A method of using alkynes to synthesize palladium catalysts

A technology of alkyne compounds and palladium catalysts, which is applied in the field of palladium catalyst synthesis, and can solve the problems of low yield, high cost, and many synthesis steps

Active Publication Date: 2016-03-09
厦门嘉氢科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method has many synthetic steps, low yield and high cost

Method used

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  • A method of using alkynes to synthesize palladium catalysts
  • A method of using alkynes to synthesize palladium catalysts
  • A method of using alkynes to synthesize palladium catalysts

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Firstly, 15 mL of 20 mM chloropalladium acid aqueous solution was prepared according to the literature method. The solution was transferred to a pressure-resistant glass container and stirred at room temperature. Afterwards, 0.3 atm acetylene gas was introduced and the reaction was continued for 15 min at room temperature. After the reaction, the solution was centrifuged and the supernatant was removed. Then, the obtained solid matter was washed twice each with ethanol and water. Afterwards, a reddish-brown powder was obtained after vacuum drying.

[0029] figure 1 After passing 0.3atm acetylene gas into 20mM chloropalladium acid aqueous solution, the originally clear solution immediately became turbid, which proved that acetylene and Pd(II) reacted rapidly.

[0030] figure 2 for from figure 1 About 1g of reddish-brown powder isolated in the container, the powder can be stored at room temperature and exposed to air for at least 6 months without significant change...

Embodiment 2

[0042] Firstly, 15 mL of 20 mM chloropalladium acid aqueous solution was prepared according to the literature method. The solution was transferred to a pressure-resistant glass container, and 640 mg of activated carbon was added. After fully stirring for 30 min, 0.3 atm acetylene gas was introduced and allowed to continue to react at room temperature for 15 min. After the reaction, the solution was centrifuged and the supernatant was removed. Then, the obtained solid matter was washed twice each with ethanol and water. The product was vacuum-dried to obtain a black powder, that is, activated carbon-supported Pd catalyst.

Embodiment 3

[0044] Firstly, 15 mL of 20 mM chloropalladium acid aqueous solution was prepared according to the literature method. The solution was transferred to a pressure-resistant glass container and stirred at room temperature. Afterwards, 0.3 atm propyne gas was introduced and the reaction was continued for 15 min at room temperature. After the reaction, the solution was centrifuged and the supernatant was removed. Then, the obtained solid matter was washed twice each with ethanol and water. Afterwards, the product was vacuum-dried to obtain a brown-black powder.

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Abstract

The invention discloses a method for synthesizing a palladium catalyst by utilizing alkyne compounds and relates to a synthesizing method of a palladium catalyst. The method comprises the following steps: adding a Pd precursor in a solvent; then adding a carrier and an alkyne compound sequentially to have a reaction; at the end of the reaction, separating, washing and drying the obtained product, thus obtaining the palladium catalyst, wherein the obtained palladium catalyst is a polymerization-alkyne-loaded palladium catalyst. Alkyne is subjected to polymerization reaction in the presence of Pd; meanwhile, Pd also can be coordinated with the generated polymer, thereby obtaining a polymerization-alkyne-immobilized Pd catalyst. Meanwhile, in order to enable the obtained catalyst to be more practical, the catalyst can be adsorbed on the carrier in situ as long as a proper amount of carrier is added directly in the reaction solution, and further an immobilized catalyst is obtained. The obtained product is easy to separate and process, and is stable to air and water. The method is simple and feasible; raw materials are easily available and are easy to synthesize in a large scale. Meanwhile, the catalyst shows favorable catalytic activity and has a wide actual application prospect.

Description

technical field [0001] The invention relates to a method for synthesizing palladium catalysts, in particular to a method for synthesizing palladium catalysts using alkyne compounds. Background technique [0002] Catalysts play an extremely important role in the modern chemical industry, almost half of the chemical products are produced using catalysts. The preparation method of the catalyst directly determines the performance of the catalyst, so it is of great significance to develop new catalyst synthesis methods and processes. Taking Pd-based catalysts as an example, supported catalysts are widely used in industry, such as palladium-carbon catalysts. However, this type of catalyst has no advantages in terms of activity and selectivity compared with common Pd metal complex catalysts (homogeneous catalysts) in many non-hydrogenation types of catalytic reactions. Therefore, for the synthesis of many fine chemicals, catalysts such as tetrakis(triphenylphosphine)palladium are...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28B01J31/30
Inventor 郑南峰李欢汤少恒
Owner 厦门嘉氢科技有限公司
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