CN113355651A - Gas phase preparation method of anhydrous aluminum fluoride - Google Patents
Gas phase preparation method of anhydrous aluminum fluoride Download PDFInfo
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- CN113355651A CN113355651A CN202110547671.XA CN202110547671A CN113355651A CN 113355651 A CN113355651 A CN 113355651A CN 202110547671 A CN202110547671 A CN 202110547671A CN 113355651 A CN113355651 A CN 113355651A
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- CN
- China
- Prior art keywords
- gas
- carrier gas
- aluminum fluoride
- silicon tetrafluoride
- aluminum chloride
- Prior art date
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- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 title claims abstract description 33
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000007789 gas Substances 0.000 claims abstract description 57
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 48
- 239000012159 carrier gas Substances 0.000 claims abstract description 40
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 6
- 238000007740 vapor deposition Methods 0.000 claims abstract description 3
- 238000005019 vapor deposition process Methods 0.000 claims abstract description 3
- 239000012071 phase Substances 0.000 claims 2
- 239000012808 vapor phase Substances 0.000 claims 2
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 4
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 3
- 238000005234 chemical deposition Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000010436 fluorite Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 229910001610 cryolite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/50—Fluorides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
Abstract
The invention relates to a preparation method of anhydrous aluminum fluoride, which is characterized in that aluminum fluoride is prepared by carrying aluminum chloride gas and silicon tetrafluoride gas by a carrier gas through a plasma vapor deposition method. The carrier gas is nitrogen or argon, and the purity of the nitrogen or the argon is more than 99.999 percent. The radio frequency power of the aluminum chloride gas entering the cavity in the vapor deposition process of the carrier gas and the silicon tetrafluoride gas through the carrier gas is 350-450W, the radio frequency is 12-16MHz, the temperature is 250-350 ℃, and the pressure of the cavity is 100-160 Pa. The gas flow rate of the aluminum chloride gas through the carrier gas is 150-180sccm, and the gas flow rate of the silicon tetrafluoride gas through the carrier gas is 100-130 sccm. In the preparation method, the raw materials of aluminum chloride and silicon tetrafluoride exist in a gas form, so that the method for preparing aluminum fluoride through gas-gas reaction improves the product quality.
Description
Technical Field
The invention relates to a gas phase preparation method of anhydrous aluminum fluoride, belonging to the technical field of fluoride.
Background
Aluminum fluoride (AlF3) is a white crystalline powder used primarily in the electrolytic aluminum industry as an additive in cryolite-alumina fused salt electrolysis (Hall-Elux). In addition, the compound can be used as a catalyst in organic synthesis, a cosolvent for ceramics and enamel, a raw material for manufacturing optical glass and artificial cryolite, an inhibitor in an alcohol production process and the like.
The aluminum fluoride products are divided into wet aluminum fluoride, dry aluminum fluoride and anhydrous aluminum fluoride, the wet aluminum fluoride is prepared by the first generation technology introduced from abroad in the 50 th of the 20 th century and is classified as an elimination process; the dry-method aluminum fluoride is mainly obtained by carrying out gas-solid reaction on hydrofluoric acid produced by fluorite and aluminum hydroxide; the anhydrous aluminum fluoride is mainly obtained by reacting anhydrous hydrogen fluoride with aluminum hydroxide; namely, the dry-method aluminum fluoride and the anhydrous aluminum fluoride take anhydrous hydrogen fluoride or hydrous hydrofluoric acid as raw materials, and the production cost is higher. At present, most hydrofluoric acid production is still the fluorite sulfuric acid method, and with the continuous rising of the price of the basic raw material fluorite, the market supply will be seriously influenced in the future. Therefore, the development of new fluorine raw material sources is increased to become the first problem facing the development of the fluorine chemical industry.
In order to solve the above problems, it is necessary to provide a method for preparing anhydrous aluminum fluoride, which is simple in preparation method and easy to operate.
