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Method for preparing dichloro(1,5-cyclooctadiene)platinum(II)

A technology for the preparation of cyclooctadiene, which is applied in the field of preparation of dichloro(1,5-cyclooctadiene) platinum (II), can solve the problems of waste of raw materials, environmental damage, harsh conditions and dangers, and achieve Reduce reaction time, reduce waste of raw materials, and reduce environmental damage

Inactive Publication Date: 2011-07-20
JINCHUAN GROUP LIMITED
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Problems solved by technology

The disadvantages of these methods are: (1) When the reaction is carried out under mild conditions, the reaction time is long; (2) The reaction needs to be carried out under high pressure, which is harsh and has certain dangers; (3) The excess of COD is too much and it is not easy to recover or recycling, resulting in waste of raw materials and environmental damage

Method used

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  • Method for preparing dichloro(1,5-cyclooctadiene)platinum(II)
  • Method for preparing dichloro(1,5-cyclooctadiene)platinum(II)

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preparation example Construction

[0011] A kind of preparation method of dichloro (1,5-cyclooctadiene) platinum (II), with potassium chloroplatinite, COD as raw material, with n-propanol as solvent, prepare noble metal catalyst dichloro (1 ,5-cyclooctadiene) a new method for platinum(II). Specific methods include:

[0012] (ⅰ) Put a certain amount of n-propanol and water (volume ratio 1.0 to 3.0:1) in step (ⅰ) in a 50L jacketed glass reactor, the inlet and outlet of the jacket are connected to the circulating oil bath heater, and the reactor The upper end is connected to the condenser tube. Stir evenly, add a certain amount of 1,5-cyclooctadiene (COD), wait for the temperature to rise to 60-90°C, add a certain amount of potassium chloroplatinite, maintain the oil bath temperature at 60-90°C, and react for 3- 4h, milky white precipitate and mother liquor were obtained;

[0013] (ii) Cool the suspension in step (i) to room temperature, vacuum filter, wash with absolute ethanol and deionized water three times ...

Embodiment 1

[0015] Add 200ml of n-propanol and 200ml of deionized water into a 2L three-necked flask, stir well, add 50ml of 1,5-cyclooctadiene (COD), wait until the temperature of the oil bath rises to 85°C, add 50g of potassium chloroplatinite, keep The oil bath temperature was 85°C for 3.5 hours, and a milky white precipitate was precipitated, cooled to room temperature, filtered with suction, washed with absolute ethanol and deionized water three times, dried and weighed. The product yield is 94.0%, and the elemental analysis results are C: 25.82%, H: 3.266%, and Pt: 52.64%.

Embodiment 2

[0017] The specific implementation rules are the same as in Example 1, except that 1L of deionized water, 1L of n-propanol, 250ml of COD, and 250g of potassium chloroplatinite are added to a 5L three-necked flask and reacted in an oil bath at 85°C for 3.5h; The yield was 96.04%; the elemental analysis results were C: 25.15%, H: 3.123%, and Pt: 52.13%.

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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 [0001] A preparation method of dichloro(1,5-cyclooctadiene) platinum (II), which relates to a method for preparing organosilicon compounds using 1,5-cyclooctadiene as a ligand in the hydrosilylation reaction Preparation method of platinum group metal compound. Background technique [0002] The hydrosilylation reaction is an important reaction for the preparation of organosilicon compounds, which are important raw materials for the preparation of silane coupling agents, silicone rubber, special silicone oils and silicone resins. The use of platinum catalysts makes the hydrosilylation reaction conditions milder, and the yield and selectivity are improved, thus showing a good application prospect. As a readily variable ligand, metal-organic complexes of 1,5-cyclooctadiene (COD) have been widely used, especially in many homogeneously catalyzed organic syntheses. Dichloro(1,5-cyclooctadiene) platinum (II) can be used as an intermediate of mononuclear and multinu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00
Inventor 易镇芳王艳艳张静郭守杰刘国旗辛冰王红梅冯燕马正明石秀龙
Owner JINCHUAN GROUP LIMITED
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