Method for purifying hafnium tetrachloride

A purification method and technology of hafnium tetrachloride, applied in the field of purification of hafnium tetrachloride, can solve the problems of harsh production conditions, complicated process operation, low production efficiency, etc. Easy-to-control effects

Pending Publication Date: 2021-04-09
SANXIANG ADVANCED MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The technological process of this method is complicated to operate. In the purification operation, if the number of gas releases is too many, the recovery rate of hafnium tetrachloride will be reduced. If the number of gas releases is too small, impurities cannot be removed, and the product cannot meet the quality standard. 9-11 hours, the production efficiency is low, and the volatilization temperature must be strictly controlled in the later stage of purification to prevent the chloride from volatilizing and re-condensing in hafnium tetrachloride, which requires strict production conditions and high technical difficulty

Method used

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  • Method for purifying hafnium tetrachloride

Examples

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Comparison scheme
Effect test

Embodiment 1

[0033] A method for purifying hafnium tetrachloride, comprising the steps of:

[0034] Step 1. Take 5000kg of crude hafnium tetrachloride with high impurity content and add it to the reaction tank, and simultaneously turn on the stirrer and heating components of the reaction tank.

[0035] Step 2, 1253kg of KCl-NaCl mixed molten salt is added to the reaction tank, wherein sodium chloride is 550kg, and potassium chloride is 700kg; the particle size of the sodium chloride and potassium chloride is 60-100 mesh, and in the mixed molten salt Contains 3kg of zirconium powder.

[0036] Step 3. Raise the temperature of the reaction tank to 270°C-280°C, and open the exhaust valve.

[0037] Step 4. Raise the temperature of the reaction tank to 580°C-590°C, and collect HfCl with a condensation trap 4 , the coagulation time is 30min-45min.

[0038] Step 5. After reducing the temperature of the double salt in the reaction tank to below 300°C, add 5000kg of crude hafnium tetrachloride wi...

Embodiment 2

[0041] A method for purifying hafnium tetrachloride, comprising the steps of:

[0042] Step 1. Take 5500 kg of crude hafnium tetrachloride with high impurity content and add it to the reaction tank, and simultaneously turn on the stirrer and heating components of the reaction tank.

[0043] Step 2, 1378.5kg of KCl-NaCl mixed molten salt is added to the reaction tank, wherein the sodium chloride is 600kg, and the potassium chloride is 775kg; the particle size of the sodium chloride and potassium chloride is 60-100 mesh, and the mixed molten salt Contains 3.5kg of zirconium powder.

[0044] Step 3. Raise the temperature of the reaction tank to 280°C-300°C, and open the exhaust valve.

[0045] Step 4. Raise the temperature of the reaction tank to 590°C-600°C, and collect HfCl with a condensation trap 4 , the coagulation time is 30min-45min.

[0046] Step 5. After reducing the temperature of the double salt in the reaction tank to below 300°C, add 5500kg of crude hafnium tetrac...

Embodiment 3

[0049] A method for purifying hafnium tetrachloride, comprising the steps of:

[0050] Step 1. Take 6000 kg of crude hafnium tetrachloride with high impurity content and add it to the reaction tank, and simultaneously turn on the stirrer and heating components of the reaction tank.

[0051] Step 2, 1505kg of KCl-NaCl mixed molten salt is added to the reaction tank, wherein sodium chloride is 680kg, and potassium chloride is 820kg; the particle size of the sodium chloride and potassium chloride is 60-100 mesh, and in the mixed molten salt Contains 5kg of zirconium powder.

[0052] Step 3. Raise the temperature of the reaction tank to 300°C-320°C, and open the exhaust valve.

[0053] Step 4. Raise the temperature of the reaction tank to 600°C-610°C, and collect HfCl with a condensation trap 4 , The coagulation time is 35min-50min.

[0054] Step 5. After reducing the temperature of the double salt in the reaction tank to below 300°C, add 6000kg of crude hafnium tetrachloride w...

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Abstract

The invention belongs to the technical field of hafnium tetrachloride purification, and particularly relates to a hafnium tetrachloride purification method. The method comprises the following steps: mixing and heating coarse HfCl4 containing impurities and mixed molten salt, which comprises sodium chloride, potassium chloride and zirconium powder; respectively opening at 270-340 DEG C to volatilize and discharge impurities with low boiling points, and opening a condensation catcher at 580-620 DEG C to condense gaseous HfCl4 so as to obtain HfCl4 with high purity; the HfCl4 purification efficiency can be effectively improved, flammable and explosive gas is prevented from being used for purification operation, and the process safety is improved.

Description

technical field [0001] The invention belongs to the technical field of hafnium tetrachloride purification, in particular to a method for purifying hafnium tetrachloride. Background technique [0002] The traditional purification of hafnium tetrachloride is mainly based on the hydrogen purification method, which uses the difference in boiling point and vapor pressure between hafnium tetrachloride and impurity chlorides to separate it through low-temperature degassing, hydrogen-filled reduction, and high-temperature degassing. The technological process of this method is complicated to operate. In the purification operation, if the number of gas releases is too many, the recovery rate of hafnium tetrachloride will be reduced. If the number of gas releases is too small, impurities cannot be removed, and the product cannot meet the quality standard. 9-11 hours, the production efficiency is low, and the volatilization temperature must be strictly controlled in the later stage of p...

Claims

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Application Information

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IPC IPC(8): C01G27/04
CPCC01G27/04C01P2006/80
Inventor 杨强文叶旦旺魏爽史鑫吴鸿霖
Owner SANXIANG ADVANCED MATERIALS
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