CN103395847A - 硫酸四氨合钯的合成方法 - Google Patents
硫酸四氨合钯的合成方法 Download PDFInfo
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- CN103395847A CN103395847A CN2013103124228A CN201310312422A CN103395847A CN 103395847 A CN103395847 A CN 103395847A CN 2013103124228 A CN2013103124228 A CN 2013103124228A CN 201310312422 A CN201310312422 A CN 201310312422A CN 103395847 A CN103395847 A CN 103395847A
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- Prior art keywords
- palladium
- sulfuric acid
- solution
- reaction
- palladous
- 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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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000010189 synthetic method Methods 0.000 title claims abstract description 16
- 229910052763 palladium Inorganic materials 0.000 title abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 60
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- NXJCBFBQEVOTOW-UHFFFAOYSA-L palladium(2+);dihydroxide Chemical compound O[Pd]O NXJCBFBQEVOTOW-UHFFFAOYSA-L 0.000 claims abstract description 12
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims abstract description 11
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 15
- RFLFDJSIZCCYIP-UHFFFAOYSA-L palladium(2+);sulfate Chemical compound [Pd+2].[O-]S([O-])(=O)=O RFLFDJSIZCCYIP-UHFFFAOYSA-L 0.000 claims description 14
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 230000009286 beneficial effect Effects 0.000 claims description 5
- 150000002941 palladium compounds Chemical class 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 238000001514 detection method Methods 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 2
- 239000002893 slag Substances 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 229910002651 NO3 Inorganic materials 0.000 abstract 1
- 239000000908 ammonium hydroxide Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 15
- 239000007788 liquid Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 125000003963 dichloro group Chemical group Cl* 0.000 description 3
- 238000009713 electroplating Methods 0.000 description 3
- 241000370738 Chlorion Species 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 2
- 235000011130 ammonium sulphate Nutrition 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical class [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 description 2
- JQPTYAILLJKUCY-UHFFFAOYSA-N palladium(ii) oxide Chemical compound [O-2].[Pd+2] JQPTYAILLJKUCY-UHFFFAOYSA-N 0.000 description 2
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Catalysts (AREA)
Abstract
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CN103395847A true CN103395847A (zh) | 2013-11-20 |
CN103395847B CN103395847B (zh) | 2016-07-06 |
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Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104028774A (zh) * | 2014-06-11 | 2014-09-10 | 励福实业(江门)贵金属有限公司 | 活化钯粉及其制备方法和应用 |
CN106430334A (zh) * | 2016-11-16 | 2017-02-22 | 重庆材料研究院有限公司 | 一种硝酸钯溶液的制备方法 |
CN108706642A (zh) * | 2018-08-06 | 2018-10-26 | 金川集团股份有限公司 | 一种四氨合碳酸氢钯的制备方法 |
CN108946829A (zh) * | 2018-08-06 | 2018-12-07 | 金川集团股份有限公司 | 一种硫酸四氨钯的电渗析制备方法 |
CN109609783A (zh) * | 2018-12-22 | 2019-04-12 | 励福(江门)环保科技股份有限公司 | 一种从含钯、铑合金的合金片中高效分离提纯钯和铑的方法 |
CN110482620A (zh) * | 2019-08-27 | 2019-11-22 | 贵研铂业股份有限公司 | 一种可量产硫酸四氨钯的精制方法 |
CN110776022A (zh) * | 2019-09-23 | 2020-02-11 | 励福(江门)环保科技股份有限公司 | 一种二氯四氨钯固体结晶的制备方法 |
