CN106555061A - 一种仲钨酸铵/三氧化钨的快速溶解方法 - Google Patents
一种仲钨酸铵/三氧化钨的快速溶解方法 Download PDFInfo
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- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 title claims abstract description 51
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 title claims abstract description 28
- 238000011978 dissolution method Methods 0.000 title claims abstract description 4
- 208000035126 Facies Diseases 0.000 claims abstract description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 230000008569 process Effects 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000004090 dissolution Methods 0.000 claims abstract description 9
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 8
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 150000002576 ketones Chemical class 0.000 claims abstract description 6
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 5
- 150000001412 amines Chemical class 0.000 claims abstract description 4
- 150000003014 phosphoric acid esters Chemical class 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000003350 kerosene Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 230000001172 regenerating effect Effects 0.000 claims description 4
- 239000001117 sulphuric acid Substances 0.000 claims description 4
- 235000011149 sulphuric acid Nutrition 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 abstract description 4
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- 230000008929 regeneration Effects 0.000 abstract description 2
- 238000011069 regeneration method Methods 0.000 abstract description 2
- 230000004044 response Effects 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract 1
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- 239000002912 waste gas Substances 0.000 abstract 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 17
- 229910052721 tungsten Inorganic materials 0.000 description 12
- 239000010937 tungsten Substances 0.000 description 12
- 238000005265 energy consumption Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 3
- -1 sec-octyl alcohols Chemical class 0.000 description 3
- 229910001930 tungsten oxide Inorganic materials 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- SJWFXCIHNDVPSH-UHFFFAOYSA-N octan-2-ol Chemical compound CCCCCCC(C)O SJWFXCIHNDVPSH-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 230000009719 regenerative response Effects 0.000 description 1
- 238000010850 salt effect Methods 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
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- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
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Abstract
本发明公开了一种仲钨酸铵/三氧化钨的快速溶解方法。将仲钨酸铵/三氧化钨固体加入酸和胺类、季铵盐类、磷酸酯类、醇、酮类的一种或多种萃取剂与调节剂和溶剂油混合所得的有机相将仲钨酸铵/三氧化钨完全溶解；再向有机相中倒入氨水、氢氧化钠溶液混合完成有机相再生；最后将有机相和钨酸盐溶液分离，有机相回用，得到钨酸盐溶液，完成了仲钨酸铵/三氧化钨的溶解过程。本发明以胺类、季铵盐类、磷酸酯类、醇、酮类作为试剂与溶剂混合得到有机相促进仲钨酸铵/三氧化钨的分解，过程温度低，反应速度快，得到钨酸盐浓度高，残碱浓度低，无废气产生，节能环保。
Description
技术领域
本发明属于湿法冶金或化工领域，具体是涉及一种仲钨酸铵/三氧化钨的快速溶解方法。
背景技术
钨是重要的战略金属资源，仲钨酸铵/三氧化钨是钨的重要化学产品。钨冶炼过程中会产生仲钨酸铵、氧化钨的合格品，或者收集到仲钨酸铵、氧化钨的废料。目前，仲钨酸铵多采用高浓度的氨水在温度为120~160℃搅拌浸出1~4小时才能完全的溶解；部分企业未来促进仲钨酸铵的分解甚至首先通过高温焙烧得到氧化钨，再采用氨水溶解得到钨酸铵溶液；某些企业则采用氢氧化钠等强碱溶解仲钨酸铵，得到钨酸钠溶液再生产得到钨酸铵溶液，上述方法过程复杂，成本高。因此，需要开发一种新型的低成本、简单的仲钨酸铵/三氧化钨溶解工艺。
