JP5065012B2 - タングステン酸およびその製造方法 - Google Patents
タングステン酸およびその製造方法 Download PDFInfo
- Publication number
- JP5065012B2 JP5065012B2 JP2007511967A JP2007511967A JP5065012B2 JP 5065012 B2 JP5065012 B2 JP 5065012B2 JP 2007511967 A JP2007511967 A JP 2007511967A JP 2007511967 A JP2007511967 A JP 2007511967A JP 5065012 B2 JP5065012 B2 JP 5065012B2
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- JP
- Japan
- Prior art keywords
- tungstic acid
- acid
- powder
- alkali metal
- tungstate
- 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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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/02—Oxides; Hydroxides
-
- 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
Description
以下の例中で製造されるタングステン酸は、種々の化学的および物理的性質に関して、例に示すようにして試験する。別記しない限りにおいて、使用される方法は以下のとおりである:
平均粒径(D50値)を、レーザー偏向によって、MasterSizer Sμ(MALVERN (ASTM B 822))によって測定し、かつ、かさ密度をASTM B 329にしたがって測定した。%は別記しない限りは、質量%である。
2個の撹拌槽反応器(反応器1および2)を含む沈澱装置を、球状のタングステン酸を連続的に沈澱させるために使用し、その際、反応器1からのオーバーフローを直接的に反応器2中に導入し、かつ反応器2からのオーバーフローを生成物懸濁液として回収した。
W:73.35%
Na:0.13%
硫酸塩:6080ppm
D50:11.84μm
かさ密度:2.1g/cm3
比重びん密度(Pycnometric density):5.38g/cm3
450℃までの乾燥損失量(熱重量測定法):7.8%
図1および2は、この方法で製造されたタングステン酸の走査型電子顕微鏡画像を示す(図1:500倍の倍率、図2:5000倍の倍率)。個々の粉末粒子は、球状の形態を示すことが明らかにみてとれる。
この例のために選択された沈澱温度は20℃であり、すべての他のパラメータは本発明による例1と同一であった。このようにして得られたタングステン酸は、困難をもってのみ濾過することができ、例1によって得られた生成物よりも顕著に粗いものであった。
例1による方法を、母液から分離された生成物を脱イオン水で80℃の温度で洗浄せず、希釈された硫酸(1lの脱イオン水中7mlの濃H2SO4)で80℃の温度で洗浄することを除いて同様に実施した。この方法で得られた球状のタングステン酸のNa含量は、233ppmのみであった。
タングステン酸を例1で示した条件下で、2個の反応器のカスケード中ではなく、単一の反応器中で反応を実施することを除いて、同様に沈澱させた。ここでは、例1中では必然的なタングステン酸ナトリウム溶液の分配を省略すべきであり、かつさらに、計量供給量を、単一の反応器中の滞留時間が、例1の反応器1および2中のすべての滞留時間と同等であるように調整した。この場合においても、球状の生成物が得られる。D50値は10.37μmであった。
Claims (10)
- 水性タングステン酸アルカリ金属塩溶液を鉱酸と、鉱酸とタングステンとのモル比が9:1〜4:1で、50〜103℃の温度で反応させることによって、ASTM B329によるかさ密度が少なくとも1.5g/cm3である、化学式H2WO4で表される球状の形態のタングステン酸粉末を製造する方法。
- 反応を70〜100℃で実施することを特徴とする、請求項1に記載の方法。
- 反応を、連続的に、連続する撹拌槽または少なくとも2個の連続する撹拌槽のカスケード中で実施する、請求項1または2に記載の方法。
- 水性タングステン酸ナトリウム溶液を、タングステン酸アルカリ金属塩溶液として使用する、請求項1から3までのいずれか1項に記載の方法。
- 50〜70質量%のH2SO4含量を有する水性硫酸を、鉱酸として使用する、請求項1から4までのいずれか1項に記載の方法。
- 反応チャンバー中の滞留時間が4〜6時間である、請求項1から5までのいずれか1項に記載の方法。
- ASTM B329によるかさ密度が、少なくとも1.5g/cm3である、化学式H2WO4で表される球状の形態のタングステン酸粉末。
- ASTM B822によって測定された平均粒径D50が3〜80μmである、請求項7に記載のタングステン酸粉末。
- アルカリ金属不純物の量が<0.5質量%である、請求項7または8に記載のタングステン酸粉末。
- タングステン金属粉末を製造するための、請求項7から9までのいずれか1項に記載のタングステン酸粉末の使用。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102004023068.4 | 2004-05-11 | ||
DE102004023068A DE102004023068B4 (de) | 2004-05-11 | 2004-05-11 | Wolframsäure und Verfahren zu deren Herstellung |
PCT/EP2005/004550 WO2005110923A1 (de) | 2004-05-11 | 2005-04-28 | Wolframsäurepulver bestehend aus sphärischen wolframsäurepartikeln und verfahren zu deren herstellung |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2007537121A JP2007537121A (ja) | 2007-12-20 |
JP5065012B2 true JP5065012B2 (ja) | 2012-10-31 |
Family
ID=34965040
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2007511967A Active JP5065012B2 (ja) | 2004-05-11 | 2005-04-28 | タングステン酸およびその製造方法 |
