CN1279012C - 制备乙酸钌(iii)溶液的方法 - Google Patents
制备乙酸钌(iii)溶液的方法 Download PDFInfo
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- CN1279012C CN1279012C CNB971257523A CN97125752A CN1279012C CN 1279012 C CN1279012 C CN 1279012C CN B971257523 A CNB971257523 A CN B971257523A CN 97125752 A CN97125752 A CN 97125752A CN 1279012 C CN1279012 C CN 1279012C
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- Prior art keywords
- ruthenium
- iii
- acetic acid
- hydrazine
- solution
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- Expired - Lifetime
Links
- 238000000034 method Methods 0.000 title claims abstract description 20
- OJLCQGGSMYKWEK-UHFFFAOYSA-K ruthenium(3+);triacetate Chemical compound [Ru+3].CC([O-])=O.CC([O-])=O.CC([O-])=O OJLCQGGSMYKWEK-UHFFFAOYSA-K 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 51
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 11
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052707 ruthenium Inorganic materials 0.000 claims description 10
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 9
- -1 ruthenium (III) carboxylate Chemical class 0.000 claims description 6
- 150000002429 hydrazines Chemical class 0.000 claims description 5
- BPEVHDGLPIIAGH-UHFFFAOYSA-N ruthenium(3+) Chemical compound [Ru+3] BPEVHDGLPIIAGH-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 2
- HDZGCSFEDULWCS-UHFFFAOYSA-N monomethylhydrazine Chemical group CNN HDZGCSFEDULWCS-UHFFFAOYSA-N 0.000 claims description 2
- RADGOBKLTHEUQO-UHFFFAOYSA-N ruthenium(4+) Chemical compound [Ru+4] RADGOBKLTHEUQO-UHFFFAOYSA-N 0.000 claims description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims 3
- 230000002459 sustained effect Effects 0.000 claims 1
- 229960000583 acetic acid Drugs 0.000 description 13
- 239000000243 solution Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- WFDIJRYMOXRFFG-UHFFFAOYSA-N acetic acid anhydride Natural products CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000012362 glacial acetic acid Substances 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 150000004820 halides Chemical class 0.000 description 3
- 239000011541 reaction mixture Substances 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- FGEKTVAHFDQHBU-UHFFFAOYSA-N dioxoruthenium;hydrate Chemical compound O.O=[Ru]=O FGEKTVAHFDQHBU-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 150000003304 ruthenium compounds Chemical class 0.000 description 2
