CN106629633A - Method for refining and removing arsenic from precipitated tellurium - Google Patents
Method for refining and removing arsenic from precipitated tellurium Download PDFInfo
- Publication number
- CN106629633A CN106629633A CN201611227386.5A CN201611227386A CN106629633A CN 106629633 A CN106629633 A CN 106629633A CN 201611227386 A CN201611227386 A CN 201611227386A CN 106629633 A CN106629633 A CN 106629633A
- Authority
- CN
- China
- Prior art keywords
- tellurium
- arsenic
- precipitation
- dearsenification
- refined
- 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
- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 62
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 62
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229910052785 arsenic Inorganic materials 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000007670 refining Methods 0.000 title abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 57
- 239000007800 oxidant agent Substances 0.000 claims abstract description 12
- 238000001556 precipitation Methods 0.000 claims description 27
- 239000002893 slag Substances 0.000 claims description 27
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 22
- 230000001590 oxidative effect Effects 0.000 claims description 15
- 235000010344 sodium nitrate Nutrition 0.000 claims description 11
- 239000004317 sodium nitrate Substances 0.000 claims description 11
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims description 3
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims 1
- 229910001948 sodium oxide Inorganic materials 0.000 claims 1
- 238000005266 casting Methods 0.000 abstract description 6
- 238000002844 melting Methods 0.000 abstract description 5
- 230000008018 melting Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- MHUWZNTUIIFHAS-XPWSMXQVSA-N 9-octadecenoic acid 1-[(phosphonoxy)methyl]-1,2-ethanediyl ester Chemical compound CCCCCCCC\C=C\CCCCCCCC(=O)OCC(COP(O)(O)=O)OC(=O)CCCCCCC\C=C\CCCCCCCC MHUWZNTUIIFHAS-XPWSMXQVSA-N 0.000 abstract 1
- 229940047047 sodium arsenate Drugs 0.000 abstract 1
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 description 6
- 239000000155 melt Substances 0.000 description 5
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910001369 Brass Inorganic materials 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000010951 brass Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 1
- 229910003069 TeO2 Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000006256 anode slurry Substances 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 235000012255 calcium oxide Nutrition 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/02—Elemental selenium or tellurium
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for refining and removing arsenic from precipitated tellurium. The method comprises the following steps: melting the precipitated tellurium; adding sodium hydroxide and an oxidizing agent into the molten precipitated tellurium to enable arsenic to form sodium arsenate to enter residues; when the residues float to the surface, fetching the residues; and casting the fetched residues. The method is simple and practical in process, simple and convenient to operate, good in arsenic removal effect and small in tellurium loss, the arsenic can be reduced to be below 0.0005 percent, and products are guaranteed to be qualified.
Description
Technical field
The present invention relates to metal technical field of wet metallurgy, and in particular to a kind of method from refining dearsenification in tellurium is separated out.
Background technology
Tellurium belongs to rare and scatter element, and tellurium and its compound are widely used, and can be used for metallurgical industry production alloy, petrochemical industry system
Standby catalyst, tellurium oxide can be used as novel solar battery critical material as glass colorant, cadmium telluride, and bismuth telluride can use
Make semiconductor and power industry etc..
At present, the country generally adopts the technology that carries out obtaining water logging after water logging by lead anode slurry refinement oxide gained tellurium slag
Slag tap (tellurium leached mud), leachate is purified, neutralize and obtain the very high TeO of purity after calcining2, by TeO2Electricity is carried out after liquid making
Product, negative electrode separates out tellurium and carries out casting mold, can obtain 99.99% smart tellurium.But in process of production when arsenic content overproof in tellurium electrolyte
When, arsenic will be exceeded in precipitation tellurium, and content reaches as high as 0.0025%, more than arsenic standard (YS/T 222-2010) content
0.0005% 4 times so that product is not up to standard.Arsenic typically adds Na in purification and liquid making in tellurium slag2S carries out partial removal, but
Arsenic can accumulate enrichment in electrolytic deposition process in tellurium electrolyte, and now, arsenic is easily in negative electrode with elemental arsenic precipitation.