Country Status (10)
Country | Link |
---|---|
US (2) | US8052956B2 (ja) |
EP (1) | EP1758823B1 (ja) |
JP (1) | JP5065012B2 (ja) |
AU (1) | AU2005243988B2 (ja) |
CA (1) | CA2566293C (ja) |
DE (1) | DE102004023068B4 (ja) |
ES (1) | ES2608611T3 (ja) |
PT (1) | PT1758823T (ja) |
RU (2) | RU2389690C2 (ja) |
WO (1) | WO2005110923A1 (ja) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9662611B2 (en) * | 2009-04-03 | 2017-05-30 | Basf Corporation | Emissions treatment system with ammonia-generating and SCR catalysts |
WO2014097698A1 (ja) * | 2012-12-17 | 2014-06-26 | 昭和電工株式会社 | タングステン微粉の製造方法 |
KR20190129762A (ko) * | 2018-05-11 | 2019-11-20 | 엘지전자 주식회사 | 전이금속산화물 미세입자 제조 방법 |
KR102494017B1 (ko) * | 2020-12-02 | 2023-01-31 | 베스트알 주식회사 | 텅스텐산 융합체 및 이를 이용하여 제조된 텅스텐 산화물 |
Family Cites Families (29)
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US1683695A (en) * | 1927-03-29 | 1928-09-11 | Silica Gel Corp | Method of preparing tungsten oxide gel |
US1972136A (en) * | 1933-03-28 | 1934-09-04 | Westinghouse Lamp Co | Precipitation of tungstic oxide |
US2366250A (en) * | 1941-02-20 | 1945-01-02 | Gen Electric | Method for purifying tungstic acid |
US2316583A (en) * | 1941-08-06 | 1943-04-13 | Westinghouse Electric & Mfg Co | Manufacture of tungstic acid |
US2368580A (en) * | 1941-10-25 | 1945-01-30 | Merck & Co Inc | Processes for the production of tungstic acid |
US2968527A (en) * | 1957-10-03 | 1961-01-17 | Columbia Southern Chem Corp | Method of recovering tungstic acid values from aqueous media |
US2993755A (en) * | 1958-08-13 | 1961-07-25 | Union Carbide Corp | Preparation of tungstic oxide |
US3193347A (en) * | 1962-06-13 | 1965-07-06 | Sherritt Gordon Mines Ltd | Process for the production of tungstic acid |
NL6504827A (ja) * | 1965-04-15 | 1966-10-17 | ||
GB1175834A (en) * | 1966-04-07 | 1969-12-23 | Atomic Energy Authority Uk | Improvements in or relating to the Chemical Production of Metal-Containing Materials as Particles and other Configurations |
GB1350389A (en) * | 1970-08-26 | 1974-04-18 | Atomic Energy Authority Uk | Processes for precipitating metal compounds |
CA1068071A (en) * | 1976-01-29 | 1979-12-18 | Hans P. Kasserra | Process for the manufacture of ammonium and alkali metal tungstates |
CA1068072A (en) * | 1976-01-29 | 1979-12-18 | Du Pont Canada Inc. | Process for the manufacture of ammonium tungstate from reduced alkaline earth metal tungstates |
CA1068070A (en) * | 1976-01-29 | 1979-12-18 | Hans P. Kasserra | Treatment of tri(alkaline earth metal) tungstates with acids |
CA1080440A (en) * | 1976-01-29 | 1980-07-01 | Denis B. Kelly | Process for the manufacture of ammonium tungstate from tungstates of alkaline earth metals |
DD148522B1 (de) | 1979-12-29 | 1983-07-27 | Gerd Baier | Verfahren zur herstellung von wolframsaeure aus wolframhaltigem schrott |
US4339424A (en) * | 1981-03-20 | 1982-07-13 | Exxon Research & Engineering Co. | Method of preparing W or Mo metal oxides |
US4675167A (en) | 1983-03-07 | 1987-06-23 | Mitsubishi Jukogyo Kabushiki Kaisha | Method of treating exhaust gases |
