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Application of palladium/active carbon catalyst in synthesizing N,N'-dibenzylethylenediamine

A technology of dibenzylethylenediamine and dibenzylideneethylenediamine is applied in the application field of palladium activated carbon catalyst in synthesizing N,N'-dibenzylethylenediamine, which can solve the problem of uneven metal active components Wide distribution, restricting the activity, selectivity and stability of supported metal catalysts, and low metal utilization rate, etc., to achieve the effect of improving metal utilization rate

Active Publication Date: 2013-06-19
嘉善县国创新能源研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Supported metal catalysts prepared by traditional methods cannot effectively adjust and control the morphology of metal particles on the surface of the support, that is, the metal active components are often dispersed on the surface of the support in the form of uneven and wide distribution, and the number of active metal active sites on the surface of the support does not vary. There is no year-on-year increase with the increase of metal loading, and a considerable part of the metal particles accumulates without exerting its proper catalytic performance, which makes the metal utilization rate low and restricts the activity, selectivity and stability of the supported metal catalyst

Method used

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  • Application of palladium/active carbon catalyst in synthesizing N,N'-dibenzylethylenediamine
  • Application of palladium/active carbon catalyst in synthesizing N,N'-dibenzylethylenediamine

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Weigh 10g of activated carbon, the specific surface area of ​​activated carbon is 1600m 2 / g, activated carbon was soaked in 120 milliliters of NaCl solution with a concentration of 0.5mol / l for 2 hours, filtered, and washed with deionized water until no chloride ions were detected. Then the treated activated carbon was formulated into 100ml slurry with a temperature of 60°C, and 10ml of H2PdCl4 solution (Pd content was 0.02g / ml) was slowly added dropwise, stirred for 4h, and then the pH value of the solution was adjusted to weak alkaline with 10% NaOH solution. (pH=7.1), and the temperature was lowered to room temperature, filtered, and washed with deionized water until neutral. The unreduced catalyst was prepared into a 150 ml slurry at 30° C., and then 2 ml of 55% hydrazine hydrate solution was slowly added dropwise, and the stirring was continued for 2 hours. The reduced catalyst was filtered, washed with deionized water until neutral, and finally dried in the air ...

Embodiment 2

[0029] Weigh 10g of activated carbon, the specific surface area of ​​activated carbon is 1600m 2 / g, activated carbon was immersed in 120 milliliters of NaCl solution with a concentration of 1.0mol / l for 2 hours, filtered, and washed with deionized water until no chloride ions were detected. Then the treated activated carbon was formulated into a 100ml slurry at a temperature of 70°C, and 20ml of H 2 PdCl 4 Solution (Pd content is 0.02g / ml), stirred for 6h, adjusted the pH value of the solution to weak alkaline (pH=8) with 10% NaOH solution, and lowered the temperature to room temperature, filtered, and washed with deionized water until neutral . The unreduced catalyst was prepared into a 150ml slurry at 30°C, and then 2ml of 55% hydrazine hydrate solution was slowly added dropwise, and the stirring was continued for 2 hours. The reduced catalyst was filtered, washed with deionized water until neutral, and finally dried in the air at room temperature, and the wet sample was ...

Embodiment 3

[0031] Weigh 10g of activated carbon, the specific surface area of ​​activated carbon is 1600m 2 / g, activated carbon was soaked in 120 ml of NaCl solution with a concentration of 1.5 mol / l for 2 hours, filtered, and washed with deionized water until no chloride ions were detected. Then the treated activated carbon was formulated into a 100ml slurry at a temperature of 80°C, and 20ml of H 2 PdCl 4 Solution (Pd content is 0.02g / ml), stirred for 6h, adjusted the pH value of the solution to weak alkaline (pH=8) with 10% NaOH solution, and lowered the temperature to room temperature, filtered, and washed with deionized water until neutral . The unreduced catalyst was prepared into a 150ml slurry at 30°C, and then 2ml of 55% hydrazine hydrate solution was slowly added dropwise, and the stirring was continued for 2 hours. The reduced catalyst was filtered, washed with deionized water until neutral, and finally dried in the air at room temperature, and the wet sample was taken and...

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Abstract

The invention discloses a palladium / active carbon catalyst and application thereof in synthesizing N,N'-dibenzylethylenediamine. The palladium / active carbon catalyst is prepared by the following steps of: impregnating active carbon by using aqueous solution of sodium halide, filtering, and washing a filter cake until halogen ions are absent; impregnating the treated active carbon by using aqueoussolution of H2PdCl4; and regulating the pH value of the solution until the solution is alkaline, filtering, washing a filter cake until the filter cake is neutral, and reducing the filter cake by using a reducing agent, and drying the obtained neutral product to obtain the palladium / active carbon catalyst. The palladium / active carbon catalyst has controllable size, most palladium particles in thecatalyst have the particle size of 2 to 5nm, the catalyst is used for synthesizing the N,N'-dibenzylethylenediamine by N,N'-dibenzylidene ethylenediamine through catalytic hydrogenation reduction, and has high activity, selectivity and stability; moreover, the catalyst is easy to prepare, environment-friendly and suitable for industrial application, and precious metal palladium is easy to recover.

Description

(1) Technical field [0001] The invention relates to a palladium activated carbon catalyst and its application in the preparation of N, N'-dibenzylethylenediamine by catalytic hydrogenation of N,N'-dibenzylideneethylenediamine. (2) Background technology [0002] N, N'-dibenzylethylenediamine diacetate (abbreviated as DBED), is widely used in the production of long-acting penicillin G, long-acting penicillin V, long-acting ampicillin and long-acting cephalosporins and other drugs. It is an important high value-added pharmaceutical intermediate, and the output value of antibiotic drugs synthesized with it is hundreds of millions. [0003] At present, the domestic DBED synthesis method basically adopts the organic synthesis method using benzyl chloride and ethylenediamine as raw materials. This route has the advantages of simple process, short process, and small investment, and is currently a relatively mature and widely used synthetic process. However, the yield of the synthe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44B01J35/10C07C211/27C07C209/70
Inventor 李小年马磊袁俊峰卢春山张群峰许孝良
Owner 嘉善县国创新能源研究院
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