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Supported double-metal catalyst capable of efficiently synthesizing DBE (Dibasic Ester) and preparation method of supported double-metal catalyst

A bimetallic catalyst and a supported technology, which is applied to the supported bimetallic catalyst for the efficient synthesis of DBE and its preparation field, can solve the problems of side reactions, slowing down the reaction speed, hydrogenolysis and polymerization, etc., and improve the hydrogenation reaction rate. , improve the effect of selectivity

Inactive Publication Date: 2018-12-11
浙江辰阳化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In addition, the current commercial Pd / C and Pt / C catalysts generally use activated carbon as the carrier. Although activated carbon has the advantages of low price and large specific surface area, the pore structure of activated carbon is mainly micropores, and the surface is neutral.
When Pd / C or Pt / C catalysts supported by activated carbon are used to prepare DBE by hydrogenation of N,N'-dibenzylidene ethylenediamine, both raw materials and products have serious diffusion resistance in the micropores of activated carbon. This not only slows down the reaction speed, but also easily leads to side reactions such as CN hydrogenolysis and polymerization, which is not conducive to the smooth progress of the reaction.

Method used

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  • Supported double-metal catalyst capable of efficiently synthesizing DBE (Dibasic Ester) and preparation method of supported double-metal catalyst
  • Supported double-metal catalyst capable of efficiently synthesizing DBE (Dibasic Ester) and preparation method of supported double-metal catalyst
  • Supported double-metal catalyst capable of efficiently synthesizing DBE (Dibasic Ester) and preparation method of supported double-metal catalyst

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Effect test

Embodiment 1

[0034] Weigh 10g of activated carbon, the particle size of activated carbon is 500 mesh, the specific surface area is 1300m2 / g, and the ash content is 1.0wt%, mix it with 0.5g urea, and treat it at 1000°C for 6h under nitrogen atmosphere to obtain nitrogen-doped Activated carbon. Then the above-mentioned nitrogen-doped activated carbon was prepared into a slurry with a temperature of 85° C. in 100 ml of deionized water, and 10 ml of H2PdCl4 solution (Pd content was 0.2 g / ml) and 10 ml of SnCl2 solution (Sn content was 0.1 g / ml) were slowly added dropwise. , stirred for 2h; the pH value of the solution was adjusted to 8 with 10wt% NaOH solution, and the temperature was lowered to room temperature, filtered, and the filter cake was washed with deionized water until neutral; then the filter cake was configured into a slurry at 85°C, and the Add 10ml of 85% hydrazine hydrate solution, stir for 2.5h, filter, wash the filter cake with deionized water until neutral, and dry it in vac...

Embodiment 2

[0036] Weigh 10g of activated carbon, the particle size of activated carbon is 800 mesh, the specific surface area is 1400m2 / g, and the ash content is 2wt%, it is placed in NH3, the gas flow rate is 1L / h, and it is treated at 900°C for 9h to obtain nitrogen-doped activated carbon. The above-mentioned nitrogen-doped activated carbon is formulated into a slurry with a temperature of 65° C. in 100 ml of deionized water, and slowly added dropwise with 6 ml of H2PtCl6 solution (Pt content is 0.1 g / ml) and 10 ml of SnCl4 solution (Sn content is 0.2 g / ml), Stir for 2.5h; use 10wt% KOH solution to adjust the pH value of the solution to 8.5, and lower the temperature to room temperature, filter, and wash the filter cake with deionized water until neutral; then configure the filter cake into a slurry at 65°C, drop Add 10ml of formaldehyde, stir for 2 hours, filter, wash the filter cake with deionized water until neutral, and dry it in vacuum at 100°C to obtain a nitrogen-doped activated ...

Embodiment 3

[0038] Weigh 10g of activated carbon, the particle size of activated carbon is 100 mesh, the specific surface area is 1100m2 / g, and the ash content is 3wt%, and it is mixed with 4g of melamine evenly, and treated at 1200°C for 3h under a helium atmosphere to obtain nitrogen-doped activated carbon. The above-mentioned nitrogen-doped activated carbon was prepared into a slurry at a temperature of 40°C in 100ml deionized water, and 10ml of Pd(NO3)2 solution (Pd content was 0.05g / ml) and 10ml of SnCl4 solution (Sn content was 0.3g / ml) were slowly added dropwise. / ml), stirred for 4 hours; adjusted the pH value of the solution to 9 with ammonia water, and lowered the temperature to room temperature, filtered, and washed the filter cake with deionized water until neutral; then configured the filter cake into a slurry at 40°C, and added dropwise 35ml of formic acid, stirred for 4 hours, filtered, the filter cake was washed with deionized water until neutral, and dried in vacuum at 80°...

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Abstract

The invention discloses a supported double-metal catalyst capable of efficiently synthesizing DBE (Dibasic Ester) and a preparation method of the supported double-metal catalyst. The supported double-metal catalyst comprises a carrier, an active component and an auxiliary agent, and is characterized in that the carrier is nitrogen-doped activated carbon; the active component is noble metal; the auxiliary agent is Sn; the loading amount of the heavy metal is 1 to 10 weight percent and the loading amount of the Sn is 1 to 5 weight percent. According to the supported double-metal catalyst disclosed by the invention, a nitrogen element in the nitrogen-doped activated carbon carrier can provide suitable alkalinity to inhibit C-N hydrogenolysis reaction, polymerization reaction of N,N'-dibenzylideneethylenediamine and the like, so that the selectivity of a target product DBE is easy to improve.

Description

technical field [0001] The invention relates to a loaded bimetallic catalyst for efficiently synthesizing DBE and a preparation method thereof. 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, long-acting cephalosporins and other drugs. At present, DBE is mainly prepared industrially from N,N'-dibenzylideneethylenediamine through catalytic hydrogenation. Among them, hydrogenation catalyst is the key technology of this process. [0003] Industrially, the catalysts used in the hydrogenation of N,N'-dibenzylideneethylenediamine to prepare DBE are mainly Pd / C and Pt / C. However, common Pd / C or Pt / C catalysts have the problem of difficult balance between activity and selectivity. This is mainly because if the activity of the Pd / C or Pt / C catalyst is too low, the polymerization reaction will easily occur and generate by-products such as polybenzylethyle...

Claims

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Application Information

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IPC IPC(8): B01J27/24C07C209/52C07C211/27
CPCB01J27/24C07C209/52C07C211/27
Inventor 李小年张群峰陈燕舞赵根富彭艳婷
Owner 浙江辰阳化工有限公司
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