CN101274777A - A method for extracting vanadium pentoxide from vanadium-containing liquid - Google Patents
A method for extracting vanadium pentoxide from vanadium-containing liquid Download PDFInfo
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- CN101274777A CN101274777A CN 200710034640 CN200710034640A CN101274777A CN 101274777 A CN101274777 A CN 101274777A CN 200710034640 CN200710034640 CN 200710034640 CN 200710034640 A CN200710034640 A CN 200710034640A CN 101274777 A CN101274777 A CN 101274777A
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 55
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 25
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 239000007788 liquid Substances 0.000 title abstract description 19
- 238000000605 extraction Methods 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 238000001556 precipitation Methods 0.000 claims abstract description 12
- 239000003350 kerosene Substances 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000000284 extract Substances 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000012074 organic phase Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 11
- 239000008346 aqueous phase Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims 1
- 238000005191 phase separation Methods 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 7
- 238000000658 coextraction Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 8
- 239000012535 impurity Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明公开了一种从含钒液体中提取五氧化二钒的方法，它是在含钒液体中加入萃取剂(N－235)及协萃剂(磺化煤油和TPB)，经萃取、洗涤、反萃、过滤、沉钒和煅烧等工艺步骤得到含钒＞98％的产品。本发明方法选择了一种高效分离富集低含量含钒液体的萃取剂(N－235)及协萃剂(磺化煤油和TPB)，简化了工艺流程，降低了生产成本，提高了钒的回收率，使含钒液中钒的收率达到97％以上；其总回收率达到95％以上，产品纯度达98％以上。The invention discloses a method for extracting vanadium pentoxide from vanadium-containing liquid, which is to add extraction agent (N-235) and co-extraction agent (sulfonated kerosene and TPB) into vanadium-containing liquid, extract and wash , back extraction, filtration, vanadium precipitation and calcination to obtain products containing more than 98% vanadium. The method of the present invention selects an extractant (N-235) and a co-extractant (sulfonated kerosene and TPB) for efficiently separating and enriching low-content vanadium-containing liquids, which simplifies the process flow, reduces production costs, and improves the vanadium content. The recovery rate makes the vanadium recovery rate in the vanadium-containing liquid reach more than 97 percent; the total recovery rate reaches more than 95 percent, and the product purity reaches more than 98 percent.
Description
技术领域 technical field
本发明涉及一种从含钒液体中提取五氧化二钒的方法。The invention relates to a method for extracting vanadium pentoxide from vanadium-containing liquid.
背景技术 Background technique
国内外从液体中提钒的方法有：(1)水解沉钒工艺：钒液加热水解沉钒-溶解-除杂-过滤-沉钒-过滤-煅烧得五氧化二钒工艺。该工艺过程反应较复杂，受溶液的性质、浓度、酸度、温度、杂质等因素的影响较大，产品质量难于控制，收率70-80％左右。(2)离子交换工艺，钒液调节一定的pH值，钒液经上柱-洗脱-除杂-过滤-沉钒-过滤-煅烧得五氧化二钒产品工艺。该工艺对选择性有了提高，杂质得到了有效控制，但是，由于树脂的吸附性，仍有杂质带入产品，除杂会带来损失，总收率在80％左右。(3)沉钒工艺，向含钒液体中加入沉淀剂，经沉钒-过滤-浸出-除杂-过滤-铵盐沉钒-过滤-煅烧得五氧化二钒产品工艺。该工艺沉钒和浸出过程较复杂，不易控制。(4)萃取工艺，钒液经萃取-洗涤-反萃-沉钒-过滤-煅烧得五氧化二钒产品工艺，该工艺由于所采用萃取剂的不同，收率、产品质量、效益皆存在很大差别。The methods for extracting vanadium from liquids at home and abroad include: (1) Hydrolysis vanadium deposition process: vanadium solution is heated and hydrolyzed for vanadium deposition-dissolution-impurity removal-filtration-vanadium deposition-filtration-calcination to obtain vanadium pentoxide. The reaction of the process is relatively complicated, greatly influenced by the properties, concentration, acidity, temperature, impurities and other factors of the solution, the product quality is difficult to control, and the yield is about 70-80%. (2) Ion exchange process, the vanadium solution is adjusted to a certain pH value, and the vanadium solution is put on the column-elution-removal-impurity-filtration-precipitation of vanadium-filtration-calcination to obtain the product process of vanadium pentoxide. The process has improved selectivity and effectively controlled impurities. However, due to the adsorption of the resin, impurities are still brought into the product, and the removal of impurities will bring losses. The total yield is about 80%. (3) Vanadium precipitation process, adding a precipitant to the vanadium-containing liquid, through vanadium precipitation - filtration - leaching - impurity removal - filtration - ammonium salt precipitation of vanadium - filtration - calcining to obtain the product process of vanadium pentoxide. The process of vanadium precipitation and leaching is complicated and difficult to control. (4) Extraction process, the vanadium liquid is extracted-washed-extracted-precipitated-vanadium-filtered-calcined to obtain the product process of vanadium pentoxide. Due to the difference of the extraction agent used in this process, the yield, product quality and benefit all exist. Big difference.
