Preparation method of dichloro(1,5-cyclooctadiene) platinum (II)

A technology of cyclooctadiene and potassium chloroplatinite, which is applied in the field of preparation of platinum group metal compounds, can solve problems such as difficult recovery or recycling, harsh conditions and danger, and excessive COD, so as to save precious metal platinum and ensure safety The effect of high stability and low COD consumption

Inactive Publication Date: 2015-09-23
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

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  • Preparation method of dichloro(1,5-cyclooctadiene) platinum (II)

Examples

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Effect test

Embodiment 1

[0011] Potassium chloroplatinite can also be prepared by purchasing finished potassium chloroplatinite. The specific preparation method will be prepared by reacting chloroplatinic acid solution prepared from platinum sponge with potassium chloride solution to prepare potassium chloroplatinate, and then hydrazine hydrochloride Potassium chloroplatinite is used as a reducing agent to reduce potassium chloroplatinate to prepare pharmaceutical intermediates; the preparation process of the chloroplatinic acid solution is to react sponge platinum with aqua regia, and after the reaction stops, add concentrated hydrochloric acid dropwise to catch the nitrate until the system stops. Until brown nitrogen oxides appear again, add appropriate amount of water to catch acid, filter and heat the filtrate to 100-200g / L; chloroplatinic acid solution reacts with potassium chloride to prepare potassium chloroplatinate solution. / L of chloroplatinic acid solution is added dropwise to the potassium...

Embodiment 2

[0014] The specific implementation rules are the same as in Example 1, except that the potassium chloroplatinite is 300g, the deionized water is 6L, and n-propanol is 6L. They are added to a 50L spherical glass reactor, and the n-propanol solution of COD (1.0:1) is 1.2 L, PEG-400 600ml, reacted in an oil bath at 55°C for 4 hours; the product yield was 90.5%; the elemental analysis results were C: 25.15%, H: 3.123%, Pt: 52.13%.

Embodiment 3

[0016] The specific implementation rules are the same as example 1, except that the potassium chloroplatinite 500g purchased is used, and the added deionized water is 10L, and 10L of n-propanol is added to a 50L spherical glass reactor, and the n-propanol solution of COD (1.0 :1) 2L, PEG-400 1L, reacted in an oil bath at 55°C for 4h; the product yield was 90.5%; the elemental analysis results were C: 25.56%, H: 3.145%, Pt: 52.76%.

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Abstract

The invention relates to a preparation method of dichloro(1,5-cyclooctadiene) platinum (II). The preparation method comprises the following steps: reacting potassium tetrachloroplatinate and ligand 1,5-cyclooctadiene (COD) with a n-propyl alcohol mixed solution in water by adding a phase transfer catalyst PEG-400 to generate the milk white precipitate dichloro(1,5-cyclooctadiene) platinum (II), wherein the mole ratio of the potassium tetrachloroplatinate to the ligand 1,5-cyclooctadiene (COD) is 1: 6.4, the volume ratio of n-propyl alcohol to deionized water is 1: 0.1, and the volume ratio of PEG-400 to COD is 1.0: 1; maintaining the reaction for 4h at the reaction temperature of 50 DEG C, performing suction filtration on the milk white precipitate, washing with absolute ethyl alcohol and water, and drying to obtain the reaction product dichloro(1,5-cyclooctadiene) platinum (II). The product yield is 90% to 95%. A solvent and platinum are recycled respectively after the treatment of a filter liquor through a rotary evaporator.

Description

technical field [0001] The invention relates to a preparation method of a platinum group metal compound with 1,5-cyclooctadiene as a ligand, in particular to a preparation method of dichloro(1,5-cyclooctadiene) platinum (II). 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 catalyst makes the hydrosilylation reaction conditions milder, the yield is improved, and the selectivity is high, 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 multinuclear platinum organic compounds in addition ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00
Inventor 于晓霞易镇芳张静郭守杰刘国旗王红梅马骞李欢马正明郅欢欢梁斌邓欣荣
Owner JINCHUAN GROUP LIMITED
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