Patent 201210087000.0 discloses a kind of method of Fire arsenic removal, adds quick lime, sodium carbonate and arsenic to occur
Reaction forms white slag, so as to reach the purpose of dearsenification.The method is intended to remove the arsenic in composition brass plate, and arsenic content is up to 1～3%,
It is about 0.2% containing arsenic in composition brass plate after removing.Using the method for precipitation tellurium deeply removing arsenic effect is not it is obvious that because analysis
Go out arsenic content in tellurium very low, it is impossible to effectively arsenic is down into less than 0.0005% from 0.0025%.Therefore, it is necessary to develop a kind of use
Make the method that removing separates out arsenic in tellurium.
The content of the invention
In view of this, it is an object of the invention to propose a kind of method from refining dearsenification in tellurium is separated out, to improve arsenic
Clearance.
Based on above-mentioned purpose, what the present invention was provided comprises the following steps from the method for separating out refining dearsenification in tellurium：To separate out
Tellurium melts；
NaOH and oxidant are added in the precipitation tellurium of fusing, is made arsenic form natrium arsenicum and is entered in slag；
When slag floats up to surface, slag is dragged for；
The slag pulled out is cast.
In some embodiments of the invention, the fusion temperature for separating out tellurium is 450～470 DEG C.
In some embodiments of the invention, the oxidant is selected from least in sodium peroxide, sodium nitrate and ozone
Kind.
In some embodiments of the invention, the addition of the oxidant is 1.2～1.5 times of theoretical amount.Often remove
1kg arsenic needs sodium peroxide 5.2kg, or needs sodium nitrate 0.89kg, or ozone 0.53kg,
In some embodiments of the invention, the addition of the NaOH is 2～3 times of theoretical amount.In the present invention
Some embodiments in, the slag making temperature be 470～500 DEG C.
In some embodiments of the invention, 20～40 minutes are kept stirring in slagging process.
In some embodiments of the invention, the cast temperature is 500～520 DEG C.
In some embodiments of the invention, arsenic 0.001～0.0025% is contained in the precipitation tellurium.
From the above it can be seen that the invention has the advantages that：Present invention process is simple, operation letter
Just, dearsenification effect is good, and tellurium loss is few, arsenic can be down into less than 0.0005%, it is ensured that product arsenic is up to standard.
Description of the drawings
Fig. 1 is the embodiment of the present invention from the process chart for separating out refining dearsenification in tellurium.
Specific embodiment
To make the object, technical solutions and advantages of the present invention become more apparent, below in conjunction with specific embodiment, and reference
Accompanying drawing, the present invention is described in more detail.
Embodiment 1
Referring to Fig. 1, it is the embodiment of the present invention from the process chart for separating out refining dearsenification in tellurium.
50kg precipitation telluriums are put into graphite crucible, using intermediate frequency heating, being heated to 450 DEG C melts precipitation tellurium.
Wherein, separate out in tellurium containing 0.0021% arsenic.
NaOH and sodium nitrate are continuously added in the precipitation tellurium for melting, wherein the addition of NaOH is theory
2 times of amount, sodium nitrate addition is 1.2 times of theoretical amount, stirs 20min, while controlling slag making temperature for 470 DEG C, then drags for slag.
The calculation of theoretical amount is:After using different oxidizing arsenic, during using sodium nitrate as oxidant, removing
1 part of arsenic needs 1.07 parts of NaOH, 0.89 part of sodium nitrate.
The slag pulled out is directed at into mold, slow casting controls 500 DEG C of cast temperature, and 4N essence telluriums can be acquired after cooling.Take
Smart telluride is tested, and wherein arsenic content is 0.0003%, less than specified in standard 0.0005%, reaches product standard requirement.
Embodiment 2
Referring to Fig. 1, it is the embodiment of the present invention from the process chart for separating out refining dearsenification in tellurium.
50kg precipitation telluriums are put into graphite crucible, using intermediate frequency heating, being heated to 460 DEG C melts precipitation tellurium.
Wherein, separate out in tellurium containing 0.0022% arsenic.
NaOH and sodium nitrate are continuously added in the precipitation tellurium for melting, wherein the addition of NaOH is theory
2.5 times of amount, the addition of sodium nitrate is 1.3 times of theoretical amount, stirs 30min, while controlling slag making temperature for 485 DEG C, is then dragged for
Slag.
