CN103030178B - 生产四水合仲钨酸铵和高纯度四水合仲钨酸铵的方法 - Google Patents
生产四水合仲钨酸铵和高纯度四水合仲钨酸铵的方法 Download PDFInfo
- Publication number
- CN103030178B CN103030178B CN201310009900.8A CN201310009900A CN103030178B CN 103030178 B CN103030178 B CN 103030178B CN 201310009900 A CN201310009900 A CN 201310009900A CN 103030178 B CN103030178 B CN 103030178B
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- CN
- China
- Prior art keywords
- ammonium paratungstate
- tetrahydrate
- decahydrate
- phase
- ammonium
- 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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- 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 description 13
- 238000000034 method Methods 0.000 title description 37
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 title description 2
- 230000036571 hydration Effects 0.000 title 2
- 238000006703 hydration reaction Methods 0.000 title 2
- -1 ammonium paratungstate tetrahydrate Chemical class 0.000 claims abstract description 44
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 52
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 31
- 229910052721 tungsten Inorganic materials 0.000 claims description 29
- 239000010937 tungsten Substances 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000012071 phase Substances 0.000 claims description 16
- 239000012074 organic phase Substances 0.000 claims description 14
- 229910001868 water Inorganic materials 0.000 claims description 13
- 150000004685 tetrahydrates Chemical class 0.000 claims description 11
- 229910021529 ammonia Inorganic materials 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims description 8
- 239000008346 aqueous phase Substances 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- DKMFARWRZBQGDG-UHFFFAOYSA-N [NH4+].O.O.O.O.O.O.O.O.O.[OH-] Chemical compound [NH4+].O.O.O.O.O.O.O.O.O.[OH-] DKMFARWRZBQGDG-UHFFFAOYSA-N 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 2
- REROKLPNVNAPBD-UHFFFAOYSA-N azane;tetrahydrate Chemical compound N.O.O.O.O REROKLPNVNAPBD-UHFFFAOYSA-N 0.000 claims 6
- 239000013049 sediment Substances 0.000 claims 1
- 238000000926 separation method Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000007900 aqueous suspension Substances 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 23
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 16
- 238000002360 preparation method Methods 0.000 description 16
- 150000004691 decahydrates Chemical class 0.000 description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- 239000012535 impurity Substances 0.000 description 7
- 239000012452 mother liquor Substances 0.000 description 7
- 238000000746 purification Methods 0.000 description 6
- 239000000956 alloy Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 5
- 239000012141 concentrate Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000000622 liquid--liquid extraction Methods 0.000 description 5
- 229910052750 molybdenum Inorganic materials 0.000 description 5
- 238000000638 solvent extraction Methods 0.000 description 5
- 229910052785 arsenic Inorganic materials 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000000113 differential scanning calorimetry Methods 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Inorganic materials [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- YOFPVMWVLDSWKR-UHFFFAOYSA-N 11-methyl-n-(11-methyldodecyl)dodecan-1-amine Chemical compound CC(C)CCCCCCCCCCNCCCCCCCCCCC(C)C YOFPVMWVLDSWKR-UHFFFAOYSA-N 0.000 description 2
- PLLBRTOLHQQAQQ-UHFFFAOYSA-N 8-methylnonan-1-ol Chemical compound CC(C)CCCCCCCO PLLBRTOLHQQAQQ-UHFFFAOYSA-N 0.000 description 2
