CN1096058A - The smelting process of special metallic arsenic - Google Patents
The smelting process of special metallic arsenic Download PDFInfo
- Publication number
- CN1096058A CN1096058A CN 93115598 CN93115598A CN1096058A CN 1096058 A CN1096058 A CN 1096058A CN 93115598 CN93115598 CN 93115598 CN 93115598 A CN93115598 A CN 93115598A CN 1096058 A CN1096058 A CN 1096058A
- Authority
- CN
- China
- Prior art keywords
- arsenic
- metallic
- pure metal
- vacuum
- low
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 33
- LULLIKNODDLMDQ-UHFFFAOYSA-N arsenic(3+) Chemical compound [As+3] LULLIKNODDLMDQ-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000003723 Smelting Methods 0.000 title description 4
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 25
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 20
- 239000012535 impurity Substances 0.000 claims abstract description 17
- GOLCXWYRSKYTSP-UHFFFAOYSA-N arsenic trioxide Inorganic materials O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 claims abstract description 15
- IKWTVSLWAPBBKU-UHFFFAOYSA-N a1010_sial Chemical compound O=[As]O[As]=O IKWTVSLWAPBBKU-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229960002594 arsenic trioxide Drugs 0.000 claims abstract description 14
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 10
- 238000004821 distillation Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000002061 vacuum sublimation Methods 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000859 sublimation Methods 0.000 claims description 3
- 230000008022 sublimation Effects 0.000 claims description 3
- 238000005660 chlorination reaction Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 241001417490 Sillaginidae Species 0.000 abstract 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 abstract 1
- 229910001950 potassium oxide Inorganic materials 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 3
- 238000012797 qualification Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- 229940086984 trisenox Drugs 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
A kind of is raw material with the Potassium oxide, smelts the method for low assorted metallic arsenic or high pure metal arsenic.It adopts the vacuum-sublimation method to remove impurities in raw materials earlier, particularly remove Sb and Bi, vacuum tightness is 0.093～0.1013MPa in its subliming furnace, temperature is 300～400 ℃, prepare low assorted white arsenic or high-purity arsenic trioxide, lower assorted metallic arsenic of reduction with carbon or chlorination-hydro-reduction production or high pure metal arsenic.This method is simpler than chlorination-distillation method impurity removal process, and cost is low, the production capacity height, and environmental pollution is little, and can produce has the different special metallic arsenics that require to foreign matter content.
Description
The present invention relates to the white arsenic is the method that raw material is smelted special metallic arsenic.
As everyone knows,, especially smelt special metallic arsenic at metal smelting arsenic, such as: in the process of the high pure metal arsenic of semiconductor industry, the removal of the impurity that metallic impurity, particularly Sb, Bi etc. are close with arsenic character is a problem that difficulty is bigger.At present, domestic is raw material with the white arsenic, and the metallic arsenic that the reduction with carbon method is produced contains As and reaches 99%, contains sb0.4%, and Bi is 0.1%.SUMITOMO CHEMICAL metal mine company (SMM) adopts Wet-process metallurgy method to produce high-purity arsenic trioxide earlier for producing high pure metal arsenic, and product contains As
2O
3Reach 99.9%, containing sb still is 0.011%.Therefore, with above-mentioned metallic arsenic or trisenox produce low assorted or high pure metal arsenic before, all also must be with impurity such as the removal of chlorination-distillation (repeatedly) method Sb, Bi.According to the U.S.'s academic annual meeting data report of international arsenic in 1988, SUMITOMO CHEMICAL metal mine company adopts following method: with As with the 7N level metallic arsenic of the high-purity arsenic trioxide production semiconductor industry of above-mentioned wet production
2O
3With the HCl dissolving, be converted into AsCl
3; Remove the muriate of heavy metal, alkali and impurity such as alkaline-earth metal and silicon by successive distillation, fractionation and rectifying, realize AsCl
3Purification because SbCl
3With AsCl
3Vapour pressure very approaching, only could be separated in stage of rectification; AsCl after the purification
3The hydrogen reducing that purifies with the palladium film becomes metallic arsenic; The metallic arsenic resublime further removes matter matter such as carbon elimination, thereby obtain high pure metal arsenic (" mountain, mouth of a river science and technology " the 2nd～3 phase in 1993 of 7N level, " metallurgical basis of arsenic and application " selects special edition, and 75-81 page or leaf, original text are deposited the Zhongnan Polytechnic Univ Library, money item number 197187) chlorination-distillation method is separated arsenic and impurity such as Sb, Bi, although can obtain good impurity-eliminating effect, there is complex process, the production cost height, problems such as throughput is low, and the environmental improvement difficulty is big.