The calculation of theoretical amount is:After using different oxidizing arsenic, during using sodium nitrate as oxidant, removing
1 part of arsenic needs 1.07 parts of NaOH, 0.89 part of sodium nitrate.
The slag pulled out is directed at into mold, slow casting controls 510 DEG C of cast temperature, and 4N essence telluriums can be acquired after cooling.Take
Smart telluride is tested, and wherein arsenic content is 0.0001%, less than specified in standard 0.0005%, reaches product standard requirement.
Embodiment 3
Referring to Fig. 1, it is the embodiment of the present invention from the process chart for separating out refining dearsenification in tellurium.
50kg precipitation telluriums are put into graphite crucible, using intermediate frequency heating, being heated to 470 DEG C melts precipitation tellurium.
Wherein, separate out in tellurium containing 0.0015% arsenic.
NaOH and sodium peroxide are continuously added in the precipitation tellurium for melting, wherein the addition of NaOH is reason
3 times of stoichiometric, the addition of sodium peroxide is 1.5 times of theoretical amount, stirs 40min, while controlling slag making temperature for 500 DEG C, then
Drag for slag.
The calculation of theoretical amount is:After using different oxidizing arsenic, added NaOH is different in slagging process,
During using sodium peroxide as oxidant, 1 part of arsenic of removing needs 1.07 parts of NaOH, 5.2 parts of sodium peroxide.
The slag pulled out is directed at into mold, slow casting controls 520 DEG C of cast temperature, and 4N essence telluriums can be acquired after cooling.Take
Smart telluride is tested, and wherein arsenic content is 0.0001%, less than specified in standard 0.0005%, reaches product standard requirement.
Embodiment 4
Referring to Fig. 1, it is the embodiment of the present invention from the process chart for separating out refining dearsenification in tellurium.
50kg precipitation telluriums are put into graphite crucible, using intermediate frequency heating, being heated to 475 DEG C melts precipitation tellurium.
Wherein, separate out in tellurium containing 0.0017% arsenic.
NaOH and ozone are continuously added in the precipitation tellurium for melting, wherein the addition of NaOH is theoretical amount
2 times, the addition of ozone is 1.4 times of theoretical amount, stirs 35min, while controlling slag making temperature for 498 DEG C, then drags for slag.
The calculation of theoretical amount is:After using different oxidizing arsenic, during using ozone as oxidant, removing 1
Part arsenic needs 1.07 parts of NaOH, 0.53 part of ozone.
The slag pulled out is directed at into mold, slow casting controls 518 DEG C of cast temperature, and 4N essence telluriums can be acquired after cooling.Take
Smart telluride is tested, and wherein arsenic content is 0.0002%, less than specified in standard 0.0005%, reaches product standard requirement.
As can be seen here, what the present invention was provided has the advantages that from the method for separating out refining dearsenification in tellurium：
1) fusion temperature for separating out tellurium is 450～470 DEG C by the present invention, is completely melt precipitation tellurium, while reduce tellurium waving
Send out loss；
2) present invention is made arsenic form natrium arsenicum and is entered in slag, to improve going for arsenic by addition NaOH and oxidant
Except rate, arsenic is down into less than 0.0005%.
Those of ordinary skill in the art should be understood：The specific embodiment of the present invention is the foregoing is only, and
The restriction present invention, all any modification, equivalent substitution and improvements within the spirit and principles in the present invention, done etc. are not used in,
Should be included within protection scope of the present invention.
Claims (9)
1. a kind of method that dearsenification is refined in tellurium from precipitation, it is characterised in that comprise the following steps：
Tellurium fusing will be separated out；
NaOH and oxidant are added in the precipitation tellurium of fusing, is made arsenic form natrium arsenicum and is entered in slag；
When slag floats up to surface, slag is dragged for；
The slag pulled out is cast.
2. the method that dearsenification is refined in the tellurium from precipitation according to claim 1, it is characterised in that the fusing of the precipitation tellurium
Temperature is 450～470 DEG C.
3. the method that dearsenification is refined in the tellurium from precipitation according to claim 1, it is characterised in that the oxidant was selected from
At least one in sodium oxide molybdena, sodium nitrate and ozone.
