature is 60 ℃, and the vaporized chlorine trifluoride (at a temperature of 40° C.) into an adsorption tower filled with fillers at a flow rate of 0.9 L / min, and stay in the adsorption tower for 5 minutes at 40° C. and 0.27 MPa to obtain a first-grade crude product of chlorine trifluoride;

[0043] (3) pass the fir...

Embodiment 3

[0048] (1) The entire purification system is deoiled, dried and vacuumized, and replaced with high-purity nitrogen for 5 times to ensure that there are no impurities other than nitrogen in the system. Fill the adsorption tower with spherical potassium fluoride particles with a diameter of 12mm and a porosity of 80% to a filling height of 700mm, and pass high-purity nitrogen to activate potassium fluoride at 400°C for 8 hours.

[0049] (2) Vaporize the chlorine trifluoride solution (the content of chlorine trifluoride is 95%) in the crude product storage tank by a vaporizer, in the vaporizer, heat transfer oil is used as a heat transfer agent, and the temperature of the heat transfer oil is 90°C, and the vaporized trifluoride Chlorine fluoride (at a temperature of 50° C.) is passed into an adsorption tower filled with packing at a flow rate of 1.8 L / min, and is retained in the adsorption tower at 80° C. and 1 MPa for 5 minutes to obtain a first-grade crude product of chlorine tr...

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Abstract

The invention discloses a purification method of chlorine trifluoride, and belongs to the field of fine chemical engineering. The purification method comprises the following steps: introducing chlorine trifluoride crude products into a tower kettle of a rectifying tower; performing vacuum-pumping on the rectifying system, starting to heat the tower kettle after the vacuum degree is stable, and performing total refluxing for 3-15 h to enable the impurity composition of which the boiling point is lower than that of chlorine trifluoride to be gathered at the top of the rectifying tower; when the temperature of the tower kettle is at a temperature of 0-5 DEG C, the temperature of the rectifying tower top is 2-3 DEG C below zero, then collecting front cut fraction at a reflux ratio of 30-300 and condensing and recovering; when the temperature of the tower kettle is 5-8 DEG C, the temperature of the rectifying tower top is 3-6 DEG C, collecting medium fraction at a reflux ratio of 10-90, and condensing and recovering; when the temperature of the tower kettle increases for 2 DEG C, that is, the temperature is 7-10 DEG C, the temperature of the rectifying tower top is 5-8 DEG C, collecting after cut fraction at a reflux ratio of 15-140, and condensing and recovering; when the temperature of the tower kettle is higher than or equal to 15 DEG C, stopping collecting after cut fraction, stopping heating, stopping vacuum-pumping, and finishing rectifying, wherein the medium fraction is the chlorine trifluoride refined product. The method is simple to operate and is high in purification efficiency.

Description

technical field [0001] The invention relates to a method for purifying chlorine trifluoride, belonging to the field of fine chemicals. Background technique [0002] Chlorine trifluoride is the most active halogen fluoride known chemically. It is a high-energy and highly reactive substance. It is mainly used in the electronics industry, nuclear industry, uranium enrichment and military applications. High-purity chlorine trifluoride is mainly used in the cleaning of CVD chambers and pipelines in the fields of semiconductors, liquid crystals, solar energy, and LEDs. It has obvious advantages in cleaning quality, efficiency, and reducing the greenhouse effect. Unlike other fluorine-containing gases used for cleaning (such as NF 3 、C 2 f 6 and CF 4 ), chlorine trifluoride can react with semiconductor materials at room temperature, and there is no need to heat the cleaning part. Therefore, the use of chlorine trifluoride can save heating parts and heating steps, and it is not ...

Claims

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Application Information

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IPC IPC(8): C01B7/24
CPCC01B7/24
Inventor 王新喜刘智慧王占卫马卫东张净普张帅宋富财王斌
Owner PERIC SPECIAL GASES CO LTD
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