发明内容
本发明的目的是针对现有技术存在的不足，提供了一种仲钨酸铵/三氧化钨的快速溶解方法，解决现有溶解工艺能耗高、耗时长、工艺复杂、操作环境不好等问题，具有节能，快速，流程简单，操作条件好等优点。
具体步骤为：
（1）将萃取剂、调节剂和溶剂混合得到有机相；萃取剂、调节剂和溶剂的体积比例分别为0.5~85%、0~70%和0~95%。
（2）将100g仲钨酸铵或三氧化钨、500~700mL步骤（1）所得有机相和50~80mL浓度为0.1~18mol/L的酸混合，在0~100℃时搅拌1~20分钟的时间，使得仲钨酸铵或三氧化钨完全溶解，得到溶解后的水相和油相混合料。
（3）向步骤（2）所得混合料中加入200~300mL浓度为0.1~20mol/L的再生剂，常温搅拌10~20分钟，使得有机相再生，同时得到钨酸盐溶液。
（4）分离步骤（3）所得的有机相和钨酸盐溶液，有机相返回溶解工序，钨酸盐溶液作为产品。
所述萃取剂为胺类、季铵盐类、磷酸酯类、醇、酮类，具体为叔胺、伯胺、季铵盐、仲辛醇、TBP和MIBK中的一种或多种.。
所述调节剂为醇、酮、酯类，具体为仲辛醇、TBP、中的一种或多种。
所述溶剂为磺化煤油、煤油、甲苯和260#溶剂油中的一种。
所述酸为盐酸、硫酸、硝酸和磷酸中的一种或多种。
所述再生剂为氢氧化钠、氢氧化钾、氨水、氯化钠和氯化铵中的一种或多种。
本发明主要机理是：
（1）本发明通过调节溶解反应体系为酸性，使得仲钨酸铵/三氧化钨结构被破坏，同时在萃取有机相的作用下，将溶液中钨同多酸或钨酸根转移至有机相中，降低水相中钨的游离浓度，促进仲钨酸铵/三氧化钨的分解，最终仲钨酸铵/三氧化钨完全分解，钨完全进入有机相中形成钨的有机化合物；
（2）钨的有机化合物在碱性物质或盐类作用下发生再生反应，得到产物为钨酸盐和有机相，即实现了仲钨酸铵/三氧化钨溶解为钨酸盐，同时有机相得到再生，可以回用。
有现有技术相比，本发明的有益效果是：
（1）本发明在室温下进行即可，温度低，能耗低。
（2）本发明反应速度快，仲钨酸铵/三氧化钨溶解时间为3~15min，工艺耗时短。
（3）本发明得到钨酸盐浓度高，如采用氨水再生，得到钨酸铵溶液中WO3浓度可以达到350g/L，便于后续生产。
（4）本发明工艺流程简短、能耗低、耗时短、操作简单、得到的钨酸盐浓度高。
附图说明
图1 为本发明的工艺流程图。
具体实施方式
下面结合实施，对本发明作进一步描述，以下实施例旨在说明本发明而不是对发明的进一步限定。
实施例1:
（1）将100g仲钨酸铵固体（WO3质量百分比含量为88.6%）、600mL有机相混合（组成为体积百分比10%N235+10%仲辛醇+70%磺化煤油）与50mL浓度为6mol/L的硫酸在25℃搅拌10分钟，仲钨酸铵的溶解率为100%。
（2）将步骤（1）所得到的物料中加入250mL质量百分比浓度为15%的氨水，常温搅拌15分钟，得到钨酸铵溶液WO3浓度为295g/L，体积为295mL，钨的直收率为98.22%。
实施例2:
（1）将100g仲钨酸铵固体（WO3质量百分比含量为88.6%）、500mL有机相混合（组成为体积百分比20%N235+10%仲辛醇+70%磺化煤油）与80mL浓度为12mol/L的盐酸在35℃搅拌9分钟，仲钨酸铵的溶解率为100%。
（2）将步骤（1）所得到的物料中加入220mL质量百分比浓度为20%的氢氧化钠，常温搅拌10分钟，得到钨酸钠溶液WO3浓度为296.1g/L，体积为298mL，钨的直收率为99.59%。
实施例3:
（1）将100g三氧化钨固体（WO3质量百分比含量为99.5%）、650mL有机相混合（组成为体积百分比25%N235+10%仲辛醇+70%磺化煤油）与60mL浓度为6mol/L的硫酸在25℃搅拌20分钟，三氧化钨的溶解率为100%。
（2）将步骤（1）所得到的物料中加入250mL质量百分比浓度为20%的氨水，常温搅拌25分钟，得到钨酸铵溶液WO3浓度为313.65g/L，体积为310mL，钨的直收率为97.72%。
尽管已经结合示例性实施例详细描述了本发明的方法， 但是本领域技术人员应该明白， 在不脱离权利要求所限定的精神和范围的情况下， 可以对实施例进行修改。
Claims (1)
1.一种仲钨酸铵/三氧化钨的快速溶解方法，其特征在于具体步骤为：
（1）将萃取剂、调节剂和溶剂混合得到有机相；萃取剂、调节剂和溶剂的体积百分比分别为0.5~85%、0~70%和0~95%；
（2）将100g仲钨酸铵或三氧化钨、500~700mL步骤（1）所得有机相和50~80mL浓度为0.1~18mol/L的酸混合，在0~100℃时搅拌1~20分钟的时间，使得仲钨酸铵或三氧化钨完全溶解，得到溶解后的水相和油相混合料；
（3）向步骤（2）所得混合料中加入200~300mL浓度为0.1~20mol/L的再生剂，常温搅拌10~20分钟，使得有机相再生，同时得到钨酸盐溶液；
（4）分离步骤（3）所得的有机相和钨酸盐溶液，有机相返回溶解工序，钨酸盐溶液作为产品；
所述萃取剂为胺类、季铵盐类、磷酸酯类、醇和酮类中的一种或多种；
所述调节剂为醇、酮和酯类中的一种或多种；
所述溶剂为磺化煤油、煤油、甲苯和260#溶剂油中的一种；
所述酸为盐酸、硫酸、硝酸和磷酸中的一种或多种；
所述再生剂为氢氧化钠、氢氧化钾、氨水、氯化钠和氯化铵中的一种或多种。
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| CN105197997A (zh) * | 2015-09-11 | 2015-12-30 | 中国有色集团（广西）平桂飞碟股份有限公司 | 仲钨酸铵深度纯化除杂的方法 |
| CN105200246A (zh) * | 2015-10-22 | 2015-12-30 | 中南大学 | 一种分离钨钼的方法 |
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| GB1013364A (en) * | 1962-10-26 | 1965-12-15 | Blair Burwell | Extraction of tungsten from tungsten-bearing ores |
| CN87101003A (zh) * | 1987-03-28 | 1988-10-19 | 华东化工学院 | 浸取—萃取联合法 |
| CN102649586A (zh) * | 2012-05-24 | 2012-08-29 | 崇义章源钨业股份有限公司 | 溶解仲钨酸铵和/或氧化钨的方法 |
| CN102942222A (zh) * | 2012-10-28 | 2013-02-27 | 孙世凡 | 一种处理废旧氧化钨制取钨酸铵的方法 |
| CN105197997A (zh) * | 2015-09-11 | 2015-12-30 | 中国有色集团（广西）平桂飞碟股份有限公司 | 仲钨酸铵深度纯化除杂的方法 |
| CN105200246A (zh) * | 2015-10-22 | 2015-12-30 | 中南大学 | 一种分离钨钼的方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109824088A (zh) * | 2019-03-23 | 2019-05-31 | 江西省鑫盛钨业有限公司 | 一种化学纯度不达标的仲钨酸铵不良品提纯的工艺 |
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