4. the method that dearsenification is refined in the tellurium from precipitation according to claim 1, it is characterised in that the addition of the oxidant
Measure as 1.2～1.5 times of theoretical amount.
5. it is according to claim 1 from separating out method that dearsenification is refined in tellurium, it is characterised in that the NaOH adds
Dosage is 2～3 times of theoretical amount.
6. it is according to claim 1 from separating out method that dearsenification is refined in tellurium, it is characterised in that the slag making temperature is
470～500 DEG C.
7. the method that dearsenification is refined in the tellurium from precipitation according to claim 6, it is characterised in that keep in slagging process
Stirring 20～40 minutes.
8. it is according to claim 1 from separating out method that dearsenification is refined in tellurium, it is characterised in that the cast temperature is
500～520 DEG C.
9. the method that dearsenification is refined in the tellurium from precipitation according to claim 1, it is characterised in that contain arsenic in the precipitation tellurium
0.001～0.0025%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611227386.5A CN106629633B (en) | 2016-12-27 | 2016-12-27 | A method of dearsenification is refined from being precipitated in tellurium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611227386.5A CN106629633B (en) | 2016-12-27 | 2016-12-27 | A method of dearsenification is refined from being precipitated in tellurium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106629633A true CN106629633A (en) | 2017-05-10 |
| CN106629633B CN106629633B (en) | 2019-05-17 |
Family
ID=58831472
Family Applications (1)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107720710A (en) * | 2017-10-23 | 2018-02-23 | 湖南华信稀贵科技股份有限公司 | A kind of method for separating out tellurium refining dearsenification |
| CN109319744A (en) * | 2017-07-31 | 2019-02-12 | 成都中建材光电材料有限公司 | A kind of preparation method of 4N tellurium |
| CN115465842A (en) * | 2022-09-02 | 2022-12-13 | 江西铜业股份有限公司 | 4N tellurium casting method |
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| CN1295135A (en) * | 2000-07-14 | 2001-05-16 | 柳州市环东金属材料厂 | Dearsenicating method during smelting lead-antimony alloy |
| CN1355324A (en) * | 2000-11-27 | 2002-06-26 | 上海飞轮有色冶炼厂 | Metallurgical technology for regenerating pure lead from Pb-contained waste without pollution |
| CN1455011A (en) * | 2003-05-06 | 2003-11-12 | 锡矿山闪星锑业有限责任公司 | Method of removing arsenic and selenium for antimony smelting by pyrometallurgy |
| CN105603224A (en) * | 2015-12-25 | 2016-05-25 | 河南豫光金铅股份有限公司 | Smelting method for preparing lead-antimony alloy from lead-containing waste |
| CN106086461A (en) * | 2016-08-18 | 2016-11-09 | 紫金矿业集团股份有限公司 | A kind of method of Copper making process slag making arsenic removal |
-
2016
- 2016-12-27 CN CN201611227386.5A patent/CN106629633B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1295135A (en) * | 2000-07-14 | 2001-05-16 | 柳州市环东金属材料厂 | Dearsenicating method during smelting lead-antimony alloy |
| CN1355324A (en) * | 2000-11-27 | 2002-06-26 | 上海飞轮有色冶炼厂 | Metallurgical technology for regenerating pure lead from Pb-contained waste without pollution |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109319744A (en) * | 2017-07-31 | 2019-02-12 | 成都中建材光电材料有限公司 | A kind of preparation method of 4N tellurium |
| CN107720710A (en) * | 2017-10-23 | 2018-02-23 | 湖南华信稀贵科技股份有限公司 | A kind of method for separating out tellurium refining dearsenification |
| CN115465842A (en) * | 2022-09-02 | 2022-12-13 | 江西铜业股份有限公司 | 4N tellurium casting method |
| CN115465842B (en) * | 2022-09-02 | 2024-03-08 | 江西铜业股份有限公司 | 4N tellurium casting method |
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Address after: 423038 No.1 Fucheng Avenue, Chenzhou hi tech Industrial Park, Hunan Province Patentee after: Hunan Baiyin Co.,Ltd. Country or region after: China Address before: 423038 No.1 Fucheng Avenue, Chenzhou hi tech Industrial Park, Hunan Province Patentee before: JINGUI SILVER INDUSTRY Co.,Ltd. Country or region before: China |