Disclosure of Invention
The invention aims to provide a method for preparing anhydrous aluminum fluoride, which can effectively alleviate the defects of complex preparation method and difficult operation in the prior art.
The technical scheme of the invention is as follows:
a preparation method of anhydrous aluminum fluoride comprises the following steps:
and carrying the aluminum chloride gas by a carrier gas and carrying the silicon tetrafluoride gas by a carrier gas to prepare the aluminum fluoride by a plasma vapor deposition method.
The carrier gas is nitrogen or argon, and the purity of the nitrogen or the argon is more than 99.999 percent.
The radio frequency power of the aluminum chloride gas entering the cavity in the vapor deposition process of the carrier gas and the silicon tetrafluoride gas through the carrier gas is 350-450W, the radio frequency is 12-16MHz, the temperature is 250-350 ℃, and the pressure of the cavity is 100-160 Pa.
The gas flow rate of the aluminum chloride gas through the carrier gas is 150-180sccm, and the gas flow rate of the silicon tetrafluoride gas through the carrier gas is 100-130 sccm.
The volume ratio of the aluminum chloride gas to the carrier gas is 1: 5-10; the volume ratio of the silicon tetrafluoride gas to the carrier gas is 1: 5-10.
The invention provides a plasma enhanced chemical vapor deposition technology for preparing aluminum fluoride, the purity can reach more than 90%, and byproducts are few.
Detailed Description
Example 1
Preparation of aluminium fluoride
The method comprises the steps of replacing air in a plasma chemical deposition chamber in advance by using nitrogen, mixing the air serving as a carrier gas with aluminum chloride gas sublimated at the temperature of 200 ℃, wherein the volume ratio of the carrier gas to the aluminum chloride gas is 5:1, allowing the mixed gas of the carrier gas and the aluminum chloride gas and the mixed gas of the carrier gas and silicon tetrafluoride to enter the chamber for deposition reaction at the radio frequency of 400W, the radio frequency of 13.56MHz, the temperature of 300 ℃ and the cavity pressure of 120Pa for 20min, and allowing the mixed gas of the carrier gas and the aluminum chloride gas to flow at 180sccm and the mixed gas of the carrier gas and the silicon tetrafluoride to flow at 120 sccm. The purity of the obtained product is 98.5 percent by adopting the standard detection of GB/T4292-2017 AF-0.
Example 2
Preparation of aluminium fluoride
The method comprises the steps of replacing air in a plasma chemical deposition chamber in advance by using nitrogen, mixing the air serving as a carrier gas with aluminum chloride gas sublimated at the temperature of 200 ℃, wherein the volume ratio of the carrier gas to the aluminum chloride gas is 5:1, allowing the mixed gas of the carrier gas and the aluminum chloride gas and the mixed gas of the carrier gas and silicon tetrafluoride to enter the chamber for deposition reaction at the radio frequency of 400W, the radio frequency of 13.56MHz, the temperature of 350 ℃ and the cavity pressure of 120Pa for 20min, and allowing the mixed gas of the carrier gas and the aluminum chloride gas to flow at the flow rate of 160sccm and the mixed gas of the carrier gas and the silicon tetrafluoride to flow at the flow rate of 140 sccm. The purity of the aluminum fluoride obtained by the standard detection of GB/T4292-2017 AF-0 is 97.2%.
Example 3
Preparation of aluminium fluoride
The method comprises the steps of replacing air in a plasma chemical deposition chamber in advance by using nitrogen, mixing the air serving as a carrier gas with aluminum chloride gas sublimated at the temperature of 200 ℃, wherein the volume ratio of the carrier gas to the aluminum chloride gas is 5:1, allowing the mixed gas of the carrier gas and the aluminum chloride gas and the mixed gas of the carrier gas and silicon tetrafluoride to enter the chamber for deposition reaction at the radio frequency of 380W, the radio frequency of 13.56MHz, the temperature of 330 ℃ and the cavity pressure of 150Pa for 20min, and allowing the mixed gas of the carrier gas and the aluminum chloride gas to flow at the flow rate of 160sccm and the mixed gas of the carrier gas and the silicon tetrafluoride to flow at the flow rate of 140 sccm. The purity of the obtained product is 96.8 percent by adopting the standard detection of GB/T4292-2017 AF-0.
