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Clay load palladium catalyst and preparation method thereof

A palladium catalyst, a catalyst technology, which is applied in the directions of catalyst activation/preparation, carbon-based compound preparation, chemical instruments and methods, etc., can solve the problems of high calcination temperature, expensive reagents, limited industrial application, etc., and achieves low energy consumption, simple composition, Simple preparation method

Inactive Publication Date: 2009-12-09
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In summary, although great progress has been made in the preparation of supported noble metal catalysts, there are still many deficiencies that limit their industrial applications.
For example, complex and tedious carrier preparation and pretreatment process, use of toxic and volatile organic solvents, high calcination temperature and use of expensive reagents

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 0.444g PdCl 2 Add 20mL of distilled water, then add 0.49g of concentrated hydrochloric acid, stir to dissolve, then dilute to 50mL with distilled water to make H2O with a concentration of 0.05M 2 PdCl 4 solution. Pipette the above H 2 PdCl 4 Add 2 mL of the solution into 25 mL of distilled water, add 1 g of organoclay (montmorillonite modified by alkyl quaternary ammonium surfactant exchange) into the above solution, and stir at room temperature for 10 min. The above mixture was filtered and washed, and then the filter cake was dried in an oven at 60°C for 24 hours. After the dried solid was ground into powder, freshly prepared 2.0wt% NaBH was added dropwise 4 solution until no more bubbles are produced. After the reaction, the above mixture was filtered, washed with a large amount of distilled water, and washed with 1mol / LAgNO 3 Check whether the chloride ion is removed, and add AgNO to the filtrate 3 The solution no longer formed a white precipitate. Th...

Embodiment 2

[0025] For the 1.0 wt% Pd-DK1-RE catalyst prepared in the above column. Pipette 1 mL (9.7 mmol) of benzyl alcohol, put it into a 50 mL glass flask, then add 10 mL of toluene, then weigh 0.05 g of catalyst and 0.1 g of K 2 CO 3 into the above mixture. At the beginning of the reaction, oxygen was passed into the reaction liquid below the liquid level through the gas guide tube, and the flow rate of oxygen was controlled at 25 mL / min. The reaction temperature was controlled at 100±1°C by an oil bath. After reacting for 2 hours, the temperature was lowered to room temperature, 0.2 g of naphthalene was added as an internal standard, and after shaking well, the catalyst was centrifuged, and the liquid product was analyzed by a Grockway GC7800 gas chromatograph. The catalytic reaction results are listed in Table 2. The catalytic performance of the catalyst remained basically unchanged after 3 cycles.

[0026] Table 2 Table 11.0wt%Pd / DK1-RE Catalyst Selective Oxidation Performanc...

Embodiment 3

[0029] For the 1.0 wt% Pd-DK1-RE catalyst prepared in the above example. Pipette 5 mL (48.5 mmol) of benzyl alcohol and put it into a 50 mL glass flask, then weigh 0.1 g of catalyst and put it into the above mixed solution. At the beginning of the reaction, oxygen was passed into the reaction liquid below the liquid level through the gas guide tube, and the flow rate of oxygen was controlled at 25 mL / min. The reaction temperature was controlled at 100±1°C by an oil bath. After reacting for 2 hours, the temperature was lowered to room temperature, 0.2 g of naphthalene was added as an internal standard, and after shaking well, the catalyst was centrifuged, and the liquid product was analyzed by a Grockway GC7800 gas chromatograph. The results of the catalytic reactions are listed in Table 3.

[0030] Table 31.0wt%Pd / DK1-RE Catalyst Selective Oxidation Performance of Benzyl Alcohol

[0031] Reaction time (h)

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Abstract

The invention provides a clay load palladium catalyst and a preparation method thereof and relates to a high-efficiency catalyst taking oxygen as an oxygen source and preparing aldehyde by alcohol selective oxidation. The catalyst comprises organic clay carrier load palladium, wherein the weight percent content of the Pd in the catalyst is 0.1% to 5%. An adsorption method is adopted to carry out preparation, and a quaternary surfactant in the organic clay can specifically and rapidly adsorb a palladium precursor body PdCl4. The adsorption method has controllable load rate of the palladium and high metal dispersion degree, and the obtained catalyst has the advantages of high catalytic activity, simple preparation technology and the like. A solvent-free reaction is carried out, and the transformation frequency (TOF) for transforming benzyl alcohol into benzaldehyde is commonly higher than 1000h and can reach 6800h under a proper condition. By repeated use for many times, the transformation rate of the benzyl alcohol and the selectivity of the benzaldehyde are not reduced obviously.

Description

technical field [0001] The invention relates to a high-efficiency solid catalyst for selectively oxidizing alcohols to synthesize aldehydes or ketones by using oxygen as an oxygen source and a preparation method thereof. Background technique [0002] Selective oxidation of alcohols to carbonyl compounds is an important reaction in organic synthesis, and it plays a key role in the fine chemical industries such as synthetic drugs, vitamins, fragrances and artificial fibers. Using traditional methods to complete this type of reaction usually requires an equal amount of inorganic oxides (such as high-valent manganese and chromium, etc.), which is not only expensive, but also causes great pollution to the environment. In recent years, some research groups at home and abroad have devoted themselves to finding environmentally friendly reaction methods and catalytic systems for the selective oxidation of alcohols. Metal Pd has extraordinary catalytic activity and has been widely us...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J21/16B01J37/00B01J23/52B01J23/42B01J23/46C07C45/37C07C47/54
Inventor 陈铁红王虎邓绍新
Owner NANKAI UNIV
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