CN101367557A - A New Method for Synthesizing Tetraammine Platinum(II) Nitrate - Google Patents
A New Method for Synthesizing Tetraammine Platinum(II) Nitrate Download PDFInfo
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- CN101367557A CN101367557A CNA2008100589561A CN200810058956A CN101367557A CN 101367557 A CN101367557 A CN 101367557A CN A2008100589561 A CNA2008100589561 A CN A2008100589561A CN 200810058956 A CN200810058956 A CN 200810058956A CN 101367557 A CN101367557 A CN 101367557A
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- 238000000034 method Methods 0.000 title claims abstract description 12
- 230000002194 synthesizing effect Effects 0.000 title claims abstract 3
- RBAKORNXYLGSJB-UHFFFAOYSA-N azane;platinum(2+);dinitrate Chemical compound N.N.N.N.[Pt+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O RBAKORNXYLGSJB-UHFFFAOYSA-N 0.000 title abstract description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 9
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 5
- PNCHTLQBARZRSO-UHFFFAOYSA-L azane;platinum(2+);diiodide Chemical compound N.N.[I-].[I-].[Pt+2] PNCHTLQBARZRSO-UHFFFAOYSA-L 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- PZKNFJIOIKQCPA-UHFFFAOYSA-N oxalic acid palladium Chemical compound [Pd].OC(=O)C(O)=O PZKNFJIOIKQCPA-UHFFFAOYSA-N 0.000 claims 3
- NWAHZABTSDUXMJ-UHFFFAOYSA-N platinum(2+);dinitrate Chemical compound [Pt+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O NWAHZABTSDUXMJ-UHFFFAOYSA-N 0.000 claims 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims 1
- 229910052740 iodine Inorganic materials 0.000 claims 1
- 239000011630 iodine Substances 0.000 claims 1
- HRGDZIGMBDGFTC-UHFFFAOYSA-N platinum(2+) Chemical compound [Pt+2] HRGDZIGMBDGFTC-UHFFFAOYSA-N 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- FGHSTPNOXKDLKU-UHFFFAOYSA-N nitric acid;hydrate Chemical compound O.O[N+]([O-])=O FGHSTPNOXKDLKU-UHFFFAOYSA-N 0.000 abstract description 2
- 229910020427 K2PtCl4 Inorganic materials 0.000 abstract 1
- 229910021529 ammonia Inorganic materials 0.000 abstract 1
- FPJNQJHCHVUNTK-UHFFFAOYSA-N platinum;dihydrate Chemical compound O.O.[Pt] FPJNQJHCHVUNTK-UHFFFAOYSA-N 0.000 description 16
- 239000000047 product Substances 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 150000003058 platinum compounds Chemical class 0.000 description 2
- -1 platinum inorganic compound Chemical class 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 229940045985 antineoplastic platinum compound Drugs 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- FVIZARNDLVOMSU-UHFFFAOYSA-N ginsenoside K Natural products C1CC(C2(CCC3C(C)(C)C(O)CCC3(C)C2CC2O)C)(C)C2C1C(C)(CCC=C(C)C)OC1OC(CO)C(O)C(O)C1O FVIZARNDLVOMSU-UHFFFAOYSA-N 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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Abstract
Description
技术领域 technical field
本发明涉及一种重要的铂配合物—硝酸四氨合铂(II)的新合成工艺，属于化学化工领域。The invention relates to a novel synthesis process of an important platinum complex-tetraammine platinum (II) nitrate, belonging to the field of chemistry and chemical engineering.
