Method for preparing palladium carbon by using organic carbon monoxide releasing molecule (CORM) and catalytic application of method

A carbon monoxide and palladium carbon technology, applied in the field of catalyst preparation, can solve the problems of low recycling rate, high catalytic activity, high loading rate, etc., and achieve the effects of reducing production cost, wide source of raw materials, and low equipment requirements

Active Publication Date: 2013-09-25
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] A technical problem to be solved by the present invention is to overcome the shortcomings of low activity and low reutilization rate of palladium carbon catalysts prepared in the prior art, and provide a non-toxic and safe liquid carbon monoxide donor to replace highly toxic carbon monoxide gas. A method for palladium carbon with high loading rate, high catalytic activity and low Pd loss

Method used

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  • Method for preparing palladium carbon by using organic carbon monoxide releasing molecule (CORM) and catalytic application of method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 1. Pretreatment of activated carbon

[0017] Take 1.0g of granular coconut shell activated carbon (coconut shell AC), wash it with tap water for 7 to 8 times to remove soluble impurities and small solid particles, and then wash it with 0.1mol / L hydrochloric acid aqueous solution for 2 to 3 times to remove oxides in the activated carbon and hydroxide, then washed with distilled water until neutral, and dried in an oven at 120°C for 24 hours to remove the moisture in the pores of activated carbon.

[0018] 2. Preparation of Palladium Carbon

[0019] According to the Pd load of 10wt.%, add 1g of pretreated coconut shell activated carbon to 7.5mL of N,N-dimethylformamide, add 0.1667g of palladium chloride, stir at 200 rpm, and heat to 70°C , constant temperature immersion reduction reaction for 8 hours, filtered, washed 2 to 3 times with distilled water, dried at 60°C for 24 hours, and prepared into palladium carbon.

Embodiment 2

[0021] The palladium carbon prepared by embodiment 1 is used in catalyzing the reaction of p-bromomethoxybenzene and phenylboronic acid, and its specific use method is as follows:

[0022] Add 63.5uL (0.5mmol) p-bromomethoxybenzene, 67.1mg (0.55mmol) phenylboronic acid, 82.1mg palladium carbon, 4mL distilled water, 20.7mg potassium carbonate to a 25mL round bottom flask, stir at room temperature for 4 hours, chemical reaction The equation is as follows:

[0023]

[0024] After the reaction is finished, filter, and the filtrate is concentrated and separated by silica gel column chromatography to obtain p-methoxybiphenyl, weighed, and the yield is calculated. The palladium carbon catalyst is washed 3 to 5 times with distilled water to remove possible residual inorganic soluble impurities, and then Wash with ethanol and ethyl acetate 3 to 5 times to remove possible residual organic impurities, dry in vacuum at 60°C for 12 hours, and recover.

[0025] The recovered palladium-c...

Embodiment 3～5

[0030] In the pretreatment step 1 of embodiment 1 activated carbon, the granular coconut shell AC used is replaced with granular coal AC, granular fruit shell AC or granular wood AC of equal quality, and other steps are the same as in Example 1, and are prepared into palladium carbon.

[0031] The prepared palladium carbon was used to catalyze the reaction of p-bromomethoxybenzene and phenylboronic acid according to the method of Example 2, and the test results are shown in Table 2.

[0032] The catalytic activity of the palladium carbon prepared by table 2 embodiment 3~5

[0033]

[0034] It can be seen from Table 2 that the palladium carbon prepared by using activated carbon with different shapes as the carrier has good catalytic activity for the reaction of p-bromomethoxybenzene and phenylboronic acid, and the conversion rate of p-bromomethoxybenzene can reach 92%. Above, the catalyst recovery rate can reach more than 99%.

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Abstract

The invention relates to a method for preparing palladium carbon by using organic carbon monoxide releasing molecule (CORM). According to the method, the palladium carbon is prepared under the ordinary pressure and the low temperature by taking non-toxic and safe formamide liquid carbon monoxide donor as a carbonylation reducing agent, active carbon material as a carrier and palladium chloride, palladium nitrate or palladium acetate as a Pd precursor. According to the method, the preparation method is simple, and the problems of the conventional palladium carbon catalyst that the metal load rate is low, the catalytic activity is not high and the loss quantity of palladium is large after the palladium is circularly utilized are solved. The obtained catalyst can be used for catalyzing cross coupling reaction between aryl halide and phenylboronic acid, wherein the catalyst still presents a high catalytic activity after being repeatedly used, and the recovery rate of the catalyst is above 90%.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and in particular relates to an effective method for reducing and preparing nano-palladium carbon catalyst by using formamide as a liquid carbon monoxide donor and its application in organic synthesis. Background technique [0002] Palladium on carbon is an important class of industrial heterogeneous catalysts, widely used in various chemical transformations catalyzed by palladium, such as unsaturated hydrocarbon reduction, nitro hydrogenation reduction, benzylation hydrogenation deprotection, and carbon-carbon bond cross-coupling reactions. Palladium-carbon catalytic process has simple production process, high conversion rate, high yield, good selectivity, and less pollution, so it is favored by the industry. Palladium-carbon catalysts have played a pivotal role in petrochemical, fine chemical, and organic synthesis fields. [0003] Through statistics on palladium-carbon catalysts ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44C07C43/205C07C41/30
Inventor 张伟强杨军周东谢遵园高子伟
Owner SHAANXI NORMAL UNIV
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