CN101844750A - Method for preparing high-purity tellurium by material containing tellurium - Google Patents
Method for preparing high-purity tellurium by material containing tellurium Download PDFInfo
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- CN101844750A CN101844750A CN201010191510A CN201010191510A CN101844750A CN 101844750 A CN101844750 A CN 101844750A CN 201010191510 A CN201010191510 A CN 201010191510A CN 201010191510 A CN201010191510 A CN 201010191510A CN 101844750 A CN101844750 A CN 101844750A
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- tellurium
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- containing material
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- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 85
- 239000000463 material Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 21
- 239000003929 acidic solution Substances 0.000 claims abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000001257 hydrogen Substances 0.000 claims abstract description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 5
- 238000002386 leaching Methods 0.000 claims abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 claims abstract 7
- 239000007800 oxidant agent Substances 0.000 claims abstract 6
- 230000001590 oxidative effect Effects 0.000 claims abstract 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 235000010265 sodium sulphite Nutrition 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 2
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 claims description 2
- 229940005991 chloric acid Drugs 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 2
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 2
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims 2
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 claims 2
- 239000004155 Chlorine dioxide Substances 0.000 claims 1
- 235000019398 chlorine dioxide Nutrition 0.000 claims 1
- GRWZHXKQBITJKP-UHFFFAOYSA-L dithionite(2-) Chemical compound [O-]S(=O)S([O-])=O GRWZHXKQBITJKP-UHFFFAOYSA-L 0.000 claims 1
- 235000010269 sulphur dioxide Nutrition 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 230000002829 reductive effect Effects 0.000 description 5
- 229910052785 arsenic Inorganic materials 0.000 description 4
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052711 selenium Inorganic materials 0.000 description 3
- 239000011669 selenium Substances 0.000 description 3
- 238000004857 zone melting Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000006256 anode slurry Substances 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- UGWKCNDTYUOTQZ-UHFFFAOYSA-N copper;sulfuric acid Chemical compound [Cu].OS(O)(=O)=O UGWKCNDTYUOTQZ-UHFFFAOYSA-N 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
一种含碲物料制备高纯碲的方法，本发明是以一种含碲的物料为原料，采用化学方法处理制备得到高纯碲。将含碲物料氧化酸浸脱铜，过滤得到粗碲；在氧化剂作用下酸性溶液浸出粗碲，经过过滤得到含碲溶液；在含碲溶液中加入还原剂，反应后加热过滤，在滤液中再次加入还原剂，在加热下反应后过滤得到碲粉；在氧化剂作用下酸性溶液溶解碲粉后加入还原剂得到精碲；在200℃～800℃下，氢气处理精碲得到高纯碲。A method for preparing high-purity tellurium from a tellurium-containing material. The invention uses a tellurium-containing material as a raw material and prepares high-purity tellurium by chemical treatment. Decopper the tellurium-containing material by oxidative acid leaching, and filter to obtain crude tellurium; under the action of an oxidant, the acidic solution leaches the crude tellurium, and obtains a tellurium-containing solution after filtration; add a reducing agent to the tellurium-containing solution, heat and filter after reaction, and re- Add a reducing agent, react under heating, and then filter to obtain tellurium powder; dissolve the tellurium powder in an acidic solution under the action of an oxidizing agent, and then add a reducing agent to obtain refined tellurium; at 200°C to 800°C, treat the refined tellurium with hydrogen to obtain high-purity tellurium.
Description
Technical field
The invention belongs to the hydrometallurgy field, particularly contain the tellurium material, the preparation high purity tellurium at the high selenium of high-copper.
Background technology
The tellurium association is in mineral such as copper, lead, zinc.At present, the tellurium major part is from copper, lead anode slurry.Roasting behind copper anode mud and the vitriol oil stirring and evenly mixing, leaching, evaporative crystallization reclaim(ed) sulfuric acid copper obtain containing the tellurium material after adding reductive agent reaction by the CN200810032022.0 patented technology in the copper sulfate mother liquor.The aforesaid method gained contains copper in the tellurium material, arsenic content height, needs through removing the high purity tellurium that impurity such as copper, arsenic wherein just can obtain having very high economic worth.
