CN1072963A - The preparation method of low-arsenic pure antimony - Google Patents
The preparation method of low-arsenic pure antimony Download PDFInfo
- Publication number
- CN1072963A CN1072963A CN 91110963 CN91110963A CN1072963A CN 1072963 A CN1072963 A CN 1072963A CN 91110963 CN91110963 CN 91110963 CN 91110963 A CN91110963 A CN 91110963A CN 1072963 A CN1072963 A CN 1072963A
- Authority
- CN
- China
- Prior art keywords
- antimony
- arsenic
- low
- plumbago crucible
- preparation
- 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.)
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- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 42
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052785 arsenic Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000010439 graphite Substances 0.000 claims abstract description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 241000196324 Embryophyta Species 0.000 claims abstract description 6
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 6
- 241000209456 Plumbago Species 0.000 claims description 13
- 229910000831 Steel Inorganic materials 0.000 claims description 8
- 239000010959 steel Substances 0.000 claims description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- MKOYQDCOZXHZSO-UHFFFAOYSA-N [Cu].[Cu].[Cu].[As] Chemical compound [Cu].[Cu].[Cu].[As] MKOYQDCOZXHZSO-UHFFFAOYSA-N 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 235000017550 sodium carbonate Nutrition 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- DLISVFCFLGSHAB-UHFFFAOYSA-N antimony arsenic Chemical compound [As].[Sb] DLISVFCFLGSHAB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052753 mercury Inorganic materials 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 13
- 239000005864 Sulphur Substances 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 11
- 239000012535 impurity Substances 0.000 abstract description 7
- 238000011084 recovery Methods 0.000 abstract description 3
- 240000003936 Plumbago auriculata Species 0.000 abstract 1
- 239000003513 alkali Substances 0.000 abstract 1
- 238000009835 boiling Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 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
- 238000004458 analytical method Methods 0.000 description 1
- 230000031709 bromination Effects 0.000 description 1
- 238000005893 bromination reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of preparation method of low-arsenic pure antimony, be characterized in that raw material is put into crucible at high temperature to be added the alkali boiling sulphur removal and fall arsenic, carry out vacuum distilling with vacuum distillation plant then, place copper wire on the screen tray on the plumbago crucible in vacuum distillation plant, make that arsenic is further separated in the antimony when vacuum distilling is volatilized.The advantage of present method is that processing charges is low, is to produce 1/10 of high purity antimony method, and the rate of recovery can reach 87%, and the main grade of antimony will reach 99.99-99.998%, and arsenic impurities can be reduced to below the 10ppm, and sulphur impurity can be reduced to 2ppm.
Description
The present invention relates to a kind of preparation method's of metallic antimony, particularly a kind of low-arsenic pure antimony preparation method.
In recent years, states such as Japan, Britain, Australia, South Korea seek a kind of new type of metal antimony product in the international market, requiring the main grade of antimony is more than 99.99%, wherein arsenic impurities must be lower than 10ppm, and the content of sulphur must be lower than 2ppm, and price must be suitable.This requirement is a difficult problem to present antimony industry.There are some to reduce the method for arsenic, sulphur in the existing antimony industrial manufacture process, as the fused-salt electrolytic refining cathode method, add composite fluxing agent electric furnace refining method and add aluminium melting arsenic removal method etc., yet these methods, the limit degree that arsenic, sulphur in the antimony reduce also can only be reduced to 100ppm, 20ppm respectively, all exceed 10 times of requirement, simultaneously, the grade of the metallic antimony that these kinds processing method is produced is the highest also can only to reach 99.98%, this shows that the preparation method of above-mentioned metallic antimony all can not satisfy external user's requirement.
If simple consider with the arsenic in the antimony, sulphur content do not reduce to 10ppm, below the 2ppm, can adopt a kind of method of producing high purity antimony, be bromination rectifying, hydrogen reducing technology, through this technology, the main grade of antimony can reach more than 99.999%, and arsenic, sulphur impurity can be reduced to below the 1-2ppm, yet through this technology, processing charges exceeds more than 10 times than the receptible price of external user, and yields poorly, and can't satisfy industrial production requirement.
In view of the foregoing, the object of the present invention is to provide that a kind of processing charges is low, the rate of recovery is high, and the main grade of antimony is reached more than 99.995%, arsenic, sulphur impurity can be reduced to the preparation method of the low-arsenic pure antimony of 10-2ppm.
The object of the present invention is achieved like this: raw material antimony is put into plumbago crucible, add the yellow soda ash that accounts for the heavy 15-20% of raw material, the electric furnace heating, temperature is controlled at 900-950 ℃, after fully stirring, cool the temperature to 750-800 ℃, leave standstill, alkaline residue is clawed, ingot casting, at this moment, the content of sulphur can be reduced to 2ppm, the content of arsenic also can be reduced to below the 100ppm, then will be through the antimony slab of preceding operation by the steel pipe stove, plumbago crucible, add in the vacuum distillation plant that electrothermal stove and molybdenum sheet sleeve constitute and carry out vacuum distilling, be about to antimony slab and put into plumbago crucible, on plumbago crucible, put a screen tray, put suitable antimony slab material on this screen tray and weigh 3/1000ths to 7/1000ths copper wire, make in the antimony arsenic when volatile matter distillation and the reaction of the copper on the screen tray, produce copper arsenide, thereby arsenic in the antimony is separated, the antimony that distills is condensate on the molybdenum sheet sleeve, and takes off from it, obtains low-arsenic pure antimony with this.
