CN112624193B - Purification method of hafnium tetrachloride - Google Patents
Purification method of hafnium tetrachloride Download PDFInfo
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- CN112624193B CN112624193B CN202011618933.9A CN202011618933A CN112624193B CN 112624193 B CN112624193 B CN 112624193B CN 202011618933 A CN202011618933 A CN 202011618933A CN 112624193 B CN112624193 B CN 112624193B
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- hfcl
- molten salt
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- chloride
- hafnium tetrachloride
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- PDPJQWYGJJBYLF-UHFFFAOYSA-J hafnium tetrachloride Chemical compound Cl[Hf](Cl)(Cl)Cl PDPJQWYGJJBYLF-UHFFFAOYSA-J 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000000746 purification Methods 0.000 title claims abstract description 18
- 150000003839 salts Chemical class 0.000 claims abstract description 55
- 239000012535 impurity Substances 0.000 claims abstract description 45
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 42
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 42
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 21
- 239000001103 potassium chloride Substances 0.000 claims abstract description 21
- 239000011780 sodium chloride Substances 0.000 claims abstract description 21
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims description 34
- 238000009833 condensation Methods 0.000 claims description 14
- 230000005494 condensation Effects 0.000 claims description 14
- 230000008018 melting Effects 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 12
- 230000004520 agglutination Effects 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 229910001514 alkali metal chloride Inorganic materials 0.000 claims description 4
- 150000001805 chlorine compounds Chemical class 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 230000002776 aggregation Effects 0.000 claims description 2
- 238000004220 aggregation Methods 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 2
- 230000008020 evaporation Effects 0.000 claims 1
- 238000001704 evaporation Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 10
- 238000009835 boiling Methods 0.000 abstract description 4
- 239000002360 explosive Substances 0.000 abstract description 3
- 238000011403 purification operation Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 229910020549 KCl—NaCl Inorganic materials 0.000 description 4
- 238000010924 continuous production Methods 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G27/00—Compounds of hafnium
- C01G27/04—Halides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to the technical field of hafnium tetrachloride purification, and in particular relates to a purification method of hafnium tetrachloride, which comprises the steps of mixing crude HfCl containing impurities 4 And mixed molten salt, wherein the mixed molten salt comprises sodium chloride, potassium chloride and zirconium powder, and is respectively opened at 270-340 ℃ to volatilize and discharge impurities with lower boiling point, and opened at 580-620 ℃ to condense the trap for gaseous HfCl 4 Condensing to obtain HfCl with higher purity 4 The method comprises the steps of carrying out a first treatment on the surface of the The invention can effectively improve HfCl 4 The purification efficiency of the process is improved, and the purification operation by using flammable and explosive gas is avoided, so that the safety of the process is improved.
Description
Technical Field
The invention belongs to the technical field of hafnium tetrachloride purification, and particularly relates to a purification method of hafnium tetrachloride.
Background
The traditional purification of hafnium tetrachloride is mainly performed by a hydrogen method, and the difference of boiling points and vapor pressures of hafnium tetrachloride and impurity chlorides is utilized to separate the hafnium tetrachloride by low-temperature degassing, hydrogen charging reduction and high-temperature degassing. The method has the advantages that the operation of the technological process is complex, in the purification operation, the recovery rate of hafnium tetrachloride is reduced due to the fact that the number of times of air release is large, impurities cannot be removed due to the fact that the number of times of air release is too small, the quality standard of products cannot be achieved, the single production time is 9-11 hours, the production efficiency is low, the volatilization temperature is strictly controlled in the later purification stage, the volatilization of chlorides is prevented from being condensed in the hafnium tetrachloride again, the requirements on production conditions are severe, and the technical difficulty is high.