At present, generally will contain the tellurium material obtains adopting electrolysis to obtain content behind the tellurium material to be 99.99% high purity tellurium, perhaps to adopt technology such as vacuum distilling, zone melting to prepare high purity tellurium high-purity containing through removal of impurities repeatedly.Electrolytic process complex process, product yield are low; Vacuum distilling is to impurity inferior separating effect such as selenium, arsenic, lead, sodium, and requires good vacuum system; Zone melting can obtain high purity tellurium, but the operational requirement strictness, and commute and tellurium form eutectiferous impurity separation difficulty, and direct yield is low, the yielding poorly of unit equipment.
Summary of the invention
The objective of the invention is to handle, impurity such as copper, selenium, arsenic are separated with tellurium, obtain the higher high purity tellurium of economic worth containing the tellurium material.
Process of the present invention is: will contain tellurium material oxidation acid leaching decopper(ing), and filter and obtain thick tellurium; Acidic solution leaches thick tellurium under the oxygenant effect, obtain containing tellurium solution through filtering, used oxygenant is hydrogen peroxide, nitric acid, nitrate, dioxide peroxide, hypochlorous acid, hypochlorite, chloric acid or oxymuriate, and it is nitric acid, hydrochloric acid or sulfuric acid that acidic solution leaches used acid; In containing tellurium solution, add reductive agent, the reaction post-heating filters, add reductive agent in filtrate once more, the reaction after-filtration obtains the tellurium powder under 0 ℃～120 ℃ temperature, and used reductive agent is sulfurous gas, S-WAT, sodium bisulfite, vat powder, formic acid or formate; Behind acid leach solution tellurium powder under the oxygenant effect, add reductive agent and obtain smart tellurium; Under 200 ℃～800 ℃, the smart tellurium of hydrogen treat obtains content more than or equal to 99.99% high purity tellurium.
Embodiment
Embodiment 1: contain in the tellurium material at 2kg that to add 6.8L concentration be in 45% salpeter solution, start and stir, at 20 ℃ of reaction 1.5h down.Then, filtration, washing, oven dry obtain thick tellurium.It is more as shown in table 1 with thick tellurium composition to contain the tellurium material:
Table 1 contains tellurium material and thick tellurium composition comparison/%
In 7.5L concentration is to add thick tellurium in 25% the hydrochloric acid soln, starts and stirs, and adding 0.2L concentration in the reaction process is 45% salpeter solution, 75 ℃ of reactions down, when thick tellurium dissolving after-filtration.In filtrate, feed SO
2Reaction produces red precipitate to stopped reaction after the black precipitate, heating and filtering occurring.After the filtration solution is heated to 85 ℃, feeds SO
2Make in the solution tellurium fully reduce after-filtration, washing, oven dry and obtain 1210g tellurium powder.
In 7.5L concentration is to add gained tellurium powder in 25% the hydrochloric acid soln, starts and stirs, and adds the 2.3L hydrogen peroxide in the reaction process altogether, 80 ℃ of reactions down, when tellurium powder dissolving after-filtration, after the filtration solution is heated to 85 ℃, feeds SO
2Make in the solution tellurium fully reduce after-filtration, washing, oven dry and obtain the smart tellurium of 1200g.Gained tellurium powder and smart tellurium composition are more as shown in table 2:
Table 2 tellurium powder and the comparison of smart tellurium composition //mgkg
-1
Gained tellurium powder is put into quartzy stove, under the hydrogen effect, through obtain after 450 ℃ of processing 1180g purity be 99.9996% high purity tellurium, its high purity tellurium composition is as shown in table 3.
