High-dispersion nitrogen-sulfur co-doped catalyst and preparation thereof, and application in synthesis of N,N-dibenzylethylenediamine

A dibenzylidene ethylenediamine, nitrogen and sulfur co-doping technology, applied in the direction of catalyst activation/preparation, preparation of amino compounds, preparation of organic compounds, etc., can solve the problem of difficult balance between activity and selectivity, easy polymerization reaction, etc. problem, to achieve the effect of more application times, inhibit hydrogenolysis reaction, and improve utilization rate

Pending Publication Date: 2021-01-08
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Common Pd / C or Pt / C catalysts commonly used in industry have the problem of difficulty in balancing activity and selectivity. If the activity of the catalyst is too low, polymerization reactions will easily occur and by-products such as polybenzylethylenediamine will be generated; if the activity is too high Then lead to severe C-N hydrogenolysis reaction, generating monobenzylethylenediamine

Method used

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  • High-dispersion nitrogen-sulfur co-doped catalyst and preparation thereof, and application in synthesis of N,N-dibenzylethylenediamine
  • High-dispersion nitrogen-sulfur co-doped catalyst and preparation thereof, and application in synthesis of N,N-dibenzylethylenediamine
  • High-dispersion nitrogen-sulfur co-doped catalyst and preparation thereof, and application in synthesis of N,N-dibenzylethylenediamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Weigh 50ml of 20wt% nitric acid solution, soak 6g of activated carbon in the nitric acid solution by slowly adding dropwise while stirring with a magnetic stirrer, and slowly heat to 80°C for 10h. After cooling to room temperature, wash with deionized water until the filtrate is neutral. Weigh 0.119g of thiourea solid, 5g of nitric acid-treated activated carbon, and mix with 30ml of deionized water. After mixing, they are ultrasonically treated at 40°C for 0.5h, and then vacuum-dried at 120°C for 24h. The dried activated carbon was placed in a tube furnace, and nitrogen gas was introduced into the furnace at 5 °C min -1 The rate was raised to 900 ° C for 2 h to obtain the required activated carbon. Dissolve sodium silicate in DMF and add deionized water to make up to 0.9g / ml, mix with 0.1g / ml chloroplatinic acid solution, stir at 70°C for 6h, and ultrasonicate at 60°C for 1h to obtain highly dispersed platinum solution. Weigh the above 1g of activated carbon and lay ...

Embodiment 2

[0031] Weigh 50ml of 20wt% nitric acid solution, soak 6g of activated carbon in the nitric acid solution by slowly adding dropwise while stirring with a magnetic stirrer, and slowly heat to 80°C for 10h. After cooling to room temperature, wash with deionized water until the filtrate is neutral. Weigh 0.06 g of thiourea solid, 5 g of nitric acid-treated activated carbon, and mix with 30 ml of deionized water. After mixing, they are ultrasonically treated at 40° C. for 0.5 h, and then vacuum-dried at 120° C. for 24 h. The dried activated carbon was placed in a tube furnace, and nitrogen gas was introduced into the furnace at 5 °C min -1 The rate was raised to 900 ° C for 2 h to obtain the required activated carbon. Dissolve sodium silicate in DMF and add deionized water to make up to 0.9g / ml, mix with 0.1g / ml chloroplatinic acid solution, stir at 70°C for 6h, and ultrasonicate at 60°C for 1h to obtain highly dispersed platinum solution. Weigh the above 1g of activated carbon ...

Embodiment 3

[0033] Weigh 50ml of 20wt% nitric acid solution, soak 6g of activated carbon in the nitric acid solution by slowly adding dropwise while stirring with a magnetic stirrer, and slowly heat to 80°C for 10h. After cooling to room temperature, wash with deionized water until the filtrate is neutral. Weigh 0.072g of thiourea solid, 5g of nitric acid-treated activated carbon, and mix with 30ml of deionized water. After mixing, they are ultrasonically treated at 40°C for 0.5h, and then vacuum-dried at 120°C for 24h. The dried activated carbon was placed in a tube furnace, and nitrogen gas was introduced into the furnace at 5 °C min -1 The rate was raised to 900 ° C for 2 h to obtain the required activated carbon. Dissolve sodium silicate in DMF and add deionized water to make up to 0.9g / ml, mix with 0.1g / ml chloroplatinic acid solution, stir at 70°C for 6h, and ultrasonicate at 60°C for 1h to obtain highly dispersed platinum solution. Weigh the above 1g of activated carbon and lay ...

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Abstract

The invention provides a high-dispersion nitrogen-sulfur co-doped catalyst and a preparation method thereof, and an application in a reaction of synthesizing N,N-dibenzylidene ethylenediamine from N,N-dibenzylidene ethylenediamine. According to the invention, thiourea is adopted for one-step doping, so that operation is convenient, pollution is reduced, and defect sites generated by doping are beneficial to adsorption of precious metal; heteroatom nitrogen in a carbon skeleton can provide proper alkalinity, so that polymerization reaction of N,N-dibenzylidene ethylenediamine is reduced; heteroatomic sulfur plays a complexing role, so that strong interaction between sulfur and platinum can properly reduce the activity of the catalyst, inhibit the generation of CN hydrogenolysis reaction andimprove the selectivity of a target product; metal nanoparticles are not easy to agglomerate or lose in hydrogenation reaction, so that the service life of the catalyst is prolonged, and under the combined action of heteroatom nitrogen and heteroatom sulfur, the stability of platinum is greatly improved; and the catalyst provided by the invention has the advantages of mild use conditions, good stability, less catalyst dosage, more application times and long service life.

Description

technical field [0001] The invention relates to a highly dispersed nitrogen-sulfur co-doped catalyst and its application in the preparation and synthesis of N,N-dibenzylethylenediamine (DBE). Background technique [0002] DBE is a pharmaceutical intermediate, mainly used in the production of long-acting penicillin G, long-acting penicillin V, long-acting ampicillin and long-acting cephalosporins. At present, DBE is mainly prepared industrially from N,N-dibenzylideneethylenediamine through catalytic hydrogenation, and the hydrogenation catalyst is the key core. Common Pd / C or Pt / C catalysts commonly used in industry have the problem of difficulty in balancing activity and selectivity. If the activity of the catalyst is too low, polymerization reactions will easily occur and by-products such as polybenzylethylenediamine will be generated; if the activity is too high It will lead to severe C-N hydrogenolysis reaction to generate monobenzylethylenediamine. [0003] Based on th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/42B01J27/24B01J21/18B01J37/02B01J35/10B01J37/18B82Y30/00B82Y40/00C07C209/52C07C211/27
CPCB01J23/42B01J27/24B01J21/18B01J37/0201B01J35/1023B01J35/1028B01J35/1038B01J35/1042B01J35/0066B01J37/18B82Y30/00B82Y40/00C07C209/52C07C211/27
Inventor 张群峰张超杰周媛卢春山丰枫李小年
Owner ZHEJIANG UNIV OF TECH
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