Advantage of the present invention is: processing charges is low, is 1/10 of the high purity antimony method of producing at present, and the rate of recovery can reach 87%, and the main grade of antimony can reach 99.99-99.998%, arsenic impurities can be reduced to below the 10ppm, and sulphur impurity can be reduced to 2ppm, can satisfy external user's requirement fully.
Detail of the present invention is provided by following embodiment:
Fig. 1 is the structural representation of vacuum distillation plant among the present invention.
Concrete working method of the present invention is: raw material antimony is put into plumbago crucible, adding accounts for raw material and weighs 15% yellow soda ash, the electric furnace heating, temperature is controlled at 900 ℃, fully stir after 3-4 hour and cool the temperature to 750 ℃, left standstill 40 minutes, alkaline residue is clawed, ingot casting, sampling analysis sulphur and arsenic, at this moment, the content of sulphur is below the 2ppm, and the content of arsenic is below the 100ppm, carry out vacuum distilling with the vacuum distillation plant (see figure 1) then, this equipment is by plumbago crucible 5, add electrothermal stove 7, steel pipe stove 1, molybdenum sheet sleeve 2 and screen tray 4,8 constitute, and the bottom of steel pipe stove 1 places and adds electrothermal stove 7, and plumbago crucible 5 places the bottom of steel pipe stove 1, place on the plumbago crucible 5 by two screen traies 4 up and down, the molybdenum sheet sleeve 2 of 8 clampings, sequence number 9 is a steel pipe stove evacuation mouth among the figure.When carrying out vacuum distilling, will put into plumbago crucible 5 through the antimony slab material 6 after arsenic falls in high temperature refining sulphur removal, on the screen tray on this crucible 4, place suitable antimony slab material and weigh 5/1000ths copper wire 3, in that being vacuumized, steel pipe stove 1 reaches 5 * 10
-3-1 * 10
-4When millimeter mercury is high, add electrothermal stove 7 energising heating, temperature reaches 780-810 ℃ (being preferably in 780 ℃), made its constant temperature 1.5-2.5 hour in crucible, copper wire 3 reactions during volatile matter distillation and on the screen tray 4, generate copper arsenide, thereby arsenic in the antimony is reduced to below the 10ppm, and the purity of its antimony can reach more than 99.995%.
Claims (2)
1, a kind of preparation method of low-arsenic pure antimony, it is characterized in that: raw material antimony is put into plumbago crucible, add the yellow soda ash that accounts for the heavy 15-20% of raw material, the electric furnace heating, temperature is controlled at 900-950 ℃, after fully stirring, cool the temperature to 750-800 ℃, leave standstill, alkaline residue is clawed, ingot casting is then by the steel pipe stove, plumbago crucible, add in the vacuum distillation plant that electrothermal stove and molybdenum sheet sleeve constitute and carry out vacuum distilling, be about to antimony slab and put into plumbago crucible, on plumbago crucible, put a screen tray, put suitable antimony slab material on this screen tray and weigh 3/1000ths to 7/1000ths copper wire, make in the antimony arsenic when volatile matter distillation and the reaction of the copper on the screen tray, produce copper arsenide, thereby arsenic in the antimony is separated, the antimony that distills is condensate on the molybdenum sheet sleeve, and takes off from it, promptly makes low-arsenic pure antimony.