Claims (5)
1. A gas phase preparation method of anhydrous aluminum fluoride is characterized by comprising the following steps:
and carrying the aluminum chloride gas by a carrier gas and carrying the silicon tetrafluoride gas by a carrier gas to prepare the aluminum fluoride by a plasma vapor deposition method.
2. The process of claim 1 wherein the carrier gas is nitrogen or argon, the purity of the nitrogen or argon being greater than 99.999%.
3. The vapor phase method of producing anhydrous aluminum fluoride according to claim 2, wherein the RF power of the aluminum chloride gas and the RF power of the silicon tetrafluoride gas entering the chamber during the vapor deposition process are 350-450W, the RF frequency is 12-16MHz, the temperature is 250-350 ℃, and the pressure of the chamber is 100-160 Pa.
4. The vapor phase preparation method of anhydrous aluminum fluoride as claimed in claim 3, wherein the gas flow rate of the aluminum chloride gas through the carrier gas is 150-180sccm, and the gas flow rate of the silicon tetrafluoride gas through the carrier gas is 100-130 sccm.
5. The gas-phase preparation method of anhydrous aluminum fluoride according to claim 4, wherein the volume ratio of the aluminum chloride gas to the carrier gas is 1:5 to 10; the volume ratio of the silicon tetrafluoride gas to the carrier gas is 1: 5-10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110547671.XA CN113355651A (en) | 2021-05-19 | 2021-05-19 | Gas phase preparation method of anhydrous aluminum fluoride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110547671.XA CN113355651A (en) | 2021-05-19 | 2021-05-19 | Gas phase preparation method of anhydrous aluminum fluoride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113355651A true CN113355651A (en) | 2021-09-07 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110547671.XA Pending CN113355651A (en) | 2021-05-19 | 2021-05-19 | Gas phase preparation method of anhydrous aluminum fluoride |
Country Status (1)
| Country | Link |
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| CN (1) | CN113355651A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102400000A (en) * | 2011-11-30 | 2012-04-04 | 云南省化工研究院 | Method for preparing aluminium-silicon alloy and aluminium fluoride through reducing silicon tetrafluoride by utilizing aluminium |
| CN110386945A (en) * | 2018-04-18 | 2019-10-29 | 成都先导药物开发股份有限公司 | A kind of big ring class kinase inhibitor |
| CN111943245A (en) * | 2019-05-16 | 2020-11-17 | 多氟多化工股份有限公司 | Method for preparing anhydrous aluminum fluoride |
-
2021
- 2021-05-19 CN CN202110547671.XA patent/CN113355651A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102400000A (en) * | 2011-11-30 | 2012-04-04 | 云南省化工研究院 | Method for preparing aluminium-silicon alloy and aluminium fluoride through reducing silicon tetrafluoride by utilizing aluminium |
| CN110386945A (en) * | 2018-04-18 | 2019-10-29 | 成都先导药物开发股份有限公司 | A kind of big ring class kinase inhibitor |
| CN111943245A (en) * | 2019-05-16 | 2020-11-17 | 多氟多化工股份有限公司 | Method for preparing anhydrous aluminum fluoride |
Non-Patent Citations (1)
| Title |
|---|
| 天津化工研究院: "《无机盐工业手册 上册》", 31 October 1979, 化学工业出版社 * |
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| PB01 | Publication | ||
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| SE01 | Entry into force of request for substantive examination | ||
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210907 |
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| RJ01 | Rejection of invention patent application after publication |