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N-heterocyclic carbene platinum complex metal carboxylate integrated catalyst and preparation method thereof

A metal carboxylate salt and catalyst technology, which is applied in the field of N-heterocyclic carbene platinum complex carboxylate metal salt integrated catalyst and its preparation, can solve the problems of low selectivity and easy generation of platinum black, and achieve easy separation , The effect of high recycling rate

Active Publication Date: 2015-02-04
HANGZHOU NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problems that the current catalysts for olefins catalyzed hydrosilylation reaction have low selectivity and the reaction is easy to produce platinum black, the present invention provides an integrated catalyst of N-heterocyclic carbene platinum complex carboxylate metal salt and its preparation method

Method used

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  • N-heterocyclic carbene platinum complex metal carboxylate integrated catalyst and preparation method thereof
  • N-heterocyclic carbene platinum complex metal carboxylate integrated catalyst and preparation method thereof
  • N-heterocyclic carbene platinum complex metal carboxylate integrated catalyst and preparation method thereof

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preparation example Construction

[0032] The preparation of catalyst and the steps of olefin hydrosilylation reaction are:

[0033] Add alkylimidazole and 1-chlorocarboxylic acid in a molar ratio of 1:1 to a round bottom flask equipped with magnetic stirring, heating and condensing devices, add trichloroethane as a reaction solvent, and at 60-90°C, Stir the reaction for 8h, cool down, pour off the supernatant, wash twice with ethyl acetate, remove the residual solvent under reduced pressure, and use it directly for the next reaction. The above prepared carboxylic acid functional imidazolium salt is dissolved in dehydrated alcohol, according to the ratio of alkylimidazole / metal chloride molar ratio of 2:1, adding ferrous, copper, zinc, calcium or magnesium chloride, at 60 At -90°C, stir the reaction for 3 hours, remove the solvent under reduced pressure, and suspend the obtained solid in anhydrous tetrahydrofuran. The imidazole molar ratio is 1:1) and stirred for 1 h, and the solvent was removed to obtain the ...

Embodiment 1

[0042] In a 100 ml three-necked flask, 1.64 g of 1-methylimidazole, 1.88 g of chloroacetic acid, and 20 ml of trichloroethane were added, the temperature was raised to 80° C., the reaction was stirred for 8 h, and cooled to room temperature. Trichloroethane was removed by decantation, washed with ethyl acetate (25 mL×2), and the residual solvent was removed under reduced pressure. The solid was dissolved with 20 ml of absolute ethanol, and 1.99 g of FeCl was added 2 4H 2 O, stirred at 80°C for 3h, removed ethanol by rotary evaporation, and dried in a vacuum oven at 70°C for 24h. The obtained solid was suspended in 25 ml of anhydrous tetrahydrofuran, 2.24 g of potassium tert-butyl alkoxide was added, stirred for 30 minutes, 39 g of Karstedt catalyst with a platinum content of 10% was added, stirred for 1 h, and the solvent was removed to obtain N-heterocyclic carbene platinum complex carboxylate Acid metal salt integrated catalyst.

[0043] Take 0.15 mmol of the catalyst, 1 ...

Embodiment 2

[0046] Take 0.15 mmol of the catalyst of Example 1, 1 mol of 1-hexene and 1.1 mol of triethoxyhydrogensilane in a closed container containing a magnetic stirrer, and react in a silicone oil bath at 80°C for 4 hours, and the conversion rate of 1-hexene is 99.6%. , β-addition product selectivity was 99.9%.

[0047] Separate the upper layer product, add another 1mol 1-hexene and 1.1mol triethoxyhydrogensilane, react under the same conditions for 4h, the conversion rate of 1-hexene is 99.0%, and the selectivity of β-addition product is 99.2%.

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Abstract

The invention relates to the field of organic high-molecular chemistry and discloses an N-heterocyclic carbene platinum complex metal carboxylate integrated catalyst and a preparation method thereof. The preparation method includes following steps: (1) carrying out a reaction between alkyl imidazole and halogenated carboxylic acid to obtain a carboxylic acid functionalized imidazolium salt; (2) carrying out a reaction with chlorides of ferrous, copper, zinc, calcium or magnesium to obtain a imidazole-based ionic liquid containing carboxylates containing the ferrous, the copper, the zinc, the calcium or the magnesium; (3) preparing an N-heterocyclic carbene ligand from the ionic liquid under effect of potassium tert-butyl alcohol; and (4) carrying out a reaction with a Karstedt catalyst to prepare the N-heterocyclic carbene platinum complex metal carboxylate integrated catalyst. The catalyst is high in selectivity, is free of generation of platinum black precipitation, is easy to separate and can be recycled.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to an integrated catalyst of N-heterocyclic carbene platinum complex carboxylate metal salt and a preparation method thereof. Background technique [0002] Olefin-catalyzed hydrosilylation reaction is one of the most important ways to synthesize organosilicon coupling agents and functional organosilicon compounds and polymers (J. Organomet. Chem., 2003, 681, 91-97). Hydrosilylation of olefins usually uses Speier catalyst (isopropanol solution of chloroplatinic acid) and Karstedt catalyst (tetramethyldivinyldisiloxane complex of platinum). Although the above two types of catalytic systems have relatively high activity, However, there are disadvantages such as low product selectivity, easy production of platinum black during catalyst storage and reaction process, and high catalyst cost. Markó et al. reported that for Karstedt catalysts, using N-heterocyclic carbene as a ligand to rep...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07F15/00C07F7/18C07F7/14
Inventor 彭家建白赢厉嘉云肖文军徐艺凇
Owner HANGZHOU NORMAL UNIVERSITY
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