The objective of the invention is in order to overcome the weak point of above-mentioned chlorination-distillation method removal of impurities, provide that a kind of technology is simple, cost is low, environmental improvement is easy, pollute little, and output height, and make arsenic and the fine separation processes of impurity such as Sb, Bi, thereby provide a kind of production low assorted metallic arsenic, until the new process of high pure metal arsenic.
For achieving the above object, the present invention adopts the vacuum-sublimation method to remove impurity, particularly Sb and Bi in the white arsenic, prepares high-purity arsenic trioxide, and reduction with carbon method is again produced low assorted metallic arsenic, or produces high pure metal arsenic with chlorination-hydrogen reduction method again.
Principle of the present invention is utilize the sublimation temperature of various metal oxides and vapour pressure different, temperature and vacuum tightness by the control subliming furnace, make the white arsenic distillation, other metal chloride then remains in the end slag, and reaches arsenic and the isolating purpose of other metallic impurity.
Vacuum-sublimation method of the present invention, vacuum degree control is in 0.0933～0.1013MPa(MPa), sublimation temperature is 300～400 ℃.
Technological process of the present invention is that the raw material white arsenic is added in the distillation electric furnace of control automatically, give earlier and heating, treat to vacuumize again after water evaporates in the material is done, make in the subliming furnace vacuum tightness reach 0.0933～0.1013MPa(700～760mmHg), temperature is controlled at 300～400 ℃, allows As
2O
3Slowly distillation.For improving arsenic and the isolating effect of other metallic impurity, generally adopt controlled repeatedly vacuum-sublimation, and successively the last time is distilled after the As that condensation obtains
2O
3, distil again, up to the As that obtains next time
2O
3Middle foreign matter content reaches the requirement of producing special metallic arsenic.With the low assorted As that obtains after the vacuum-sublimation
2O
3Send in the line frequency furnace that adopts carbon reduction method metal smelting arsenic, can produce the low special metallic arsenics of impurity such as containing Sb, Bi, such as the metallic arsenic that contains sb＜50PPM(0.005%), Bi＜40PPM(0.004%).High-purity As with the back acquisition that repeatedly distils
2O
3With getting AsCl behind hydrogen chloride gas chlorination, the separatory
3, use hydrogen reducing AsCl then
3, promptly adopt chlorination-hydrogen reduction method can produce 19 kinds of total impurities＜1 * 10 such as containing Sb, Bi, S, Pb, Cu, Zn, K, Na, Ca, Fe
-6High pure metal arsenic, wherein: Sb＜5 * 10-7, Bi＜5 * 10
-9, S＜7 * 10
-8, and the high pure metal arsenic of producing with the inventive method carbon containing not basically, be particularly conducive to semi-conductor industry and use.
The technical qualification and the index of embodiments of the invention are listed in table 1, and wherein embodiment 1～3, are the low assorted As that produces with the inventive method
2O
3Be raw material, the reduction with carbon method is produced low assorted metallic arsenic, and embodiment 4～5th, with high-purity As of the inventive method production
2O
3Be raw material, produce high pure metal arsenic with chlorination-hydrogen reduction method.
The present invention adopts metallic impurity, particularly Sb and the Bi in the vacuum-sublimation method separate arsenic trioxide, and technology is simple, cost is low, the production capacity height, and environmental pollution is little, and operation control flexibly, can satisfy and produce the needs that foreign matter content had the different special metallic arsenics that require.