发明内容 Contents of the invention
本发明的目的是提供一种钒的回收率高、杂质少的从含钒液体中提取五氧化二钒的方法。The purpose of the present invention is to provide a method for extracting vanadium pentoxide from vanadium-containing liquid with high recovery rate of vanadium and few impurities.
本发明的技术方案如下：在含钒液体中按5-25∶90-70∶5的比例加入萃取剂(N-235)及协萃剂(磺化煤油和TPB)，调节含钒液体的pH值为1-3，水相与有机相按4∶1进行萃取，振荡5-10分钟，静置20-60分钟，待分层；将水相分离后，用工艺水洗涤有机相3-5次；采用1molNaCl-1mol NaOH体系对有机相进行反萃，控制水相中钒含量在20g/L以上；经反萃所得含钒液，调节其pH值为7-8，加入含钒量1-3倍的NH4Cl，常温下搅拌10-30分钟，静置24小时得偏钒酸铵沉淀；过滤得到固体偏钒酸铵，在550℃氧化煅烧2-4小时得到纯度＞98.％的精钒。The technical scheme of the present invention is as follows: add extraction agent (N-235) and co-extraction agent (sulfonated kerosene and TPB) in the ratio of 5-25:90-70:5 in the vanadium-containing liquid to adjust the pH of the vanadium-containing liquid The value is 1-3, the water phase and the organic phase are extracted at a ratio of 4:1, shaken for 5-10 minutes, left standing for 20-60 minutes, and separated; after separating the water phase, wash the organic phase with process water for 3-5 Second; adopt 1molNaCl-1mol NaOH system to carry out back-extraction to organic phase, control the vanadium content in aqueous phase more than 20g/L; Gained vanadium-containing liquid through back-extraction, adjust its pH value to be 7-8, add vanadium content 1- 3 times NH 4 Cl, stirred at room temperature for 10-30 minutes, and stood still for 24 hours to obtain ammonium metavanadate precipitation; filtered to obtain solid ammonium metavanadate, oxidized and calcined at 550°C for 2-4 hours to obtain purity>98.% Refined vanadium.
本发明的方法由于选择了一种高效分离富集低含量含钒液体的萃取剂(N-235)及协萃剂(磺化煤油和TPB)，简化了工艺流程，降低了生产成本，提高了钒的回收率，使含钒液中钒的收率达到97％以上；其总回收率达到95％以上，产品纯度达98％以上。The method of the present invention simplifies the process flow, reduces the production cost and improves the efficiency of the extraction agent (N-235) and co-extraction agent (sulfonated kerosene and TPB) due to the selection of a high-efficiency separation and enrichment of low-content vanadium-containing liquid extractant (N-235) The recovery rate of vanadium makes the recovery rate of vanadium in the vanadium-containing liquid reach more than 97%, the total recovery rate reaches more than 95%, and the product purity reaches more than 98%.
具体实施方式： Detailed ways:
实施例一：Embodiment one:
(1)萃取：将萃取剂(N-235)、协萃剂(磺化煤油和TPB)，按5∶90∶5比例混合，调节含钒(2.15g/L)液体的pH值为1.5，水相与有机相按4∶1进行萃取，振荡5分钟，静置20分钟，待分层；(1) Extraction: Mix the extraction agent (N-235) and co-extraction agent (sulfonated kerosene and TPB) in a ratio of 5:90:5 to adjust the pH value of the vanadium-containing (2.15g/L) liquid to 1.5, The aqueous phase and the organic phase were extracted at a ratio of 4:1, oscillated for 5 minutes, and stood for 20 minutes until the layers were separated;
(2)洗涤：将水相分离后，用工艺水洗涤有机相4次；(2) Washing: after separating the aqueous phase, wash the organic phase 4 times with process water;
(3)反萃：采用1mol NaCl-1mol NaOH体系对有机相进行反萃，控制水相中钒含量在20g/L以上；(3) Stripping: use 1mol NaCl-1mol NaOH system to strip the organic phase, and control the vanadium content in the aqueous phase to be above 20g/L;
(4)沉钒：经反萃所得含钒液，调节其pH值为7.2，加入含钒量2.5倍的NH4Cl，常温下搅拌15分钟，静置24小时得偏钒酸铵沉淀；(4) Precipitation of vanadium: adjust the pH of the vanadium-containing liquid obtained by stripping to 7.2, add NH 4 Cl with 2.5 times the vanadium content, stir at room temperature for 15 minutes, and stand for 24 hours to obtain ammonium metavanadate precipitation;
(5)过滤：过滤得到固体偏钒酸铵；(5) filter: filter to obtain solid ammonium metavanadate;
(6)煅烧：将固体偏钒酸铵在550℃氧化煅烧4小时得到纯度＞98.％的精钒。(6) Calcination: oxidize and calcinate solid ammonium metavanadate at 550°C for 4 hours to obtain refined vanadium with a purity >98.%.