- 239000004440 Isodecyl alcohol Substances 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 238000005349 anion exchange Methods 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000011777 magnesium Chemical class 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 description 2
- 238000005477 sputtering target Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000002699 waste material Substances 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
- 239000002253 acid Substances 0.000 description 1
- 238000000184 acid digestion Methods 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 238000002419 base digestion Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012527 feed solution Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/60—Compounds characterised by their crystallite size
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
-
- 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
- C01P2006/10—Solid density
-
- 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
- C01P2006/11—Powder tap density
-
- 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)
- Inorganic Compounds Of Heavy Metals (AREA)
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102007005287.3 | 2007-02-02 | ||
| DE102007005287A DE102007005287B4 (de) | 2007-02-02 | 2007-02-02 | Verfahren zur Herstellung von Ammoniumparawolframattetrahydrat und hochreines Ammoniumparawolframattetrahydrat |
| CN2008800039201A CN101600653B (zh) | 2007-02-02 | 2008-01-29 | 生产四水合仲钨酸铵和高纯度四水合仲钨酸铵的方法 |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008800039201A Division CN101600653B (zh) | 2007-02-02 | 2008-01-29 | 生产四水合仲钨酸铵和高纯度四水合仲钨酸铵的方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103030178A CN103030178A (zh) | 2013-04-10 |
| CN103030178B true CN103030178B (zh) | 2015-11-18 |
Family
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Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008800039201A Active CN101600653B (zh) | 2007-02-02 | 2008-01-29 | 生产四水合仲钨酸铵和高纯度四水合仲钨酸铵的方法 |
| CN201310009900.8A Active CN103030178B (zh) | 2007-02-02 | 2008-01-29 | 生产四水合仲钨酸铵和高纯度四水合仲钨酸铵的方法 |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008800039201A Active CN101600653B (zh) | 2007-02-02 | 2008-01-29 | 生产四水合仲钨酸铵和高纯度四水合仲钨酸铵的方法 |
Country Status (8)
| Country | Link |
|---|---|
| US (2) | US8168155B2 (enExample) |
| EP (1) | EP2118018B1 (enExample) |
| JP (2) | JP5361739B2 (enExample) |
| CN (2) | CN101600653B (enExample) |
| DE (1) | DE102007005287B4 (enExample) |
| ES (1) | ES2745085T3 (enExample) |
| PT (1) | PT2118018T (enExample) |
| WO (1) | WO2008092838A1 (enExample) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102007005286B4 (de) | 2007-02-02 | 2009-08-27 | H.C. Starck Gmbh | Verfahren zur Herstellung von Ammoniumparawolframathydraten und Ammoniumparawolframatdekahydrat |
| JP5636142B2 (ja) * | 2009-03-02 | 2014-12-03 | 三菱マテリアル株式会社 | 高純度パラタングステン酸アンモニウムの製造方法 |
| JP4797099B2 (ja) * | 2009-10-01 | 2011-10-19 | Ｊｘ日鉱日石金属株式会社 | 高純度タングステン粉末の製造方法 |
| US9865402B2 (en) | 2013-12-27 | 2018-01-09 | Showa Denko K.K. | Anode body for tungsten capacitors |
| CN109289940B (zh) * | 2018-10-24 | 2021-03-05 | 赣州海创钨业有限公司 | 一种仲钨酸铵生产用离子交换装置 |
| CN111689520B (zh) * | 2020-06-17 | 2023-04-18 | 赣州有色冶金研究所有限公司 | 一种二段真空制备十水合仲钨酸铵的方法 |
| CN113816428A (zh) * | 2021-10-26 | 2021-12-21 | 赣州市海龙钨钼有限公司 | 一种制备仲钨酸铵的工艺 |
| CN113816429B (zh) * | 2021-11-12 | 2023-04-18 | 江西钨业股份有限公司 | 仲钨酸铵的颗粒粗化方法 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4623534A (en) * | 1985-03-21 | 1986-11-18 | Gte Products Corporation | Method for producing ammonium paratungstate |
| CN1377980A (zh) * | 2002-02-06 | 2002-11-06 | 王旭升 | 一种用高钼钨矿制备高纯仲钨酸铵的方法 |
Family Cites Families (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1150962B (de) * | 1959-02-10 | 1963-07-04 | Gen Mills Inc | Verfahren zur Abtrennung von Wolframverbindungen aus waessrigen, wolframhaltigen Loesungen |