The technical qualification of the embodiment of the invention and index table one
| Embodiment condition and index | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| 1, raw material | |||||
| As 2O 3% | 96.75 | 97.84 | 97.15 | 97.5 | 97.4 |
| Sb% | 0.18 | 0.16 | 0.25 | 0.20 | 0.19 |
| Bi% | 0.1 | 0.09 | 0.12 | 0.09 | 0.1 |
| 2, vacuum-sublimation technical qualification | |||||
| Temperature ℃ | 310 | 400 | 350 | 315 | 300 |
| Vacuum tightness MPa | 0.0933 | 0.100 | 0.0987 | 0.1007 | 0.1013 |
| 3, the As after the distillation 2O 3Technical indicator | |||||
| As 2O 3% | 99.96 | 99.95 | 99.95 | 99.9999 | 99.9999 |
| Sb% | 0.0045 | 0.0038 | 0.0047 | 4×10 -5 | 5×10 -5 |
| Bi% | 0.0039 | 0.0035 | 0.004 | 5×10 -7 | 4.5×10 -7 |
| 4, special metallic arsenic technical indicator | |||||
| As% | 99.90 | 99.91 | 99.90 | 99.9999 | 99.9999 |
| Sb% | 0.0048 | 0.0042 | 0.0048 | 4×10 -5 | 5×10 -5 |
| Bi% | 0.0041 | 0.0039 | 0.0041 | 6×10 -7 | 5×10 -7 |
| * 19 kinds of total impurities % | ＜1×10 －4 | ＜1×10 －4 | |||
＊Sb、Bi、S、Mn、Fe、Al、Ca、Zn、Pb、Cr、Cu、Cd、Ag、Co、Ni、Te、Se、K、Na
Claims (3)
1, a kind of with impure height, particularly containing the high white arsenic of Sb, Bi is raw material, the reduction with carbon method is produced low assorted metallic arsenic, or with the method that chlorination-hydrogen reduction method is produced high pure metal arsenic, it is characterized in that adopting the vacuum-sublimation method to remove impurities in raw materials earlier, particularly remove Sb and Bi, prepare low assorted or high-purity arsenic trioxide, reduction with carbon again, or the low assorted metallic arsenic of chlorination one hydrogen reduction method production, or high pure metal arsenic.
2, the low assorted metallic arsenic of production according to claim 1, or the method for high pure metal arsenic, the vacuum tightness when it is characterized in that vacuum-sublimation three oxidations two periodicals is 0.0933～0.1013MPa, sublimation temperature is 300～400 ℃.
3, the low foreign metal arsenic of production according to claim 1, or the method for high pure metal arsenic, after it is characterized in that white arsenic put into the distillation electric furnace, Ying Xianyu heats, treat that water evaporates is done in the material after, vacuumize beginning vacuum-sublimation operation again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93115598 CN1030842C (en) | 1993-12-02 | 1993-12-02 | Smelting method of special metal arsenic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93115598 CN1030842C (en) | 1993-12-02 | 1993-12-02 | Smelting method of special metal arsenic |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1096058A true CN1096058A (en) | 1994-12-07 |
| CN1030842C CN1030842C (en) | 1996-01-31 |
Family
ID=4991167
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93115598 Expired - Fee Related CN1030842C (en) | 1993-12-02 | 1993-12-02 | Smelting method of special metal arsenic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1030842C (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004035846A1 (en) * | 2002-10-17 | 2004-04-29 | Beijing Goldtech Co., Ltd | The non-pollution process of extracting arsenic in vacuum and the equipment thereof |
| CN101144125B (en) * | 2006-09-11 | 2010-05-12 | 昆明鸿世达高技术材料有限责任公司 | Industrialized producing method for high-purity arsenic |
| CN101921921A (en) * | 2010-08-19 | 2010-12-22 | 云南锡业集团（控股）有限责任公司 | Method for treating arsenic-containing material by using electric arc furnace |
| CN102002604A (en) * | 2010-12-17 | 2011-04-06 | 扬州高能新材料有限公司 | Metal arsenic reformer |