- 229910001927 ruthenium tetroxide Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- GZLCNRXKVBAALW-UHFFFAOYSA-N O=[Ru](=O)=O Chemical compound O=[Ru](=O)=O GZLCNRXKVBAALW-UHFFFAOYSA-N 0.000 description 1
- 229910019891 RuCl3 Inorganic materials 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 159000000021 acetate salts Chemical class 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000012018 catalyst precursor Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- UIEKGNOQMSLELJ-UHFFFAOYSA-N sodium ruthenium(6+) Chemical compound [Ru+6].[Na+] UIEKGNOQMSLELJ-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910009112 xH2O Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table
- C07F15/0006—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table compounds of the platinum group
- C07F15/0046—Ruthenium compounds
- C07F15/0053—Ruthenium compounds without a metal-carbon linkage
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
一种生产乙酸钌(III)溶液的方法，包括将氧化钌(IV)在乙酸存在下与化学计算量的肼还原剂反应。
Description
本发明涉及贵金属化合物的改进。更具体的说，本发明涉及钌化合物的改进和其生产方法。
乙酸钌(III)是一个术语，在本文中将用来描述[Ru3O(OAc)6(H2O)n(AcOH)3-n]OAc(式中n值为0-3)和其去溶剂化处理的产品，即[Ru3O(OAc)6]OAc，以及主要含有乙酸钌(III)、可能混合有较少量其它的钌的乙酸盐、氧化物和/或氢氧化物的产品。尽管乙酸钌(III)不是一种大宗的或商品性的化学品，但乙酸钌(III)本身是已知的，并且可以购买到。它可以作为其它钌化合物的原料，并且已建议作为催化剂或催化剂前体。
通常被认可的制备乙酸钌(III)的方法涉及RuCl3.xH2O与乙酸/乙酸酐或乙酸钠在乙醇中反应，但是这条路线的缺点在于产率很低并且产品被其它钌品种例如[Ru2(OAc)4Cl]以及氯化物和/或钠离子污染。一个可选择的方法是使钌(VIII)氧化物与乙酸和例如乙醛或乙醇的还原剂的混合物进行反应。后一个反应由于钌(VIII)氧化物的爆炸特性而有危险性，尽管这个反应可以指望生产出高纯度的产品。需要提供改进的适于大规模高产率地生产高纯度乙酸钌(III)的方法。已知的方法总是生产出带有例如卤化物之类的杂质和不希望有的金属杂质污染的产品，卤化物杂质促使设备和/或容器腐蚀，不希望有的金属杂质使催化工艺的选择性受损害。另一种不希望的杂质是硫，那是一种著名的催化剂毒剂。
本发明提供用于高产率地生产乙酸钌(III)溶液的方法，包括在乙酸存在下将钌(VI)氧化物与化学计算量的肼还原剂进行反应。
该方法按要求分二个步骤进行，第一步是将钌(IV)在乙酸存在下用肼还原剂还原为钌(III)，然后采用加热，优选用回流加热较长一段时间，例如8～24小时。乙酸反应剂可以是冰醋酸，但优选含水的醋酸，通过将冰醋酸用小比例的水稀释来制备，含水醋酸能够容易地生成优选的乙酸组合物的乙酸钌(III)溶液。
推荐的肼比例是95-115％的化学计算需求量。反应的化学计算量要求1摩尔肼对4摩尔钌，因为肼作为4个电子的还原剂起反应。肼的用量优选为尽可能地接近化学计算量，以避免钌(IV)显著的过-或欠-还原反应。在这个过程中，肼转化为氮气排出。所用的肼优选为水溶液的，还也可以使用净液状的，或者呈固体或溶液形式的肼盐。肼还原剂可以是一种取代的肼，例如甲肼，在这种情况下化学计算量要改变。但是这同样会从取代肼生成不想要的副产品，例如甲胺，污染最终产物。对于某些应用，这样的污染可能无所谓。
可以认为该还原反应用下列的方程式描述：
产物作为溶液可以令人满意地采用冷却反应混合物和用过滤或离心方法除去未反应的钌(IV)氧化物来回收。可以作为固体通过多种本领域的技术人员熟知的方式分离，例如溶液浓缩分离、喷射干燥、或通过低温处理或通过加人合适的溶剂沉淀出化合物。
本发明还提供溶解在乙酸水溶液和杂质例如氮(不大于200ppm)、卤化物(不大于50ppm)含量低的乙酸钌(III)。优选使溶液含有不超过50ppm的硫和不超过100ppm的金属杂质。最令人满意的是使乙酸浓度在40和80％wt.％之间，使钌浓度在4和8wt.％之间。
水合钌(IV)氧化物原料本身是一种已知的化合物，但对于本发明，要求使用醇还原钌(VI)酸钠来制备。钌(VI)酸钠本身是一种已知的材料。
本发明还延伸至其它的羧酸钌上，可以按照类似乙酸盐的方式制备。
本发明通过实施例的方式进一步描述，该实施例只按照如下的方式实施。
实施例1