| DE1244141B (de) | 1962-10-26 | 1967-07-13 | Blair Burwell | Verfahren zur Herstellung von hochreinem Ammoniumparawolframat |
| US4092400A (en) | 1977-04-11 | 1978-05-30 | Engelhard Minerals & Chemicals Corp. | Process for recovering high purity tungsten compositions from wolframite ores |
| US4115513A (en) | 1977-08-16 | 1978-09-19 | Westinghouse Electric Corp. | Processing of ammonium paratungstate from tungsten ores |
| JPS5761632A (en) * | 1980-10-02 | 1982-04-14 | Toshiba Corp | Production of crude particles of ammonium paratungstenate crystal |
| US4450144A (en) * | 1981-01-19 | 1984-05-22 | Amax Inc. | Ammonium hydroxide stripping of tungsten from organic solvents |
| JPH0227287B2 (ja) * | 1985-11-07 | 1990-06-15 | Nippon Mining Co | Kojundoparatangusutensananmoniumuketsushonoseizohoho |
| JPH07121807B2 (ja) * | 1987-12-25 | 1995-12-25 | 株式会社ジャパンエナジー | 高純度パラタングステン酸アンモニウム結晶の製造方法 |
| US4969336A (en) * | 1989-08-04 | 1990-11-13 | Cryo-Cell International, Inc. | Cryogenic storage apparatus, particularly with automatic retrieval |
| DE19724183C2 (de) | 1996-07-05 | 1999-03-25 | Starck H C Gmbh Co Kg | Verfahren zur Herstellung reiner Alkali- und/oder Ammonium-Wolframat-Lösungen |
| DE19628816A1 (de) | 1996-07-17 | 1998-01-22 | Sawatzki Viktor | Verfahren zur Herstellung von Parawolframat |
| JP2005126321A (ja) * | 2003-09-30 | 2005-05-19 | Jfe Mineral Co Ltd | タングステン酸アンモニウムの製造方法 |
| DE102007005286B4 (de) * | 2007-02-02 | 2009-08-27 | H.C. Starck Gmbh | Verfahren zur Herstellung von Ammoniumparawolframathydraten und Ammoniumparawolframatdekahydrat |
-
2007
- 2007-02-02 DE DE102007005287A patent/DE102007005287B4/de active Active
-
2008
- 2008-01-29 CN CN2008800039201A patent/CN101600653B/zh active Active
- 2008-01-29 CN CN201310009900.8A patent/CN103030178B/zh active Active
- 2008-01-29 EP EP08708317.6A patent/EP2118018B1/de active Active
- 2008-01-29 PT PT08708317T patent/PT2118018T/pt unknown
- 2008-01-29 JP JP2009547659A patent/JP5361739B2/ja active Active
- 2008-01-29 US US12/524,968 patent/US8168155B2/en active Active
- 2008-01-29 ES ES08708317T patent/ES2745085T3/es active Active
- 2008-01-29 WO PCT/EP2008/051000 patent/WO2008092838A1/de not_active Ceased
-
2010
- 2010-11-12 US US12/945,038 patent/US8226923B2/en active Active
-
2013
- 2013-07-08 JP JP2013143060A patent/JP5940025B2/ja active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4623534A (en) * | 1985-03-21 | 1986-11-18 | Gte Products Corporation | Method for producing ammonium paratungstate |
| CN1377980A (zh) * | 2002-02-06 | 2002-11-06 | 王旭升 | 一种用高钼钨矿制备高纯仲钨酸铵的方法 |
Non-Patent Citations (2)
| Title |
|---|
| A re-investigation of the thermal decomposition of ammonium paratungstate;G. J. FRENCH et al;《JOURNAL OF MATERIALS SCIENCE 》;19811231;第16卷;3427-3436页 * |
| In Situ XAS and XRD Studies on the Structural Evolution of Ammonium Paratungstate During Thermal Decomposition;Olga Kirilenko et al;《Eur. J. Inorg. Chem》;20051231;第2005卷(第11期);第2125-2126页以及图3 * |
Also Published As
| Publication number | Publication date |
|---|---|
| EP2118018B1 (de) | 2019-06-26 |
| JP2010517903A (ja) | 2010-05-27 |
| US20110070148A1 (en) | 2011-03-24 |
| JP2013212985A (ja) | 2013-10-17 |
| CN103030178A (zh) | 2013-04-10 |
| DE102007005287A1 (de) | 2008-08-14 |
| CN101600653A (zh) | 2009-12-09 |
| WO2008092838A1 (de) | 2008-08-07 |
| US8226923B2 (en) | 2012-07-24 |
| DE102007005287B4 (de) | 2009-10-01 |
| PT2118018T (pt) | 2019-09-17 |
| CN101600653B (zh) | 2013-07-17 |
| EP2118018A1 (de) | 2009-11-18 |
| ES2745085T3 (es) | 2020-02-27 |
| JP5361739B2 (ja) | 2013-12-04 |
| US8168155B2 (en) | 2012-05-01 |
| US20100028250A1 (en) | 2010-02-04 |
| JP5940025B2 (ja) | 2016-06-29 |
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