Disclosure of Invention
In order to overcome the defects in the prior art, the technical problems to be solved by the invention are as follows: provides a purification method of hafnium tetrachloride with high recovery efficiency and low process difficulty.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for purifying hafnium tetrachloride, comprising the steps of:
step one, crude HfCl containing impurities 4 Respectively adding the mixed molten salt and the molten salt into a molten pool of a reaction tank, and under a sealed environmentStirring and heating to melt to obtain (Na/K) 2 HfCl 4 The temperature of the heating and melting is 270-340 ℃, and the mixed molten salt comprises sodium chloride, potassium chloride and zirconium powder;
wherein, a part of impurities volatilize to generate gaseous impurity chlorides, and the other part of impurities generate impurity alkali metal chloride double salts which are dissolved in a molten pool;
opening an exhaust valve of the reaction tank to discharge the gaseous impurity chloride out of the reaction tank;
step two, when the gaseous impurity chloride is completely discharged from the reaction tank, closing an exhaust valve of the reaction tank, and raising the temperature of the reaction tank for heating and melting to 580-620 ℃ to enable the (Na/K) 2 HfCl 4 Volatilizing to obtain gaseous HfCl 4 ；
Step three, collecting the gaseous HfCl in the step two through a condensation trap 4 Obtaining purified liquid HfCl 4 ；
Wherein, still include the following step:
step four, the temperature of the heating and melting of the reaction tank is reduced to below 300 ℃, and crude HfCl containing impurities is continuously added 4 And the mixed molten salt is arranged in a molten pool of a reaction tank, the heating and melting temperature is increased to 270-340 ℃, and stirring and heating and melting are continuously carried out in a sealed environment, thus obtaining (Na/K) 2 HfCl 4 The gaseous impurity chloride and the impurity alkali metal chloride double salt are used for opening an exhaust valve of the reaction tank, and the gaseous impurity chloride is discharged out of the reaction tank;
step five, repeating the step two to the step four, and continuously collecting the purified liquid HfCl 4 。
In the first step, the mass ratio of sodium chloride to potassium chloride in the mixed molten salt is 1: (1.2-1.5).
Wherein in the first step, the HfCl containing impurities 4 The mass ratio of the molten salt to the mixed molten salt is 4:1.
Wherein in the fourth step, the impurity-containing HfCl 4 The mass ratio of the molten salt to the mixed molten salt is 1: (0.1-0.12).
In the third step, the volatilization and aggregation time of the condensation trap is 30-50min.
In the first or fourth step, the mass percentage of the zirconium powder in the mixed molten salt is 0.2-0.5%.
Wherein, in the mixed molten salt, the content of potassium chloride in the potassium chloride molten salt is more than or equal to 98 percent, and the granularity is 60-100 meshes.
Wherein, in the mixed molten salt, the sodium chloride content in the sodium chloride molten salt is more than or equal to 99 percent, and the granularity is 60-100 meshes.
The reaction tank comprises a tank body, an exhaust valve, a condensation catcher, a stirrer and a heating component;
the tank body is a hollow cylinder, and is made of stainless steel;
the exhaust valve is arranged on the tank body and is communicated with a reaction cavity surrounded by the tank body, and the exhaust valve is used for exhausting the gaseous impurity chloride out of the reaction tank;
the condensation catcher is arranged on the tank body and communicated with the reaction cavity enclosed by the tank body, and is used for collecting gaseous HfCl 4 Agglutination and collection;
the stirrer is arranged in the tank body;
the heating component is connected with a reaction cavity surrounded by the tank body, and the heating component comprises a heating resistance wire.
The invention has the beneficial effects that:
1. melting and stirring the impurities, hafnium tetrachloride and the mixed molten salt by heating together at 270-340 ℃ to obtain TiCl 4 、SiCl 4 The impurities with low boiling point are removed by heating and volatilizing to improve the condensed gaseous HfCl when the subsequent heating is carried out to 580-620 DEG C 4 Is of a purity of (3);
2. accelerating FeCl by adding zirconium powder into mixed molten salt 3 Can absorb chloride ions in a molten pool and reduce corrosion to a reaction tank;
3. in the production process, flammable and explosive gases such as hydrogen are not required to be added, so that the process safety is effectively improved;
4. the materials are not required to be transferred in the production process, the materials are easy to control in the production process, the heating and melting temperature of the reaction tank, the exhaust valve and the condensation catcher are easy to control, the operation is convenient, and the purification efficiency of hafnium tetrachloride is effectively improved.