将如上所述制备的水合氧化钌(IV)(43.88g)转放到250ml烧杯中并与冰醋酸(42.3g)充分混合，再转到一个250ml装备有Teflon涂层的搅拌棒的圆底烧瓶里。悬浮液用另一部分冰醋酸(42.3g)洗涤然后用水(9.0g)洗涤。强烈地搅拌悬浮液然后在10分钟内通过移液管缓慢地加入肼(4.37g的15.26wt.％水溶液)。肼的用量是化学计算量比例的110％，该比例以反应混合物中确定的钌含量为基计。发生强烈的泡腾和逐渐升温大约15℃。将烧瓶装上用于回流的Liebig冷凝器并慢慢加热以便回流，回流持续21小时，在这个期间反应混合物变成了深绿色溶液。停止搅拌并冷却烧瓶，静置24小时。产物用直径7cm玻璃纤维滤布过滤，生成作为钌(III)的一种透明的深绿色产品溶液(141.0g)，含有5.59wt.％的钌(III)。这相应于总产率为98.5％。产品溶液含有小于50ppm卤化物和小于100ppm的氮。
Claims (9)
1、一种生产羧酸钌(III)溶液的方法，该方法包括将氧化钌(IV)在羧酸存在下与肼还原剂反应，其包括在羧酸存在下通过所述的还原剂将钌(IV)还原为钌(III)的第一步骤和将所述的钌(III)加热8至24小时的持续一段时间的第二步骤。
2、权利要求1的方法，其中肼还原剂为取代的肼。
3、权利要求2的方法，其中取代的肼为甲基肼。
4、权利要求1-3任一项的方法，其中羧酸钌(III)为乙酸钌(III)，羧酸为乙酸。
5、权利要求1-3任一项的方法，其中所述的还原剂以95-115％的化学计算量存在。
6、权利要求4的方法，其中所述的还原剂以95-115％的化学计算量存在。
7、权利要求4的方法，其中产生一种溶液，该溶液中钌浓度是4-8重量％，乙酸浓度是40-80重量％。
8、权利要求5的方法，其中产生一种溶液，该溶液中钌浓度是4-8重量％，乙酸浓度是40-80重量％。
9、权利要求6的方法，其中产生一种溶液，该溶液中钌浓度是4-8重量％，乙酸浓度是40-80重量％。
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US031823 | 1987-03-30 | ||
| US3182396P | 1996-11-26 | 1996-11-26 | |
| US031,823 | 1996-11-26 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1191858A CN1191858A (zh) | 1998-09-02 |
| CN1279012C true CN1279012C (zh) | 2006-10-11 |
Family
ID=21861602
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB971257523A Expired - Lifetime CN1279012C (zh) | 1996-11-26 | 1997-11-26 | 制备乙酸钌(iii)溶液的方法 |
Country Status (18)
| Country | Link |
|---|---|
| US (1) | US5886204A (zh) |
| EP (1) | EP0844251B1 (zh) |
| JP (1) | JP3999320B2 (zh) |
| KR (1) | KR100536791B1 (zh) |
| CN (1) | CN1279012C (zh) |
| AR (1) | AR010654A1 (zh) |
| BR (1) | BR9705903A (zh) |
| CA (1) | CA2222119C (zh) |
| DE (1) | DE69714384T2 (zh) |
| ID (1) | ID18998A (zh) |
| MY (1) | MY117386A (zh) |
| NO (1) | NO975429L (zh) |
| NZ (1) | NZ329244A (zh) |
| RU (1) | RU2184119C2 (zh) |
| SA (1) | SA98190044B1 (zh) |
| TW (1) | TW521075B (zh) |
| UA (1) | UA56134C2 (zh) |
| ZA (1) | ZA9710220B (zh) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100406534B1 (ko) * | 2001-05-03 | 2003-11-20 | 주식회사 하이닉스반도체 | 루테늄 박막의 제조 방법 |
| JP5293930B2 (ja) * | 2007-03-22 | 2013-09-18 | Ｊｓｒ株式会社 | 化学気相成長材料及び化学気相成長方法 |
| WO2009116191A1 (ja) * | 2008-03-17 | 2009-09-24 | Jsr株式会社 | ジルテニウム錯体および化学気相成長の材料と方法 |
| DE102007014914B4 (de) * | 2007-03-26 | 2013-09-12 | Heraeus Precious Metals Gmbh & Co. Kg | Katalytisch hochwirksame Edelmetall-Carboxylat-Verbindungen von Ir, Ru, Rh, Pd, Pt und Au |
| CN115141093A (zh) * | 2022-06-28 | 2022-10-04 | 浙江微通催化新材料有限公司 | 一种醋酸钌的制备方法 |
