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Method for removing water in hydrogen fluoride by reactive distillation

A technology of reactive distillation and hydrogen fluoride, which is applied in the fields of fluorine/hydrogen fluoride, chemical industry, climate sustainability, etc. It can solve the problems of difficult separation of impurities, high operation risk, and low water removal efficiency, and achieve safe operation and simple process , High water removal efficiency

Active Publication Date: 2016-01-06
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing technology for removing water in hydrogen fluoride has problems such as high operational risk, low water removal efficiency, and other difficult-to-separate impurities.
At present, there is no report about the use of reactive distillation to remove moisture in hydrogen fluoride in published patents and other documents

Method used

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  • Method for removing water in hydrogen fluoride by reactive distillation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 1 kg of tungsten tetrafluoride with a diameter of 0.1mm into the reaction kettle 1 through the feed port I2, vacuumize the entire reaction device with a vacuum pump 4, and use the helium in the helium cylinder 5 for purging, and repeat for 10 Vacuum replacement treatment. Then, 100 kg of liquefied hydrogen fluoride was fed into the reactor 1 through the feed port II6. Utilize heating furnace 10 to heat reactor 1, utilize condenser 3 to lower the temperature, make the temperature difference between reactor 1 and condenser 3 be 5~10 ℃, pressure difference be 0.01~0.02MPa, the rectifying tower The water removal rectification temperature is controlled at 60-80°C for rectification. Take out a small amount of hydrogen fluoride from the condenser 3 through the sampling port 9 for analysis. When the water content in the hydrogen fluoride drops below 1ppm, adjust the rectification collection temperature of the rectification tower to 20-30°C and maintain a pressure differenc...

Embodiment 2

[0030] Add 1 kg of tungsten tetrafluoride with a diameter of 1 mm into the reaction kettle 1 through the feed port I2, vacuumize the entire reaction device with the vacuum pump 4, and use the helium in the helium cylinder 5 to purge, repeat 10 times Vacuum replacement treatment. Then, 800 kg of liquefied hydrogen fluoride was added into the reactor 1 through the feed port II6. Utilize heating furnace 10 to heat reactor 1, utilize condenser 3 to lower the temperature, make the temperature difference between reactor 1 and condenser 3 be 5~10 ℃, pressure difference be 0.01~0.02MPa, the rectifying tower The water removal rectification temperature is controlled at 80-100°C for rectification. Take out a small amount of hydrogen fluoride from the condenser 3 through the sampling port 9 for analysis. When the water content in the hydrogen fluoride drops below 1ppm, adjust the rectification collection temperature of the rectification tower to 30-40°C and maintain a pressure difference...

Embodiment 3

[0032] Add 0.5 kg of tungsten tetrafluoride with a diameter of 0.5 mm into the reaction kettle 1 through the feed port I2, vacuumize the entire reaction device with the vacuum pump 4, and use the helium in the helium cylinder 5 for purging, and repeat 10 vacuum replacement treatments. Then, 500 kg of liquefied hydrogen fluoride was fed into the reactor 1 through the feed port II6. Utilize heating furnace 10 to heat reactor 1, utilize condenser 3 to lower the temperature, make the temperature difference between reactor 1 and condenser 3 be 5~10 ℃, pressure difference be 0.01~0.02MPa, the rectifying tower The water removal rectification temperature is controlled at 70-90°C for rectification. Take out a small amount of hydrogen fluoride from the condenser 3 through the sampling port 9 for analysis. When the water content in the hydrogen fluoride drops below 1ppm, adjust the rectification collection temperature of the rectification tower to 25-35°C and maintain a pressure differe...

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Abstract

The invention relates to a method for removing water in hydrogen fluoride by reactive distillation, and belongs to the field of chemical technology. The method comprises the following steps: tungsten tetrafluoride is added into a reaction vessel, vacuumizing and displacing treatment is carried out for a whole reaction system, liquefied hydrogen fluoride is added into the reaction vessel; the reaction vessel is heated, a condenser is cooled, wherein the temperature difference between the reaction vessel and the condenser is 5-10 DEG C, the pressure difference is 0.01-0.02 MPa, and the de-watering rectification temperature of a distillation tower is controlled within 60-100 DEG C for distillation; a small amount of hydrogen fluoride is taken from the condenser for analysis, when the water content of the hydrogen fluoride reduces below 1 ppm, the distillation collection temperature of the distillation tower is adjusted to 20-40 DEG C, and the pressure difference of 0.01-0.02 MPa is kept, and hydrogen fluoride in the condenser is collected into a low-temperature storing device. According to the method, the de-watering efficiency is high, and the water content of the hydrogen fluoride can be reduced below 1 ppm. The method has the advantages of simple process and operation safety; the impurity is easy to separate, and the method is suitable for industrial production of high purity hydrogen fluoride.

Description

technical field [0001] The invention relates to a method for removing moisture in hydrogen fluoride by reactive distillation, which belongs to the technical field of chemical industry. Background technique [0002] Hydrogen fluoride is a widely used chemical, and its main application fields are as follows: (1) As a raw material for the preparation of fluorine-containing compounds, it is used for the preparation of fluorine salts, fluorine-containing refrigerants, fluorine-containing plastics, fluorine-containing rubber, fluorine-containing resins and Fluorine source for substances such as fluorine-containing medicines or pesticides; (2) as a strong acid etchant for etching glass, pickling metals, and etching semiconductor surfaces; (3) as a catalyst for alkylation reactions; (4) as a Analytical reagent; (5) as cleaning gas. [0003] Industrial hydrogen fluoride is produced by heating reaction of fluorite and sulfuric acid: [0004] CaF 2 +H 2 SO 4 →2HF+CaSO 4 [0005]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B7/19
CPCY02P20/10
Inventor 柳彤李翔宇宋富财郑秋艳胡帅张净普朱文东孙秋丽
Owner PERIC SPECIAL GASES CO LTD
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