Detailed Description
In order to describe the technical contents, the achieved objects and effects of the present invention in detail, the following description will be made with reference to the embodiments.
Example 1:
a method for purifying hafnium tetrachloride, comprising the steps of:
step 1, adding 5000kg of crude hafnium tetrachloride with high impurity content into a reaction tank, and simultaneously starting a stirrer and a heating component of the reaction tank.
Step 2, adding 1253kg of KCl-NaCl mixed molten salt into a reaction tank, wherein the sodium chloride is 550kg, and the potassium chloride is 700kg; the granularity of the sodium chloride and the potassium chloride is 60-100 meshes, and 3kg of zirconium powder is contained in the mixed molten salt.
And step 3, raising the temperature of the reaction tank to 270-280 ℃ and opening the exhaust valve.
Step 4, raising the temperature of the reaction tank to 580-590 ℃, and collecting HfCl by a condensation trap 4 The agglutination time is 30min-45min.
And 5, after the temperature of the double salt in the reaction tank is reduced to below 300 ℃, adding 5000kg of crude hafnium tetrachloride with high impurity content, 220kg of NaCl and 280kg of KCl mixed molten salt as supplementary raw materials, wherein the mixed molten salt contains 1.5kg of zirconium powder.
And 6, repeating the heating and condensing processes of the reaction tank to realize continuous production of materials.
Example 2:
a method for purifying hafnium tetrachloride, comprising the steps of:
step 1, adding 5500kg of crude hafnium tetrachloride with high impurity content into a reaction tank, and simultaneously starting a stirrer and a heating component of the reaction tank.
Step 2, adding 1378.5kg of KCl-NaCl mixed molten salt into a reaction tank, wherein the sodium chloride is 600kg, and the potassium chloride is 775kg; the granularity of the sodium chloride and the potassium chloride is 60-100 meshes, and 3.5kg of zirconium powder is contained in the mixed molten salt.
And step 3, raising the temperature of the reaction tank to 280-300 ℃ and opening the exhaust valve.
Step 4, raising the temperature of the reaction tank to 590-600 ℃ and collecting HfCl by a condensation trap 4 The agglutination time is 30min-45min.
And 5, after the temperature of the double salt in the reaction tank is reduced to below 300 ℃, 5500kg of crude hafnium tetrachloride with high impurity content, 250kg of NaCl and 300kg of KCl mixed molten salt as supplementary raw materials are added, wherein the mixed molten salt contains 1.8kg of zirconium powder.
And 6, repeating the heating and condensing processes of the reaction tank to realize continuous production of materials.
Example 3:
a method for purifying hafnium tetrachloride, comprising the steps of:
step 1, adding 6000kg of crude hafnium tetrachloride with high impurity content into a reaction tank, and simultaneously starting a stirrer and a heating component of the reaction tank.
Step 2, adding 1505kg of KCl-NaCl mixed molten salt into a reaction tank, wherein the sodium chloride is 680kg, and the potassium chloride is 820kg; the granularity of the sodium chloride and the potassium chloride is 60-100 meshes, and 5kg of zirconium powder is contained in the mixed molten salt.
And step 3, raising the temperature of the reaction tank to 300-320 ℃ and opening the exhaust valve.
Step 4, raising the temperature of the reaction tank to 600-610 ℃ and collecting HfCl by a condensation trap 4 The agglutination time is 35min-50min.
And 5, after the temperature of the double salt in the reaction tank is reduced to below 300 ℃, adding 6000kg of crude hafnium tetrachloride with more impurity content, 270kg of NaCl and 330kg of KCl mixed molten salt as supplementary raw materials, wherein the mixed molten salt contains 2.1kg of zirconium powder.