| CN115536520A (zh) * | 2022-11-02 | 2022-12-30 | 金川集团股份有限公司 | 一种醋酸钌的制备方法 |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1405592A (en) * | 1971-08-11 | 1975-09-10 | Johnson Matthey Co Ltd | Compounds of ruthenium |
| JPS63315509A (ja) * | 1987-06-17 | 1988-12-23 | Hitachi Ltd | 蒸発缶の硝酸液処理システム |
-
1997
- 1997-11-12 EP EP97309107A patent/EP0844251B1/en not_active Expired - Lifetime
- 1997-11-12 ZA ZA9710220A patent/ZA9710220B/xx unknown
- 1997-11-12 DE DE69714384T patent/DE69714384T2/de not_active Expired - Lifetime
- 1997-11-13 US US08/969,664 patent/US5886204A/en not_active Expired - Lifetime
- 1997-11-21 JP JP32179597A patent/JP3999320B2/ja not_active Expired - Lifetime
- 1997-11-24 KR KR1019970062382A patent/KR100536791B1/ko not_active IP Right Cessation
- 1997-11-24 NZ NZ329244A patent/NZ329244A/xx unknown
- 1997-11-25 UA UA97115644A patent/UA56134C2/uk unknown
- 1997-11-25 TW TW086117657A patent/TW521075B/zh active
- 1997-11-25 CA CA002222119A patent/CA2222119C/en not_active Expired - Lifetime
- 1997-11-26 AR ARP970105554A patent/AR010654A1/es unknown
- 1997-11-26 MY MYPI97005717A patent/MY117386A/en unknown
- 1997-11-26 ID IDP973767A patent/ID18998A/id unknown
- 1997-11-26 CN CNB971257523A patent/CN1279012C/zh not_active Expired - Lifetime
- 1997-11-26 RU RU97120622/04A patent/RU2184119C2/ru active
- 1997-11-26 NO NO975429A patent/NO975429L/no unknown
- 1997-11-26 BR BR9705903A patent/BR9705903A/pt not_active Application Discontinuation
-
1998
- 1998-05-05 SA SA98190044A patent/SA98190044B1/ar unknown
Also Published As
| Publication number | Publication date |
|---|---|
| KR100536791B1 (ko) | 2006-04-21 |
| SA98190044B1 (ar) | 2006-05-13 |
| US5886204A (en) | 1999-03-23 |
| BR9705903A (pt) | 1999-05-18 |
| ID18998A (id) | 1998-05-28 |
| CA2222119C (en) | 2007-01-30 |
| CA2222119A1 (en) | 1998-05-26 |
| RU2184119C2 (ru) | 2002-06-27 |
| NZ329244A (en) | 1999-02-25 |
| NO975429D0 (no) | 1997-11-26 |
| DE69714384D1 (de) | 2002-09-05 |
| DE69714384T2 (de) | 2002-11-14 |
| KR19980042700A (ko) | 1998-08-17 |
| EP0844251B1 (en) | 2002-07-31 |
| ZA9710220B (en) | 1999-05-12 |
| MY117386A (en) | 2004-06-30 |
| EP0844251A1 (en) | 1998-05-27 |
| UA56134C2 (uk) | 2003-05-15 |
| JP3999320B2 (ja) | 2007-10-31 |
| CN1191858A (zh) | 1998-09-02 |
| JPH10168027A (ja) | 1998-06-23 |
| NO975429L (no) | 1998-05-27 |
| MX9709135A (es) | 1998-09-30 |
| AR010654A1 (es) | 2000-06-28 |
| TW521075B (en) | 2003-02-21 |
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