US4629503A (en) * | 1985-04-17 | 1986-12-16 | Ramot - University Authority For Applied Research And Industrial Development | Process for the recovery of tungsten in a pure form from tungsten-containing materials |
HU203132B (en) | 1985-10-15 | 1991-05-28 | Mta Mueszaki Fiz Kutato Inteze | Process for producing purified volfram and/or molybden isopolyacids or salts from impure alkalic volfram and/or molybden metal-salt solutions |
JPS63182218A (ja) * | 1987-01-21 | 1988-07-27 | Toshiba Corp | Ecd用高純度タングステン酸化物又はモリブデン酸化物 |
GB2218651A (en) * | 1988-05-18 | 1989-11-22 | British Nuclear Fuels Plc | Solvent extraction contactors |
JP2834199B2 (ja) * | 1989-07-21 | 1998-12-09 | 触媒化成工業株式会社 | タングステン超微粒子の製造方法 |
US5192365A (en) * | 1991-06-06 | 1993-03-09 | Engelhard Corporation | Buff rutile pigment compositions |
JP3415716B2 (ja) * | 1996-03-12 | 2003-06-09 | 株式会社資生堂 | 紫外線遮蔽剤及び紫外線遮蔽効果を有する皮膚外用剤 |
RU2173300C1 (ru) * | 2000-01-05 | 2001-09-10 | ОАО "Забайкальский горно-обогатительный комбинат" | Способ переработки вольфрамсодержащих концентратов с получением вольфрамовой кислоты |
JP3899237B2 (ja) * | 2001-03-30 | 2007-03-28 | 株式会社アライドマテリアル | 微粒タングステン酸化物とその製造方法 |
CN1470656A (zh) * | 2002-07-26 | 2004-01-28 | 四川自贡特种金属制粉厂 | 利用白钨矿粉生产钨酸的方法 |
ES2380691T3 (es) | 2003-04-22 | 2012-05-17 | R.T. Vanderbilt Company, Inc. | Composiciones de aceite lubricante que comprenden wolframato de di-tridecilamonio |
-
2004
- 2004-05-11 DE DE102004023068A patent/DE102004023068B4/de not_active Expired - Lifetime
-
2005
- 2005-04-28 EP EP05733951.7A patent/EP1758823B1/de active Active
- 2005-04-28 RU RU2006143543/15A patent/RU2389690C2/ru active
- 2005-04-28 ES ES05733951.7T patent/ES2608611T3/es active Active
- 2005-04-28 RU RU2009130566/05A patent/RU2525548C2/ru active
- 2005-04-28 PT PT57339517T patent/PT1758823T/pt unknown
- 2005-04-28 WO PCT/EP2005/004550 patent/WO2005110923A1/de active Application Filing
- 2005-04-28 US US11/579,775 patent/US8052956B2/en active Active
- 2005-04-28 JP JP2007511967A patent/JP5065012B2/ja active Active
- 2005-04-28 AU AU2005243988A patent/AU2005243988B2/en active Active
- 2005-04-28 CA CA2566293A patent/CA2566293C/en active Active
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2011
- 2011-09-23 US US13/241,750 patent/US8454931B2/en active Active
Also Published As
Publication number | Publication date |
---|---|
RU2525548C2 (ru) | 2014-08-20 |
RU2009130566A (ru) | 2011-02-20 |
ES2608611T3 (es) | 2017-04-12 |
DE102004023068A1 (de) | 2005-12-15 |
DE102004023068B4 (de) | 2008-06-19 |
WO2005110923A1 (de) | 2005-11-24 |
PT1758823T (pt) | 2016-12-07 |
US20120045647A1 (en) | 2012-02-23 |
US8052956B2 (en) | 2011-11-08 |
EP1758823B1 (de) | 2016-10-12 |
RU2389690C2 (ru) | 2010-05-20 |
RU2006143543A (ru) | 2008-06-20 |
AU2005243988B2 (en) | 2011-03-10 |
EP1758823A1 (de) | 2007-03-07 |
US20070224096A1 (en) | 2007-09-27 |
US8454931B2 (en) | 2013-06-04 |
CA2566293A1 (en) | 2005-11-24 |
AU2005243988A1 (en) | 2005-11-24 |
CA2566293C (en) | 2014-04-01 |
JP2007537121A (ja) | 2007-12-20 |
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