Table 3 high purity tellurium composition/mgkg
-1
Embodiment 2: contain in the tellurium material at 2kg that to add 8L concentration be in 4% sulphuric acid soln, start and stir, add the 0.4L hydrogen peroxide in the reaction process, 20 ℃ down reaction 3.5h after-filtration, washing, oven dry to obtain purity be 76.01% thick tellurium, it is as shown in table 4 to contain the tellurium material component:
Table 4 contains tellurium material component/%
In 10L concentration is to add thick tellurium in 20% the hydrochloric acid soln, starts and stirs, and adds the 0.5L hydrogen peroxide in the reaction process, 80 ℃ of reactions down, when thick tellurium dissolving after-filtration.In filtrate, add sodium sulfite solution, produce red precipitate to stopped reaction after the black precipitate, heating and filtering occurring.After the filtration solution is heated to 85 ℃, add sodium sulfite solution make tellurium in the solution fully reduce after-filtration, washing, oven dry to obtain 1000g purity be 99.92% tellurium powder.
In 10L concentration is to add gained tellurium powder in 20% the hydrochloric acid soln, start and stir, add the 2L hydrogen peroxide in the reaction process altogether, 80 ℃ of reactions down, when tellurium powder dissolving after-filtration, after the filtration solution is heated to 85 ℃, add sodium sulfite solution make tellurium in the solution fully reduce after-filtration, washing, oven dry to obtain 995g purity be 99.99% smart tellurium.
Gained tellurium powder is put into quartzy stove, under the hydrogen effect, through obtain after 420 ℃ of processing 980g purity be 99.999% high purity tellurium, its high purity tellurium composition is as shown in table 5.
Table 5 high purity tellurium composition/mgkg
-1
Claims (5)
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| CN201010191510A CN101844750A (en) | 2010-06-04 | 2010-06-04 | Method for preparing high-purity tellurium by material containing tellurium |
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| CN201010191510A CN101844750A (en) | 2010-06-04 | 2010-06-04 | Method for preparing high-purity tellurium by material containing tellurium |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102139863A (en) * | 2011-05-03 | 2011-08-03 | 嘉兴市达泽光电技术有限公司 | Method for purifying tellurium by using crucible |
| CN102153054A (en) * | 2011-05-03 | 2011-08-17 | 嘉兴市达泽光电技术有限公司 | Preparation method of high purity tellurium |
| CN105445268A (en) * | 2015-11-18 | 2016-03-30 | 西北矿冶研究院 | Analysis method for determining tellurium in high-selenium tellurium slag |
| CN106006572A (en) * | 2016-05-12 | 2016-10-12 | 云南驰宏资源综合利用有限公司 | Method for recycling tellurium from tellurium anode slime |
| CN106241751A (en) * | 2016-08-22 | 2016-12-21 | 广东先导稀材股份有限公司 | The method reclaiming tellurium from alloy |
| CN106517106A (en) * | 2016-10-29 | 2017-03-22 | 乐山凯亚达光电科技有限公司 | Efficient purification method of high-purity tellurium |
| CN106868319A (en) * | 2016-12-21 | 2017-06-20 | 中南大学 | A kind of method that high purity tellurium is obtained in the immersion liquid from alkali containing arsenic |
| CN107190272A (en) * | 2017-04-25 | 2017-09-22 | 中南大学 | A kind of method for preparing tellurium powder |
| CN112390231A (en) * | 2019-08-15 | 2021-02-23 | 中南大学 | Method for preparing refined tellurium from tellurium dioxide powder |