实施例二：Embodiment two:
按照上述工艺过程，将萃取剂(N-235)、协萃剂(磺化煤油和TPB)，按一定比例混合(10∶85∶5)，调节含钒(2.15g/L)液体的pH值为2.0，水相与有机相按4∶1进行萃取，振荡8分钟，静置40分钟；分离水相后，用工艺水洗涤有机相4次；采用1mol NaCl-1mol NaOH体系对有机相进行反萃，控制水相中钒含量在20g/L以上；调节其pH值为7.4，加入含钒量2倍的NH4Cl，常温下搅拌20分钟，静置24小时得偏钒酸铵沉淀；过滤得到固体偏钒酸铵，在550℃氧化煅烧3小时得到纯度＞98.％的精钒。According to the above process, the extraction agent (N-235), co-extraction agent (sulfonated kerosene and TPB) are mixed in a certain ratio (10:85:5), and the pH value of the liquid containing vanadium (2.15g/L) is adjusted 2.0, the water phase and the organic phase were extracted at a ratio of 4:1, shaken for 8 minutes, and left to stand for 40 minutes; after separating the water phase, the organic phase was washed 4 times with process water; the organic phase was reversed with 1mol NaCl-1mol NaOH system Extraction, control the vanadium content in the water phase above 20g/L; adjust its pH value to 7.4, add NH4Cl with 2 times the vanadium content, stir at room temperature for 20 minutes, and stand for 24 hours to obtain ammonium metavanadate precipitation; filter to obtain solid Ammonium metavanadate is oxidized and calcined at 550°C for 3 hours to obtain refined vanadium with a purity >98.%.
实施例三：Embodiment three:
按照上述工艺过程，将萃取剂(N-235)、协萃剂(磺化煤油和TPB)，按一定比例混合(20∶75∶5)，调节含钒(2.15g/L)液体的pH值为2.5，水相与有机相按4∶1进行萃取，振荡10分钟，静置50分钟；分离水相后，用工艺水洗涤有机相4次；采用1mol NaCl-1mol NaOH体系对有机相进行反萃，控制水相中钒含量在20g/L以上；调节其pH值为7.1，加入含钒量2.1倍的NH4Cl，常温下搅拌15分钟，静置24小时得偏钒酸铵沉淀；过滤得到固体偏钒酸铵，在550℃氧化煅烧4小时得到纯度＞98.％的精钒。According to the above process, the extraction agent (N-235), co-extraction agent (sulfonated kerosene and TPB) are mixed in a certain ratio (20:75:5), and the pH value of the vanadium-containing (2.15g/L) liquid is adjusted 2.5, the water phase and the organic phase were extracted at a ratio of 4:1, shaken for 10 minutes, and left to stand for 50 minutes; after separating the water phase, the organic phase was washed 4 times with process water; the organic phase was reversed with 1mol NaCl-1mol NaOH system Extraction, control the vanadium content in the water phase above 20g/L; adjust its pH value to 7.1, add NH4Cl with 2.1 times the vanadium content, stir at room temperature for 15 minutes, and stand for 24 hours to obtain ammonium metavanadate precipitation; filter to obtain solid Ammonium metavanadate is oxidized and calcined at 550°C for 4 hours to obtain refined vanadium with a purity >98.%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928830A (en) * | 2010-09-25 | 2010-12-29 | 吉首大学 | A method for extracting vanadium from vanadium-containing liquid |
| CN102826603A (en) * | 2012-09-20 | 2012-12-19 | 电子科技大学 | Preparation method of vanadium pentoxide nanofibers |
| CN102849795A (en) * | 2011-07-02 | 2013-01-02 | 全喆 | Preparation of high-purity vanadium pentoxide |
| WO2015161659A1 (en) * | 2014-04-21 | 2015-10-29 | 中国科学院过程工程研究所 | Method for simultaneously preparing high-purity vanadium and heteropolyacid catalyst |
| CN106966431A (en) * | 2017-05-15 | 2017-07-21 | 天津市风船化学试剂科技有限公司 | A kind of preparation method of the high-purity ammonium metavanadate of 4N assigned stages |
-
2007
- 2007-03-26 CN CN 200710034640 patent/CN101274777A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928830A (en) * | 2010-09-25 | 2010-12-29 | 吉首大学 | A method for extracting vanadium from vanadium-containing liquid |
| CN102849795A (en) * | 2011-07-02 | 2013-01-02 | 全喆 | Preparation of high-purity vanadium pentoxide |
| CN102849795B (en) * | 2011-07-02 | 2014-12-17 | 全喆 | Preparation of high-purity vanadium pentoxide |
| CN102826603A (en) * | 2012-09-20 | 2012-12-19 | 电子科技大学 | Preparation method of vanadium pentoxide nanofibers |
| WO2015161659A1 (en) * | 2014-04-21 | 2015-10-29 | 中国科学院过程工程研究所 | Method for simultaneously preparing high-purity vanadium and heteropolyacid catalyst |
| CN106966431A (en) * | 2017-05-15 | 2017-07-21 | 天津市风船化学试剂科技有限公司 | A kind of preparation method of the high-purity ammonium metavanadate of 4N assigned stages |
| CN106966431B (en) * | 2017-05-15 | 2018-10-16 | 天津市风船化学试剂科技有限公司 | A kind of preparation method of the high-purity ammonium metavanadate of 4N assigned stages |
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