背景技术 Background technique
硝酸四氨合铂(II)([Pt(NH3)4](NO3)2)是一种重要的铂化合物，它具有水溶性好、溶液化学性质相对稳定，且在受热分解时能直接得到金属铂，是制备铂载体催化剂较理想的前驱体化合物。例如，[Pt(NH3)4](NO3)2用作前驱体化合物可以制备出高活性的Pt/C和Pt/SiO2催化剂(SobczakI.，Ziolek M.，Nowacka M.，Microporousand Mesoporous Materials，(2005)，78(2-3)，103-116；Shih Cheng-Chieh ChangJen-Ray，Materials Chemistry and Physics，(2005)，92(1)，89-97。同时，还可以[Pt(NH3)4](NO3)2为中间体，合成各种铂的化合物。例如，[Pt(NH3)4](NO3)2与氯亚铂酸钾反应生成具有一维导电性质的材料[Pt(NH3)4][PtCl4](Fontana M.，ChanzyH.D.，Caseri W.R.，Chemistry of Materials，2002，14(4)，1730-1735)Tetraammine platinum (II) nitrate ([Pt(NH 3 ) 4 ](NO 3 ) 2 ) is an important platinum compound, which has good water solubility, relatively stable chemical properties of the solution, and can be directly decomposed by heat Metal platinum is obtained, which is an ideal precursor compound for preparing platinum-carrier catalysts. For example, [Pt(NH 3 ) 4 ](NO 3 ) 2 can be used as a precursor compound to prepare highly active Pt/C and Pt/SiO 2 catalysts (SobczakI., Ziolek M., Nowacka M., Microporousand Mesoporous Materials , (2005), 78(2-3), 103-116; Shih Cheng-Chieh ChangJen-Ray, Materials Chemistry and Physics, (2005), 92(1), 89-97. At the same time, [Pt(NH 3 ) 4 ](NO 3 ) 2 as an intermediate to synthesize various platinum compounds. For example, [Pt(NH 3 ) 4 ](NO 3 ) 2 reacts with potassium chloroplatinite to generate materials with one-dimensional conductive properties [Pt(NH 3 ) 4 ][PtCl 4 ] (Fontana M., Chanzy H.D., Caseri WR, Chemistry of Materials, 2002, 14(4), 1730-1735)
[Pt(NH3)4](NO3)2的合成目前文献和专利报道的方法均以[Pt(NH3)4]Cl2为起始原料。Sidorenko Yu.A.，Gerasimova L.K.，Chuprov V.V.(俄罗斯专利申请号RU 2005-140133)报道的方法为：[Pt(NH3)4]Cl2和NH4HCO3反应，得到[Pt(NH3)4](HCO3)2沉淀，将沉淀定量溶于硝酸后浓缩得到产物。另外一种常规的合成是将[Pt(NH3)4]Cl2和AgNO3定量反应后，过滤分离AgCl沉淀后，浓缩母液得到产物。但目前[Pt(NH3)4]Cl2是以K2PtCl4为原料，在一定的温度和pH下与NH4Ac和氨水反应，生成不溶于水的中间体[Pt(NH3)2Cl2]，过滤分离后溶于氨水得到[Pt(NH3)4]Cl2 Synthesis of [Pt(NH 3 ) 4 ](NO 3 ) 2 The methods reported in current literature and patents all use [Pt(NH 3 ) 4 ]Cl 2 as the starting material. The method reported by Sidorenko Yu.A., Gerasimova LK, Chuprov VV (Russian Patent Application No. RU 2005-140133) is: [Pt(NH3) 4 ]Cl 2 reacts with NH 4 HCO 3 to obtain [Pt(NH 3 ) 4 ](HCO 3 ) 2 was precipitated, and the precipitate was quantitatively dissolved in nitric acid and then concentrated to obtain the product. Another conventional synthesis is to quantitatively react [Pt(NH 3 ) 4 ]Cl 2 and AgNO 3 , filter and separate the AgCl precipitate, and concentrate the mother liquor to obtain the product. But at present, [Pt(NH 3 ) 4 ]Cl 2 is made of K 2 PtCl 4 , reacts with NH 4 Ac and ammonia water at a certain temperature and pH to form a water-insoluble intermediate [Pt(NH 3 ) 2 Cl 2 ], filtered and separated, dissolved in ammonia water to obtain [Pt(NH 3 ) 4 ]Cl 2
由K2PtCl4制备中间体[Pt(NH3)2Cl2]非常困难，需严格控制温度和pH值，产率一般不超过70％，现世界上仅有几家大公司如John-Matthey，Merck公司掌握该技术诀窍。所以中间体[Pt(NH3)2Cl2]包括cis-和trans-[Pt(NH3)2Cl2]价格非常昂贵，通过[Pt(NH3)2Cl2]中间体合成[Pt(NH3)4](NO3)2成本相当高，经济上可行性差。It is very difficult to prepare the intermediate [Pt(NH 3 ) 2 Cl 2 ] from K 2 PtCl 4 , and it is necessary to strictly control the temperature and pH value. The yield generally does not exceed 70%. There are only a few large companies in the world such as John-Matthey , Merck has the know-how. Therefore, the intermediate [ Pt (NH 3 ) 2 Cl 2 ] including cis- and trans-[Pt(NH 3 ) 2 Cl 2 ] is very expensive, and [ Pt ( NH 3 ) 4 ](NO 3 ) 2 has a rather high cost and poor economic feasibility.