CN111732133A (zh) * | 2020-06-17 | 2020-10-02 | 中船重工黄冈贵金属有限公司 | 一种硫酸四氨钯的制备方法 |
CN112169811A (zh) * | 2020-10-27 | 2021-01-05 | 金川集团股份有限公司 | 一种硫酸钯溶液的制备方法 |
CN112897600A (zh) * | 2021-03-15 | 2021-06-04 | 徐州浩通新材料科技股份有限公司 | 一种硫酸四氨钯(ⅱ)的制备方法 |
CN114702527A (zh) * | 2022-03-08 | 2022-07-05 | 徐州浩通新材料科技股份有限公司 | 一种由钯粉制备硫酸乙二胺钯(ⅱ)的方法 |
CN114773181A (zh) * | 2022-03-08 | 2022-07-22 | 徐州浩通新材料科技股份有限公司 | 一种水合双草酸根钯(ⅱ)酸的制备方法 |
CN115872465A (zh) * | 2022-10-13 | 2023-03-31 | 浙江凯大催化新材料有限公司 | 一种低卤素低碱金属含量的硝酸钯溶液的制备方法及其应用 |
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EP1057902A2 (en) * | 1999-06-01 | 2000-12-06 | Lucent Technologies Inc. | Improved process for synthesizing a palladium replenisher for electroplating baths |
CN101362781A (zh) * | 2008-09-24 | 2009-02-11 | 昆明贵金属研究所 | 草酸四氨合钯(ⅱ)的合成方法 |
CN102242276A (zh) * | 2011-06-13 | 2011-11-16 | 白银万山稀贵金属科技有限责任公司 | 从工业固体废料中提取贵金属钯的工艺 |
CN102616869A (zh) * | 2012-04-07 | 2012-08-01 | 昆明贵金属研究所 | 一种硫酸四氨合钯的合成方法 |
-
2013
- 2013-07-24 CN CN201310312422.8A patent/CN103395847B/zh active Active
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EP1057902A2 (en) * | 1999-06-01 | 2000-12-06 | Lucent Technologies Inc. | Improved process for synthesizing a palladium replenisher for electroplating baths |
CN101362781A (zh) * | 2008-09-24 | 2009-02-11 | 昆明贵金属研究所 | 草酸四氨合钯(ⅱ)的合成方法 |
CN102242276A (zh) * | 2011-06-13 | 2011-11-16 | 白银万山稀贵金属科技有限责任公司 | 从工业固体废料中提取贵金属钯的工艺 |
CN102616869A (zh) * | 2012-04-07 | 2012-08-01 | 昆明贵金属研究所 | 一种硫酸四氨合钯的合成方法 |
Non-Patent Citations (2)
Title |
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R. ESKENAZI, ET AL.: "SULPHATO COMPLEXES OF PALLADIUM (II)", 《J. INORG. NUCL. CHEM.》 * |
余建民: "《贵金属化合物及配合物合成手册》", 28 February 2009, 化学工业出版社 * |
Cited By (19)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104028774A (zh) * | 2014-06-11 | 2014-09-10 | 励福实业(江门)贵金属有限公司 | 活化钯粉及其制备方法和应用 |
CN106430334A (zh) * | 2016-11-16 | 2017-02-22 | 重庆材料研究院有限公司 | 一种硝酸钯溶液的制备方法 |
CN108706642A (zh) * | 2018-08-06 | 2018-10-26 | 金川集团股份有限公司 | 一种四氨合碳酸氢钯的制备方法 |
CN108946829A (zh) * | 2018-08-06 | 2018-12-07 | 金川集团股份有限公司 | 一种硫酸四氨钯的电渗析制备方法 |
CN109609783B (zh) * | 2018-12-22 | 2020-11-10 | 励福(江门)环保科技股份有限公司 | 一种从含钯、铑合金的合金片中高效分离提纯钯和铑的方法 |
CN109609783A (zh) * | 2018-12-22 | 2019-04-12 | 励福(江门)环保科技股份有限公司 | 一种从含钯、铑合金的合金片中高效分离提纯钯和铑的方法 |
CN110482620B (zh) * | 2019-08-27 | 2021-10-22 | 贵研铂业股份有限公司 | 一种可量产硫酸四氨钯的精制方法 |
CN110482620A (zh) * | 2019-08-27 | 2019-11-22 | 贵研铂业股份有限公司 | 一种可量产硫酸四氨钯的精制方法 |
CN110776022A (zh) * | 2019-09-23 | 2020-02-11 | 励福(江门)环保科技股份有限公司 | 一种二氯四氨钯固体结晶的制备方法 |
CN111732133A (zh) * | 2020-06-17 | 2020-10-02 | 中船重工黄冈贵金属有限公司 | 一种硫酸四氨钯的制备方法 |
CN112169811A (zh) * | 2020-10-27 | 2021-01-05 | 金川集团股份有限公司 | 一种硫酸钯溶液的制备方法 |
CN112897600A (zh) * | 2021-03-15 | 2021-06-04 | 徐州浩通新材料科技股份有限公司 | 一种硫酸四氨钯(ⅱ)的制备方法 |
CN112897600B (zh) * | 2021-03-15 | 2021-11-19 | 徐州浩通新材料科技股份有限公司 | 一种硫酸四氨钯(ⅱ)的制备方法 |
CN114702527A (zh) * | 2022-03-08 | 2022-07-05 | 徐州浩通新材料科技股份有限公司 | 一种由钯粉制备硫酸乙二胺钯(ⅱ)的方法 |
CN114773181A (zh) * | 2022-03-08 | 2022-07-22 | 徐州浩通新材料科技股份有限公司 | 一种水合双草酸根钯(ⅱ)酸的制备方法 |
CN114702527B (zh) * | 2022-03-08 | 2024-06-04 | 徐州浩通新材料科技股份有限公司 | 一种由钯粉制备硫酸乙二胺钯(ⅱ)的方法 |
CN114773181B (zh) * | 2022-03-08 | 2024-06-11 | 徐州浩通新材料科技股份有限公司 | 一种水合双草酸根钯(ⅱ)酸的制备方法 |
CN115872465A (zh) * | 2022-10-13 | 2023-03-31 | 浙江凯大催化新材料有限公司 | 一种低卤素低碱金属含量的硝酸钯溶液的制备方法及其应用 |
CN115872465B (zh) * | 2022-10-13 | 2023-11-03 | 浙江凯大催化新材料有限公司 | 一种低卤素低碱金属含量的硝酸钯溶液的制备方法及其应用 |
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