| CN112960654A (en) * | 2020-04-20 | 2021-06-15 | 金川集团股份有限公司 | Method for efficiently separating selenium and tellurium from acidic liquid |
| CN113307233A (en) * | 2021-05-28 | 2021-08-27 | 金川镍钴研究设计院有限责任公司 | Method for purifying and selenium-removing tellurium-containing metal material |
| CN113387336A (en) * | 2021-06-15 | 2021-09-14 | 中南大学 | Method for removing selenium from tellurium ingot |
| CN113428844A (en) * | 2021-06-25 | 2021-09-24 | 铜陵有色金属集团股份有限公司 | Production equipment and production process of 6N-grade high-purity tellurium |
| CN117963849A (en) * | 2024-01-25 | 2024-05-03 | 昆明理工大学 | A method for preparing 7N tellurium |
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Cited By (20)
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|---|---|---|---|---|
| CN102153054A (en) * | 2011-05-03 | 2011-08-17 | 嘉兴市达泽光电技术有限公司 | Preparation method of high purity tellurium |
| CN102139863A (en) * | 2011-05-03 | 2011-08-03 | 嘉兴市达泽光电技术有限公司 | Method for purifying tellurium by using crucible |
| CN105445268B (en) * | 2015-11-18 | 2018-12-28 | 西北矿冶研究院 | Analysis method for determining tellurium in high-selenium tellurium slag |
| CN105445268A (en) * | 2015-11-18 | 2016-03-30 | 西北矿冶研究院 | Analysis method for determining tellurium in high-selenium tellurium slag |
| CN106006572A (en) * | 2016-05-12 | 2016-10-12 | 云南驰宏资源综合利用有限公司 | Method for recycling tellurium from tellurium anode slime |
| CN106006572B (en) * | 2016-05-12 | 2018-06-12 | 云南驰宏资源综合利用有限公司 | A kind of method from tellurium earth of positive pole recycling tellurium |
| CN106241751A (en) * | 2016-08-22 | 2016-12-21 | 广东先导稀材股份有限公司 | The method reclaiming tellurium from alloy |
| CN106517106A (en) * | 2016-10-29 | 2017-03-22 | 乐山凯亚达光电科技有限公司 | Efficient purification method of high-purity tellurium |
| CN106868319A (en) * | 2016-12-21 | 2017-06-20 | 中南大学 | A kind of method that high purity tellurium is obtained in the immersion liquid from alkali containing arsenic |
| CN107190272B (en) * | 2017-04-25 | 2019-05-17 | 中南大学 | A method of preparing tellurium powder |
| CN107190272A (en) * | 2017-04-25 | 2017-09-22 | 中南大学 | A kind of method for preparing tellurium powder |
| CN112390231A (en) * | 2019-08-15 | 2021-02-23 | 中南大学 | Method for preparing refined tellurium from tellurium dioxide powder |
| CN112390231B (en) * | 2019-08-15 | 2022-06-28 | 中南大学 | A kind of method for preparing refined tellurium from tellurium dioxide powder |
| CN112960654A (en) * | 2020-04-20 | 2021-06-15 | 金川集团股份有限公司 | Method for efficiently separating selenium and tellurium from acidic liquid |
| CN113307233A (en) * | 2021-05-28 | 2021-08-27 | 金川镍钴研究设计院有限责任公司 | Method for purifying and selenium-removing tellurium-containing metal material |
| CN113387336A (en) * | 2021-06-15 | 2021-09-14 | 中南大学 | Method for removing selenium from tellurium ingot |
| CN113387336B (en) * | 2021-06-15 | 2022-05-20 | 中南大学 | Method for removing selenium from tellurium ingot |
| CN113428844A (en) * | 2021-06-25 | 2021-09-24 | 铜陵有色金属集团股份有限公司 | Production equipment and production process of 6N-grade high-purity tellurium |
| CN113428844B (en) * | 2021-06-25 | 2023-08-01 | 安徽铜冠产业技术研究院有限责任公司 | Production equipment and production process of 6N-level high-purity tellurium |
| CN117963849A (en) * | 2024-01-25 | 2024-05-03 | 昆明理工大学 | A method for preparing 7N tellurium |
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Application publication date: 20100929 |