发明内容 Contents of the invention
本发明的目的是提供一种合成硝酸四氨合铂(II)的新工艺，该工艺是直接以常用的铂的无机化合物K2PtCl4为起始原料，通过三步反应得到[Pt(NH3)4](NO3)2产品。该方法避过了[Pt(NH3)2Cl2]中间体，反应易控制，产率高，得到的产品纯度高。本发明的合成方法是：(1)将K2PtCl4与KI和氨水反应生成顺式-二碘二氨合铂中间体，(2)中间体与硝酸银作用，得到水合物硝酸顺式-二水二氨合铂，(3)水合物和浓氨水反应得到目标产品硝酸四氨合铂(II)。其合成路线和化学反应如下：The purpose of this invention is to provide a new process for the synthesis of tetraammine platinum (II) nitrate, which is directly using the commonly used platinum inorganic compound K 2 PtCl 4 as starting material, and obtains [Pt(NH 3 ) 4 ] (NO 3 ) 2 product. The method avoids the [Pt(NH 3 ) 2 Cl 2 ] intermediate, the reaction is easy to control, the yield is high, and the obtained product has high purity. The synthetic method of the present invention is: (1) K 2 PtCl 4 is reacted with KI and ammoniacal liquor to generate the cis-diiododiammine platinum intermediate, (2) the intermediate reacts with silver nitrate to obtain hydrate nitrate cis- Diammine platinum dihydrate, (3) hydrate and concentrated ammonia water react to obtain the target product tetraammine platinum (II) nitrate. Its synthetic route and chemical reaction are as follows:
K2PtCl4+4KI→K2PtI4+4KClK 2 PtCl 4 +4KI→K 2 PtI 4 +4KCl
K2PtI4+2NH3→cis-[Pt(NH3)2I2]↓+2KIK 2 PtI 4 +2NH 3 →cis-[Pt(NH 3 ) 2 I 2 ]↓+2KI
cis-[Pt(NH3)2I2]+2AgNO3→cis-[Pt(NH3)2(H2O)2](NO3)2+2AgI↓cis-[Pt(NH 3 ) 2 I 2 ]+2AgNO 3 →cis-[Pt(NH 3 ) 2 (H 2 O) 2 ](NO 3 ) 2 +2AgI↓
cis-[Pt(NH3)2(H2O)2](NO3)2+2NH3→[Pt(NH3)4](NO3)2 cis-[Pt(NH 3 ) 2 (H 2 O) 2 ](NO 3 ) 2 +2NH 3 →[Pt(NH 3 ) 4 ](NO 3 ) 2
本发明的特点是采用反应易控制，操作简单，产率高(>90％)，产品纯度99.0％(以金属铂计)，适合规模生产。The present invention is characterized in that the reaction is easy to control, the operation is simple, the yield is high (>90%), the product purity is 99.0% (calculated by metal platinum), and it is suitable for large-scale production.
具体实施方式 Detailed ways
(1)顺式-二碘二氨合铂cis-[Pt(NH3)2I2]中间体的制备(1) Preparation of cis-[Pt(NH 3 ) 2 I 2 ] intermediate of cis-diiododiammine platinum
称取100g K2PtCl4(241mmol)溶于500ml水中，过滤除去不溶物，在45℃下，缓慢加入含KI 240g(1.45mol，过量50％)的水溶液200ml，避光反应4小时后，滴加1：1氨水(过量30％)，得到黄色沉淀，放置2小时，过滤收集，分别用水、乙醇洗涤后在60—70℃下真空干燥4小时，得到cis-[Pt(NH3)2I2]112g，产率96％，铂含量39.7％(计算值40.4％)。Weigh 100g of K 2 PtCl 4 (241mmol) and dissolve it in 500ml of water, filter to remove insoluble matter, slowly add 240g of KI (1.45mol, excess 50%) in 200ml of aqueous solution at 45°C, and react in the dark for 4 hours, drop Add 1:1 ammonia water (excess 30%) to get a yellow precipitate, let it stand for 2 hours, collect by filtration, wash with water and ethanol respectively, and then vacuum dry at 60-70°C for 4 hours to obtain cis-[Pt(NH 3 ) 2 I 2 ] 112 g, yield 96%, platinum content 39.7% (calculated value 40.4%).
(2)[Pt(NH3)4](NO3)2的合成(2) Synthesis of [Pt(NH 3 ) 4 ](NO 3 ) 2
称取100g的cis-[Pt(NH3)2I2](207mmol)，悬浮500ml水中，加入等当量的硝酸银70.3g(414mmol)，在45℃下搅拌反应5小时，检查反应完全后过滤除去AgI沉淀，母液冷冻干燥至近干后，溶于过量的氨水中，在65℃减压浓缩至干，得到白色结晶，再在70℃下进一步真空干燥，得75.5g[Pt(NH3)4](NO3)2产品，产率94％，产品纯度99.2％(以铂含量50.0％计算)。以起始原料K2PtCl4计，产率90.2％，Weigh 100g of cis-[Pt(NH 3 ) 2 I 2 ](207mmol), suspend in 500ml of water, add 70.3g (414mmol) of equivalent silver nitrate, stir and react at 45°C for 5 hours, check the completion of the reaction and filter Remove the AgI precipitate, freeze-dry the mother liquor to nearly dryness, dissolve in excess ammonia water, concentrate to dryness under reduced pressure at 65°C to obtain white crystals, and further vacuum-dry at 70°C to obtain 75.5g [Pt(NH 3 ) 4 ](NO 3 ) 2 product with a yield of 94% and a product purity of 99.2% (calculated based on a platinum content of 50.0%). Based on the starting material K 2 PtCl 4 , the yield is 90.2%,
特征结构参数：<1>元素分析：测定值H4.51％，N21.22％，Pt50.0％与理论值H4.61％，N21.34％，Pt50.4％一致。<2>ESI+-MS：m/e＝132([Pt(NH3)4]2+/2，100％)。<3>IR(cm-1，KBr)：3272(s，v(NH3))，1586(m，δa(HNH))，1384(s，v3(NO3)+δs(HNH))，857(m，p(NH3))，822(m，v3(NO3 -))，508(m，v(Pt-N))。<4>1H NMR(dmso，500MHz)：4.07(12H，4NH3)。这些参数符合[Pt(NH3)4](NO3)2元素组成和化学结构。Characteristic structural parameters: <1>Elemental analysis: measured values H4.51%, N21.22%, Pt50.0% are consistent with theoretical values H4.61%, N21.34%, Pt50.4%. <2>ESI + -MS: m/e=132 ([Pt(NH 3 ) 4 ] 2+ /2, 100%). <3>IR(cm -1 , KBr): 3272(s, v(NH 3 )), 1586(m, δ a (HNH)), 1384(s, v 3 (NO 3 )+δ s (HNH) ), 857(m, p(NH 3 )), 822(m, v 3 (NO 3 - )), 508(m, v(Pt-N)). <4> 1 H NMR (dmso, 500 MHz): 4.07 (12H, 4NH 3 ). These parameters are consistent with the elemental composition and chemical structure of [Pt(NH 3 ) 4 ](NO 3 ) 2 .
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| CN105540685A (en) * | 2016-01-22 | 2016-05-04 | 昆明贵金属研究所 | Method for preparing tetraammineplatinum hydrogen carbonate |
| CN105540685B (en) * | 2016-01-22 | 2017-04-26 | 昆明贵金属研究所 | Method for preparing tetraammineplatinum hydrogen carbonate |
| CN108706642A (en) * | 2018-08-06 | 2018-10-26 | 金川集团股份有限公司 | A kind of preparation method of four amminos bicarbonate palladium |
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| CN110721730A (en) * | 2019-10-16 | 2020-01-24 | 南京劲鸿茂科技有限公司 | Synthetic method and application of platinum compound for exhaust gas purification catalyst |
| CN114106052A (en) * | 2021-11-09 | 2022-03-01 | 昆明贵金属研究所 | Tetranuclear platinum carboxylate, synthetic method and application thereof in preparation of platinum black |
| CN114106052B (en) * | 2021-11-09 | 2023-07-28 | 昆明贵金属研究所 | Tetranuclear platinum carboxylate, synthesis method and its application in the preparation of platinum black |
| CN113979490A (en) * | 2021-11-17 | 2022-01-28 | 西安科技大学 | A kind of method and application of hydrothermal preparation of cubic structure dinitrosodiammine platinum |
| CN114057242A (en) * | 2021-11-17 | 2022-02-18 | 西安科技大学 | A kind of method and application of preparing spherical dinitrosodiammine platinum by hydrothermal method |
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