2, the preparation method of low-arsenic pure antimony according to claim 1 is characterized in that: reach 5 * 10 at the steel pipe stove evacuation
-3-1 * 10
-4When millimeter mercury is high, add electrothermal stove energising heating, temperature reaches 780-810 ℃ in crucible, makes its constant temperature 1.5-2.5 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91110963 CN1072963A (en) | 1991-12-03 | 1991-12-03 | The preparation method of low-arsenic pure antimony |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91110963 CN1072963A (en) | 1991-12-03 | 1991-12-03 | The preparation method of low-arsenic pure antimony |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1072963A true CN1072963A (en) | 1993-06-09 |
Family
ID=4910374
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91110963 Pending CN1072963A (en) | 1991-12-03 | 1991-12-03 | The preparation method of low-arsenic pure antimony |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1072963A (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1051581C (en) * | 1997-07-18 | 2000-04-19 | 孔祥成 | Method and device for preparing stibic white with jamesonite |
| CN1295365C (en) * | 2005-04-30 | 2007-01-17 | 云南省通海大方科技有限公司 | Vacuum recrystallization method for purifying metallic antimony and equipment thereof |
| CN102251126A (en) * | 2011-07-11 | 2011-11-23 | 昆明理工大学 | Method for removing arsenic impurities from tin |
| CN103184353A (en) * | 2011-12-29 | 2013-07-03 | 广东先导稀材股份有限公司 | Preparation method of high-purity antimony |
| CN103526049A (en) * | 2013-10-30 | 2014-01-22 | 四川鑫龙碲业科技开发有限责任公司 | Arsenic removal method used in pyrometallurgucal process for antimony |
| CN103572074A (en) * | 2012-08-02 | 2014-02-12 | 湖南东港锑品有限公司 | Method for treating arsenic in high-arsenic raw antimony by reflecting furnace |
| CN103614567A (en) * | 2013-11-20 | 2014-03-05 | 上海申和热磁电子有限公司 | Vacuum distillation material discharge method |
| CN104561567A (en) * | 2014-12-10 | 2015-04-29 | 昆明理工大学 | High-arsenic antimony alloy dearsenication method by vacuum distillation |
| CN104561605A (en) * | 2015-01-22 | 2015-04-29 | 兰州有色冶金设计研究院有限公司 | Device and method for treating antimony-arsenic materials |
| CN106591588A (en) * | 2017-01-10 | 2017-04-26 | 峨眉山市元素新材料科技有限公司 | Vacuum distillation device for preparing 6N indium |
| CN106756110A (en) * | 2016-12-15 | 2017-05-31 | 衡阳华砷科技有限公司 | A kind of antimony material method of purification based on arsenic distillation |
| CN108130450A (en) * | 2018-02-05 | 2018-06-08 | 南通鑫祥锌业有限公司 | A kind of alloy zinc belt and preparation method thereof |
| CN109055768A (en) * | 2018-02-24 | 2018-12-21 | 虔东稀土集团股份有限公司 | A method of it preparing the vacuum drying oven of High purity samarium metal and its prepares High purity samarium metal |
| CN116751991A (en) * | 2023-06-20 | 2023-09-15 | 成都中建材光电材料有限公司 | A kind of production method of low arsenic metal antimony |
-
1991
- 1991-12-03 CN CN 91110963 patent/CN1072963A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1051581C (en) * | 1997-07-18 | 2000-04-19 | 孔祥成 | Method and device for preparing stibic white with jamesonite |
| CN1295365C (en) * | 2005-04-30 | 2007-01-17 | 云南省通海大方科技有限公司 | Vacuum recrystallization method for purifying metallic antimony and equipment thereof |
| CN102251126A (en) * | 2011-07-11 | 2011-11-23 | 昆明理工大学 | Method for removing arsenic impurities from tin |
| CN103184353A (en) * | 2011-12-29 | 2013-07-03 | 广东先导稀材股份有限公司 | Preparation method of high-purity antimony |
| CN103572074A (en) * | 2012-08-02 | 2014-02-12 | 湖南东港锑品有限公司 | Method for treating arsenic in high-arsenic raw antimony by reflecting furnace |
| CN103526049A (en) * | 2013-10-30 | 2014-01-22 | 四川鑫龙碲业科技开发有限责任公司 | Arsenic removal method used in pyrometallurgucal process for antimony |
| CN103614567B (en) * | 2013-11-20 | 2017-03-15 | 上海申和热磁电子有限公司 | Vacuum distilling material method for fetching |
| CN103614567A (en) * | 2013-11-20 | 2014-03-05 | 上海申和热磁电子有限公司 | Vacuum distillation material discharge method |
| CN104561567A (en) * | 2014-12-10 | 2015-04-29 | 昆明理工大学 | High-arsenic antimony alloy dearsenication method by vacuum distillation |
| CN104561605A (en) * | 2015-01-22 | 2015-04-29 | 兰州有色冶金设计研究院有限公司 | Device and method for treating antimony-arsenic materials |
| CN104561605B (en) * | 2015-01-22 | 2016-06-15 | 兰州有色冶金设计研究院有限公司 | A kind of device processing antimony arsenic material |
| CN106756110A (en) * | 2016-12-15 | 2017-05-31 | 衡阳华砷科技有限公司 | A kind of antimony material method of purification based on arsenic distillation |
| CN106591588A (en) * | 2017-01-10 | 2017-04-26 | 峨眉山市元素新材料科技有限公司 | Vacuum distillation device for preparing 6N indium |
| CN108130450A (en) * | 2018-02-05 | 2018-06-08 | 南通鑫祥锌业有限公司 | A kind of alloy zinc belt and preparation method thereof |
| CN109055768A (en) * | 2018-02-24 | 2018-12-21 | 虔东稀土集团股份有限公司 | A method of it preparing the vacuum drying oven of High purity samarium metal and its prepares High purity samarium metal |
| CN116751991A (en) * | 2023-06-20 | 2023-09-15 | 成都中建材光电材料有限公司 | A kind of production method of low arsenic metal antimony |
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| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |