Sulfur carbon sphere-supported noble metal catalyst and its preparation and application in synthesis of N, N'-dibenzylethylenediamine

A precious metal catalyst and catalyst technology, which is applied in the preparation of amino compounds, the preparation of organic compounds, catalysts for physical/chemical processes, etc. Complex steps and other problems, to achieve the effect of being beneficial to industrial application, excellent catalytic performance, and simple synthesis method

Inactive Publication Date: 2018-12-18
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The experimental steps of this kind of method are simple, but the adsorption force between the sulfur-containing complex and the active site is not strong, so the effect of sulfur doping is not ideal, and it is often necessary to continuously add to the reactor
Therefore, this type of method is likely to cause a series of new problems such as separation and pollution to the subsequent process; the other is for the surface modification of the carrier, and the method of doping a large number of basic groups such as S is often to combine the carrier with a sulfur-containing compound such as h 2 S, elemental S, etc. are roasted at high temperature. The experimental steps of this method are complicated, and it is not easy to control the formation of specific surface sulfur-containing groups.

Method used

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  • Sulfur carbon sphere-supported noble metal catalyst and its preparation and application in synthesis of N, N'-dibenzylethylenediamine
  • Sulfur carbon sphere-supported noble metal catalyst and its preparation and application in synthesis of N, N'-dibenzylethylenediamine
  • Sulfur carbon sphere-supported noble metal catalyst and its preparation and application in synthesis of N, N'-dibenzylethylenediamine

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Take 100ml of deionized water in a three-necked flask, install a condensation reflux device in one port, and seal the other two ports with glass stoppers; then add 0.5g cetyltrimethylammonium bromide and 1.5g cysteine ​​solid, set The temperature of the water bath was 30°C, and magnetic stirring was started for 1 h until the solid was completely dissolved. Subsequently, add 5 g of 4,4'-thiodisalicylic acid thiophenol solid, continue to stir for 0.5 h until the solid is completely dissolved, then open one of the glass stoppers, and slowly add 2 ml of concentrated H 2 SO 4 The solution is in the above mixed solution, and the rate of addition is strictly controlled to prevent the temperature rise caused by the heat of dissolution from exceeding 2°C. Continue magnetic stirring, from room temperature to 60°C at a heating rate of 0.1°C / min, keep for 6h, then continue to rise to 90°C at a heating rate of 0.1°C / min, keep for 6h, and finally continue to rise to boiling at a hea...

Embodiment 2

[0044] Take 100ml of deionized water in a three-necked flask, install a condensation reflux device in one port, and seal the other two ports with glass stoppers; then add 1g of cetyltrimethylammonium bromide and 2g of cysteine ​​solid, and set the temperature of the water bath At 30°C, start magnetic stirring for 1 h until the solid is completely dissolved. Subsequently, 8 g of 4,4'-thiodisalicylic acid thiophenol solid was added, and stirring was continued for 0.5 h until the solid was completely dissolved, then one of the glass stoppers was opened, and 2 ml of concentrated H 2 SO 4 The solution is in the above mixed solution, and the rate of addition is strictly controlled to prevent the temperature rise caused by the heat of dissolution from exceeding 2°C. Continue magnetic stirring, from room temperature to 60°C at a heating rate of 0.1°C / min, keep for 8h, then continue to rise to 90°C at a heating rate of 0.1°C / min, keep for 8h, and finally continue to rise at a heating ...

Embodiment 3

[0048] Take 100ml of deionized water in a three-necked flask, install a condensation reflux device in one port, and seal the other two ports with glass stoppers; then add 1g of cetyltrimethylammonium bromide and 2g of cysteine ​​solid, and set the temperature of the water bath At 30°C, start magnetic stirring for 1 h until the solid is completely dissolved. Subsequently, add 10 g of 4,4'-thiodisalicylic acid thiophenol solid, continue to stir for 0.5 h until the solid is completely dissolved, then open one of the glass stoppers, and slowly add 2 ml of concentrated H 2 SO 4 The solution is in the above mixed solution, and the rate of addition is strictly controlled to prevent the temperature rise caused by the heat of dissolution from exceeding 2°C. Continue magnetic stirring, raise the temperature from room temperature to 60°C at a rate of 1°C / min, keep for 12 hours, then continue to increase the rate of temperature at 1°C / min to 90°C, keep for 12 hours, and finally continue ...

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Abstract

The invention discloses a sulfur carbon sphere-supported noble metal catalyst and its preparation and application in synthesis of N, N'-dibenzylethylenediamine. The catalyst is composed of sulfur carbon spheres and an active component supported on the surface of the sulfur carbon sphere. The S of the sulfur carbon sphere exists in the form of a C-S bond on the sulfur carbon sphere skeleton and surface. The mass ratio of S to C is 0.05 to 10%. The active component comprises platinum group metal particles with particle diameters of 4 to 10nm. Based on the sulfur carbon sphere mass, the loading ratio of the active component is 5-20%. The sulfur carbon sphere-supported noble metal catalyst is spherical, and has the particle diameter of 100-1000nm, a pore volume of 0.15-1.0ml / g, a specific surface area of 300-1000m<2> / g, an average pore diameter of 0.5-2nm and a micropore ratio of 60-85%. The sulfur carbon sphere-supported noble metal catalyst has the characteristics of high conversion rate, high catalytic activity, high stability and high reaction rate in preparation of N, N'-dibenzylethylenediamine shown in the formula (II) through catalytic hydrogenation reduction of N, N'-dibenzylidene ethanediamine.

Description

(1) Technical field [0001] The invention relates to a sulfur-carbon sphere-supported noble metal catalyst, its preparation method and its application in catalytic hydrogenation reduction reaction of N,N'-dibenzylethylenediamine. (2) Technical background [0002] N,N'-Dibenzylethylenediamine (abbreviated as DBE) is an important pharmaceutical intermediate, and its derivative N,N'-dibenzylethylenediamine diacetate (abbreviated as DBED) is widely used in the production Antibiotics such as long-acting penicillin G, long-acting penicillin V, long-acting clobenicillin, and long-acting cephalosporins. At present, the domestic synthetic DBE method basically still adopts the organic synthesis method using benzyl chloride and ethylenediamine as raw materials. This route has the advantages of simple process, short flow process, small investment, etc., but the synthetic process product yield is low (only About 30%), product quality is poor, environmental pollution is big, seriously res...

Claims

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Application Information

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IPC IPC(8): B01J27/22B01J35/08B01J35/10C07C209/52C07C211/27
CPCC07C209/52B01J27/22B01J35/51B01J35/615B01J35/617B01J35/643B01J35/635B01J35/633C07C211/27
Inventor 卢春山季豪克张雪洁王昊朱倩文周烨彬岑亚青李小年
Owner ZHEJIANG UNIV OF TECH
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