| CN102002603A (en) * | 2010-12-17 | 2011-04-06 | 扬州高能新材料有限公司 | Large arsenide reduction furnace |
| CN102321813A (en) * | 2011-09-30 | 2012-01-18 | 昆明理工大学 | Method for preparing raw arsenic by vacuum carbon thermal reduction of arsenic trioxide |
| CN107043862A (en) * | 2017-03-24 | 2017-08-15 | 中南大学 | A kind of As2O3The method that reduction prepares metallic arsenic |
| CN107881351A (en) * | 2017-11-30 | 2018-04-06 | 广东先导先进材料股份有限公司 | The device for deoxidizing and method of high purity arsenic |
| CN110144463A (en) * | 2019-05-21 | 2019-08-20 | 铜仁学院 | A method for resource utilization of arsenic and calcium slag |
| CN110819810A (en) * | 2019-11-21 | 2020-02-21 | 株洲冶炼集团股份有限公司 | Comprehensive recovery method for purifying cobalt-nickel slag by zinc hydrometallurgy arsenic salt |
| CN116445741A (en) * | 2023-03-16 | 2023-07-18 | 中南大学 | A method for arsenic purification |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225479B (en) * | 2008-01-25 | 2010-06-02 | 郑桂昌 | A vacuum sublimation purification method for high-purity arsenic and its vacuum sublimation furnace |
-
1993
- 1993-12-02 CN CN 93115598 patent/CN1030842C/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004035846A1 (en) * | 2002-10-17 | 2004-04-29 | Beijing Goldtech Co., Ltd | The non-pollution process of extracting arsenic in vacuum and the equipment thereof |
| RU2293130C2 (en) * | 2002-10-17 | 2007-02-10 | Бейджин Голдтек Ко., Лтд. | Arsenic vacuum extraction method without contamination of environment and equipment for preforming the same |
| US7534389B2 (en) | 2002-10-17 | 2009-05-19 | Beijing Goldtech Co., Ltd. | Apparatus and process for extracting arsenic in vacuum |
| CN101144125B (en) * | 2006-09-11 | 2010-05-12 | 昆明鸿世达高技术材料有限责任公司 | Industrialized producing method for high-purity arsenic |
| CN101921921A (en) * | 2010-08-19 | 2010-12-22 | 云南锡业集团（控股）有限责任公司 | Method for treating arsenic-containing material by using electric arc furnace |
| CN102002603A (en) * | 2010-12-17 | 2011-04-06 | 扬州高能新材料有限公司 | Large arsenide reduction furnace |
| CN102002604A (en) * | 2010-12-17 | 2011-04-06 | 扬州高能新材料有限公司 | Metal arsenic reformer |
| CN102002604B (en) * | 2010-12-17 | 2012-07-04 | 扬州高能新材料有限公司 | Metal arsenic reformer |
| CN102321813A (en) * | 2011-09-30 | 2012-01-18 | 昆明理工大学 | Method for preparing raw arsenic by vacuum carbon thermal reduction of arsenic trioxide |
| CN107043862A (en) * | 2017-03-24 | 2017-08-15 | 中南大学 | A kind of As2O3The method that reduction prepares metallic arsenic |
| CN107043862B (en) * | 2017-03-24 | 2019-07-12 | 中南大学 | A kind of As2O3The method that reduction prepares metallic arsenic |
| CN107881351A (en) * | 2017-11-30 | 2018-04-06 | 广东先导先进材料股份有限公司 | The device for deoxidizing and method of high purity arsenic |
| CN110144463A (en) * | 2019-05-21 | 2019-08-20 | 铜仁学院 | A method for resource utilization of arsenic and calcium slag |
| CN110819810A (en) * | 2019-11-21 | 2020-02-21 | 株洲冶炼集团股份有限公司 | Comprehensive recovery method for purifying cobalt-nickel slag by zinc hydrometallurgy arsenic salt |
| CN116445741A (en) * | 2023-03-16 | 2023-07-18 | 中南大学 | A method for arsenic purification |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1030842C (en) | 1996-01-31 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| CI01 | Correction of invention patent gazette |
Correction item: Abstract Correct: arsenic trioxide False: Three, two potassium oxide Number: 49 Page: 60 Volume: 10 |
|
| ERR | Gazette correction |
Free format text: CORRECT: ABSTRACT; FROM: POTASSIUM OXIDE TO: ARSENIC OXIDE |
|
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| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |