CN102127117A - Method for preparing dichloro(1,5-cyclooctadiene)platinum(II) - Google Patents
Method for preparing dichloro(1,5-cyclooctadiene)platinum(II) Download PDFInfo
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- CN102127117A CN102127117A CN2010105602860A CN201010560286A CN102127117A CN 102127117 A CN102127117 A CN 102127117A CN 2010105602860 A CN2010105602860 A CN 2010105602860A CN 201010560286 A CN201010560286 A CN 201010560286A CN 102127117 A CN102127117 A CN 102127117A
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Abstract
The invention provides a method for preparing dichloro(1,5-cyclooctadiene)platinum(II) and relates to a method for preparing a platinum group metal compound which is used in an addition reaction of silicon and hydrogen for preparing an organic silicon compound and takes 1,5-cyclooctadiene as the ligand. The method is characterized in that a preparation process comprises reacting potassium chloroplatinite with 1,5-cyclooctadiene (COD) serving as the ligand in mixed solvent of water and normal propyl alcohol to obtain dichloro(1,5-cyclooctadiene)platinum(II) milky precipitate and obtaining the reaction product dichloro(1,5-cyclooctadiene)platinum(II) by suction filtration, washing with absolute ethanol and water and drying, wherein the temperature is controlled to be 60 to 90 DEG C in a reaction process, and the reaction time is 3 to 4 hours. The key technical point of the preparation method provided by the invention is to raise the reaction temperature to 60 to 90 DEG C and reduce the reaction time to 3 to 4 hours from 48 hours reported in documents. Thus, the reaction time is reduced effectively, and raw material waste and environmental damage are reduced.
Description
Technical field
The preparation method of a kind of dichloro (1, the 5-cyclooctadiene) platinum (II) relates to 1 of a kind of addition reaction of silicon with hydrogen that is used to prepare silicoorganic compound, and the 5-cyclooctadiene is the preparation method of the platinum group metal compounds of part.
Background technology
Addition reaction of silicon with hydrogen is the important reaction of preparation silicoorganic compound, and these silicoorganic compound are important raw and processed materials of preparation silane coupling agent, silicon rubber, extraordinary silicone oil and silicone resin etc.The use of platinum catalyst makes the addition reaction of silicon with hydrogen condition become gentle, and productive rate and selectivity improve, thereby have shown good application prospects.As a kind of variable easily ligand, 1, a metal-organic complex of 5-cyclooctadiene (COD) has obtained widespread use, particularly in the organic synthesis of a lot of homogeneous catalysis irreplaceable widespread use is arranged.Dichloro (1, the 5-cyclooctadiene) platinum (II) can be used as the intermediate of monokaryon and multinuclear platinum organic compound except that being used for addition reaction of silicon with hydrogen, also can be applicable in the vapour deposition and antitumor drug of platinum, has important use and is worth and market outlook.
About dichloro (1, the 5-cyclooctadiene) platinum (II) synthetic bibliographical information and few, and be its breadboard preparation of report.These documents are starting raw material with chloro-platinous acid, potassium chloroplatinite or dichloro (DMSO) platinum, or under mild conditions, add auxiliary agent also by the very long reaction times, or under condition of high voltage, synthesize dichloro (1 with part COD reaction, the 5-cyclooctadiene) platinum (II), as seen document J. Organomet. Chem., 1973,59,411-428; Inorg. Synth., 1990,28,346-349; Canadian Journal of Chemistry (1996), 74 (11), 1998-2001; Russian Journal of General Chemistry (Translation of Zhurnal Obshchei Khimii) (1999), 69 (8), 1345. the relevant dichloro (1 that other can find, the 5-cyclooctadiene) document of platinum is nearly more than 1500 piece, all is its character of report and the application in every field.The shortcoming of these methods is: (1) is reflected at when carrying out under the mild conditions, long reaction time; (2) reaction need under high pressure be carried out, and condition is harsh and have certain danger; (3) COD is excessive too many, is difficult for reclaiming or recycle, causes wastage of material and environmental disruption.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, proposes a kind ofly can effectively reduce the reaction times, the preparation method of dichloro (1, the 5-cyclooctadiene) platinum (II) of minimizing wastage of material and environmental disruption.
The objective of the invention is to be achieved through the following technical solutions.
A kind of dichloro (1, the 5-cyclooctadiene) preparation method of platinum (II), it is characterized in that its preparation process with potassium chloroplatinite and ligand 1,5-cyclooctadiene COD reacts in water and n-propyl alcohol mixed solvent, generates dichloro (1, the 5-cyclooctadiene) platinum (II) milky white precipitate, through suction filtration, dehydrated alcohol and water washing, drying obtains reaction product dichloro (1, the 5-cyclooctadiene) platinum (II), the reaction process controlled temperature is 60～90 ℃, reaction 3～4h.
The preparation method of a kind of dichloro of the present invention (1, the 5-cyclooctadiene) platinum (II) is characterized in that potassium chloroplatinite and ligand 1 in the reaction process, and the mol ratio of 5-cyclooctadiene COD is 1.1～2.0:1.
The preparation method of a kind of dichloro of the present invention (1, the 5-cyclooctadiene) platinum (II), the volume ratio that it is characterized in that its n-propyl alcohol and deionized water is 1.0～3.0:1.
A kind of dichloro (1 of the present invention, the 5-cyclooctadiene) preparation method of platinum (II), adopt potassium chloroplatinite, COD, synthetic dichloro (1 in the n-propyl alcohol solvent, the 5-cyclooctadiene) platinum (II), the key of its technology is to improve temperature of reaction to 60～90 ℃, makes time of finishing reaction foreshorten to 3～4h by the 48h of bibliographical information.Effectively reduce the reaction times, reduced wastage of material and environmental disruption.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
The preparation method of a kind of dichloro (1, the 5-cyclooctadiene) platinum (II) is a raw material with potassium chloroplatinite, COD, is solvent with the n-propyl alcohol, the novel method of preparation noble metal catalyst dichloro (1, the 5-cyclooctadiene) platinum (II) under the certain temperature.Concrete grammar comprises:
(ⅰ) (volume ratio is 1.0～3.0:1) to place 50L jacketed glass still, and chuck is imported and exported and connect the circulation oil bath heater, termination prolong on the reactor with a certain amount of n-propyl alcohol and water in the step (ⅰ).Stir, add a certain amount ofly 1,5-cyclooctadiene (COD) treats that temperature rises to 60～90 ℃ ℃, adds a certain amount of potassium chloroplatinite, keeps 60～90 ℃ of oil bath temperatures, reaction 3～4h, milky white precipitate and mother liquor;
(ⅱ) suspension in the step (ⅰ) is cooled to room temperature, vacuum filtration, dehydrated alcohol and deionized water respectively wash three times, obtain solid product dichloro (1, the 5-cyclooctadiene) platinum (II), and weighing also after the drying, calculated yield is 94%～97%.
Embodiment 1
Add the 200ml n-propyl alcohol in the 2L there-necked flask respectively, the 200ml deionized water stirs, add 50ml1,5-cyclooctadiene (COD) treats that oil bath temperature rises to 85 ℃, adds the 50g potassium chloroplatinite, keep 85 ℃ of reactions of oil bath temperature 3.5h, separate out milky white precipitate, be chilled to room temperature, suction filtration, dehydrated alcohol, deionized water wash respectively 3 times, and drying is weighed.Product yield is 94.0%, and results of elemental analyses is C:25.82%, H:3.266%, Pt:52.64%.
Embodiment 2
Concrete detailed rules for the implementation are with example 1, and different is that deionized water is 1L, and n-propyl alcohol 1L, COD are 250ml, and potassium chloroplatinite is 250g, join in the 5L there-necked flask 85 ℃ of reactions of oil bath 3.5h; Product yield is 96.04%; Results of elemental analyses is C:25.15%, H:3.123%, Pt:52.13%.
Embodiment 3
Concrete detailed rules for the implementation are with example 1, and different is that deionized water is 10L, and n-propyl alcohol 10L, COD are 2.0L, and potassium chloroplatinite is 2000g, join in the 50L glass reaction still 85 ℃ of reactions of oil bath 3.5h; Product yield is 95.6%; Results of elemental analyses is C:25.56%, H:3.145%, Pt:52.76%.
Claims (3)
1. dichloro (1, the 5-cyclooctadiene) preparation method of platinum (II), it is characterized in that its preparation process with potassium chloroplatinite and ligand 1,5-cyclooctadiene COD reacts in water and n-propyl alcohol mixed solvent, generates dichloro (1, the 5-cyclooctadiene) platinum (II) milky white precipitate, the shallow lake is through suction filtration, dehydrated alcohol and water washing, and drying obtains reaction product dichloro (1, the 5-cyclooctadiene) platinum (II), the reaction process controlled temperature is 60～90 ℃, reaction 3～4h.
2. the preparation method of a kind of dichloro according to claim 1 (1, the 5-cyclooctadiene) platinum (II) is characterized in that potassium chloroplatinite and ligand 1 in the reaction process, and the mol ratio of 5-cyclooctadiene COD is 1.1～2.0:1.
3. the preparation method of a kind of dichloro according to claim 1 (1, the 5-cyclooctadiene) platinum (II), the volume ratio that it is characterized in that its n-propyl alcohol and deionized water is 1.0～3.0:1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926884A (en) * | 2015-04-23 | 2015-09-23 | 金川集团股份有限公司 | Preparation method of dichloro(1,5-cyclooctadiene) platinum (II) |
| CN106632496A (en) * | 2016-11-29 | 2017-05-10 | 金川集团股份有限公司 | Preparation method of (1,5-cyclooctadiene) rhodium chloride (I) dimers |
| CN108368141A (en) * | 2015-08-27 | 2018-08-03 | 莫门蒂夫性能材料股份有限公司 | Platinum (II) diene complexes with chelating divalent anion ligand and its purposes in hydrosilylation reactions |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101054395A (en) * | 2006-04-11 | 2007-10-17 | 中国科学院福建物质结构研究所 | Platinum metal pyridine complexes with light sensitive and solvent color transition effect |
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2010
- 2010-11-26 CN CN2010105602860A patent/CN102127117A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101054395A (en) * | 2006-04-11 | 2007-10-17 | 中国科学院福建物质结构研究所 | Platinum metal pyridine complexes with light sensitive and solvent color transition effect |
Non-Patent Citations (3)
| Title |
|---|
| 《Journal of Organometallic Chemistry》 19731001 H. C. Clark等, Reactions of (pi-1,5-cyclooctadiene)organoplatinum(II) compounds and the synthesis of perfluoroalkylplatinum complexes 第411-428页 1-3 第59卷, * |
| ANDREW R. L. SKAUGE等,: "High-pressure methods as a tool in organometallic syntheses: facilitation of oxidative addition to platinum(II)", 《CANADIAN JOURNAL OF CHEMISTRY》 * |
| H. C. CLARK等,: "Reactions of (π-1,5-cyclooctadiene)organoplatinum(II) compounds and the synthesis of perfluoroalkylplatinum complexes", 《JOURNAL OF ORGANOMETALLIC CHEMISTRY》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926884A (en) * | 2015-04-23 | 2015-09-23 | 金川集团股份有限公司 | Preparation method of dichloro(1,5-cyclooctadiene) platinum (II) |
| CN108368141A (en) * | 2015-08-27 | 2018-08-03 | 莫门蒂夫性能材料股份有限公司 | Platinum (II) diene complexes with chelating divalent anion ligand and its purposes in hydrosilylation reactions |
| CN106632496A (en) * | 2016-11-29 | 2017-05-10 | 金川集团股份有限公司 | Preparation method of (1,5-cyclooctadiene) rhodium chloride (I) dimers |
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Application publication date: 20110720 |