And 6, repeating the heating and condensing processes of the reaction tank to realize continuous production of materials.
Example 4:
a method for purifying hafnium tetrachloride, comprising the steps of:
step 1, adding 6500kg of crude hafnium tetrachloride with high impurity content into a reaction tank, and simultaneously starting a stirrer and a heating component of the reaction tank.
Step 2, adding 1630kg of KCl-NaCl mixed molten salt into a reaction tank, wherein the content of sodium chloride is 725kg, and the content of potassium chloride is 900kg; the granularity of the sodium chloride and the potassium chloride is 60-100 meshes, and 5kg of zirconium powder is contained in the mixed molten salt.
And step 3, raising the temperature of the reaction tank to 320-340 ℃ and opening the exhaust valve.
Step 4, raising the temperature of the reaction tank to 610-620 ℃ and collecting HfCl by a condensation trap 4 The agglutination time is 35min-50min.
And 5, after the temperature of the double salt in the reaction tank is reduced to below 300 ℃, 6500kg of crude hafnium tetrachloride with high impurity content, 290kg of NaCl and 360kg of KCl mixed molten salt as supplementary raw materials are added, wherein the mixed molten salt contains 2.4kg of zirconium powder.
And 6, repeating the heating and condensing processes of the reaction tank to realize continuous production of materials.
Detection example:
HfCl before and after purification in examples 1 to 4 4 Impurity analysis (instrument was FMX36, sperk germany) was performed by inductively coupled plasma emission spectrometry, respectively, with the following analysis results:
TABLE 1
As can be seen from the analysis of Table 1, the purification method of hafnium tetrachloride provided by the invention can effectively reduce crude HfCl containing impurities 4 Is a component of the catalyst.
In summary, the invention provides a purification method of hafnium tetrachloride by heating and melting together an alkali metal oxide, hafnium tetrachloride and a mixed molten salt at 270-340 ℃ to stir TiCl 4 、S iCl 4 The impurities with low boiling point are removed by heating and volatilizing to improve the condensed gaseous HfCl when the subsequent heating is carried out to 580-620 DEG C 4 Is of a purity of (3);accelerating FeCl by adding zirconium powder into mixed molten salt 3 Can absorb chloride ions in a molten pool and reduce corrosion to a reaction tank; the process safety is effectively improved without adding flammable and explosive gases such as hydrogen and the like in the production process; the materials are not required to be transferred in the production process, the investment, the melting temperature, the exhaust valve and the condensation catcher of the materials are easy to control in the production process, the operation is convenient, and the purification efficiency of hafnium tetrachloride is effectively improved.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent modifications made by the teachings of the present invention, or direct or indirect application in the relevant art, are intended to be included within the scope of the present invention.
Claims (8)
1. A method for purifying hafnium tetrachloride, comprising the steps of:
step one, crude HfCl containing impurities 4 And the mixed molten salt are respectively added into a molten pool of a reaction tank, stirred and heated to be melted in a sealed environment, thus obtaining (Na/K) 2 HfCl 4 The temperature of the heating and melting is 270-340 ℃, and the mixed molten salt comprises sodium chloride, potassium chloride and zirconium powder;
wherein, a part of impurities volatilize to generate gaseous impurity chlorides, and the other part of impurities generate impurity alkali metal chloride double salts which are dissolved in a molten pool;
opening an exhaust valve of the reaction tank to discharge the gaseous impurity chloride out of the reaction tank;
step two, when the gaseous impurity chloride is completely discharged from the reaction tank, closing an exhaust valve of the reaction tank, and raising the temperature of the reaction tank for heating and melting to 580-620 ℃ to enable the (Na/K) 2 HfCl 4 Volatilizing to obtain gaseous HfCl 4 ；
Step three, collecting the gaseous HfCl in the step two through a condensation trap 4 Obtaining purified liquid HfCl 4 ；
Step four, the temperature of the heating and melting of the reaction tank is reduced to below 300 ℃, and crude Hf containing impurities is continuously addedCl 4 And the mixed molten salt is put in a molten pool of a reaction tank, the heating and melting temperature is increased to 270-340 ℃, and stirring, heating and melting are carried out under a sealed environment continuously, thus obtaining (Na/K) 2 HfCl 4 The gaseous impurity chloride and the impurity alkali metal chloride double salt are used for opening an exhaust valve of the reaction tank, and the gaseous impurity chloride is discharged out of the reaction tank;
step five, repeating the step two to the step four, and continuously collecting the purified liquid HfCl 4 ；
In the first or fourth step, the mass percentage of the zirconium powder in the mixed molten salt is 0.2-0.5%.
2. The purification method of hafnium tetrachloride according to claim 1, wherein in the first step, the mass ratio of sodium chloride to potassium chloride in the mixed molten salt is 1: (1.2-1.5).
3. The method according to claim 1, wherein in the first step, the impurity-containing HfCl 4 The mass ratio of the molten salt to the mixed molten salt is 4:1.
4. The method for purifying hafnium tetrachloride according to claim 1, wherein in the fourth step, the impurity-containing HfCl 4 The mass ratio of the molten salt to the mixed molten salt is 1: (0.1-0.12).
5. The method for purifying hafnium tetrachloride according to claim 1, wherein in the third step, the evaporation and aggregation time of the condensation trap is 30 to 50 minutes.
6. The purification method of hafnium tetrachloride according to claim 1, wherein the potassium chloride content in the potassium chloride molten salt is 98% or more and the particle size is 60 to 100 mesh.
7. The purification method of hafnium tetrachloride according to claim 1, wherein the sodium chloride content in the sodium chloride molten salt is 99% or more and the particle size is 60 to 100 mesh.
8. The method of purifying hafnium tetrachloride according to claim 1, wherein the reaction tank comprises a tank body, a vent valve, a condensation trap, a stirrer, and a heating assembly;
the tank body is a hollow cylinder, and is made of stainless steel;
the exhaust valve is arranged on the tank body and is communicated with a reaction cavity surrounded by the tank body, and the exhaust valve is used for exhausting the gaseous impurity chloride out of the reaction tank;
the condensation catcher is arranged on the tank body and communicated with the reaction cavity enclosed by the tank body, and is used for collecting gaseous HfCl 4 Agglutination and collection;
the stirrer is arranged in the tank body;
the heating component is connected with a reaction cavity surrounded by the tank body, and the heating component comprises a heating resistance wire.
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|---|---|---|---|---|
| CN1993295A (en) * | 2004-07-09 | 2007-07-04 | 欧洲塞扎斯“锆”公司 | Method for separating and purifying hafnium and zirconium |
| CN101638249A (en) * | 2009-09-04 | 2010-02-03 | 石政君 | Zirconium tetrachloride purification method |
| CN208716864U (en) * | 2018-07-16 | 2019-04-09 | 中核晶环锆业有限公司 | A kind of hafnium tetrachloride purifying plant |
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| CN112047378A (en) * | 2020-09-21 | 2020-12-08 | 宝钛华神钛业有限公司 | Zirconium tetrachloride purification method based on hydrogen reduction method |
-
2020
- 2020-12-31 CN CN202011618933.9A patent/CN112624193B/en active Active
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| CN1993295A (en) * | 2004-07-09 | 2007-07-04 | 欧洲塞扎斯“锆”公司 | Method for separating and purifying hafnium and zirconium |
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| CN208716864U (en) * | 2018-07-16 | 2019-04-09 | 中核晶环锆业有限公司 | A kind of hafnium tetrachloride purifying plant |
| CN111994951A (en) * | 2020-09-21 | 2020-11-27 | 宝钛华神钛业有限公司 | Method for recovering hafnium tetrachloride in crude zirconium tetrachloride purification process |
| CN112047378A (en) * | 2020-09-21 | 2020-12-08 | 宝钛华神钛业有限公司 | Zirconium tetrachloride purification method based on hydrogen reduction method |
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| Title |
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