Method for preparing catalyst for preparing secondary amines by hydrogenation of nitrile compounds, catalyst product and application of catalyst product

A technology of catalysts and compounds, applied in the preparation of catalysts for the hydrogenation of nitrile compounds to secondary amines and its products and applications, can solve the problems of waste of raw materials, no obvious economic advantages, equipment corrosion, etc., and achieve process environmental protection, Excellent catalytic performance, less poisonous effect

Active Publication Date: 2018-08-14
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods are simple and reliable, but have many obvious disadvantages: one, often obtain the mixture of primary, secondary, and tertiary amines, and the product needs additional purification, which not only increases the cost but also causes waste of raw materials; two, A large amount of halogen-containing wastewater will be produced during the ammonification of haloalkane. Not only the equipment is seriously co

Method used

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  • Method for preparing catalyst for preparing secondary amines by hydrogenation of nitrile compounds, catalyst product and application of catalyst product
  • Method for preparing catalyst for preparing secondary amines by hydrogenation of nitrile compounds, catalyst product and application of catalyst product
  • Method for preparing catalyst for preparing secondary amines by hydrogenation of nitrile compounds, catalyst product and application of catalyst product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Example 1: Preparation of 3Ni-Pd / C catalyst and its activity test in benzonitrile hydrogenation reaction

[0074] Preparation of 3Ni-Pd / C catalyst:

[0075] First, it is synthesized by impregnation method, and Pd is loaded on the activated carbon carrier (Pd / C), and then the nickel oxide additive is deposited (total 3 deposition cycles) on the Pd / C sample by atomic layer deposition method, A 3Ni-Pd / C catalyst is obtained.

[0076] Specifically, add 150ml of deionized water to a 250ml beaker, add 10ml of pre-configured 0.02mol / L PdCl 2 Hydrochloric acid solution (wherein the concentration of hydrochloric acid is about 0.1mol / L, the purpose is to increase the PdCl 2 Solubility of solids) and 350 mg of sodium citrate dihydrate (as a stabilizer to help better control particle size). After uniform magnetic stirring, 400 mg of activated carbon carrier (Sigma Aldrich) was added, ultrasonically stirred for 20 min to disperse the activated carbon in water, and stirred at room...

Embodiment 2

[0083] Embodiment 2: Preparation of 3Ni-Pd / C catalyst and its activity test in nitriles hydrogenation reaction

[0084] The 3Ni-Pd / C catalyst described in Example 1 was used to catalyze the hydrogenation of different nitrile reaction substrates to prepare the corresponding secondary amines. The reaction test procedure is similar to the activity test 1 part in the implementation example 1, but one or more conditions in the substrate type, temperature and substrate consumption have been changed, and the analysis results are shown in Table 2. Table 2 shows the reaction results of the 3Ni-Pd / C catalyst prepared according to Example 1 of the present invention in Example 2 to catalyze the hydrogenation of different nitriles to prepare corresponding secondary amines. As can be seen from this table 2, utilize the high-efficiency catalyst prepared by the present invention, for ten kinds of different nitriles (relate to aliphatic nitrile and aromatic nitrile), all can obtain correspondi...

Embodiment 3

[0087] Example 3: Preparation of 5Ni-Pd / C catalyst and its activity test in benzonitrile hydrogenation reaction

[0088] Preparation of 5Ni-Pd / C catalyst: Firstly, it was synthesized by impregnation method, and Pd was loaded on the activated carbon support (Pd / C), which was the same as in Example 1. Then use the atomic layer deposition method to deposit the nickel oxide additive on the Pd / C sample. The deposition method is the same as that of Example 1, except that the deposition cycle is changed to 5 cycles to obtain a 5Ni-Pd / C catalyst. According to the elemental analysis test (ICP-AES), the mass content of Pd is 4.5 wt%, and the mass content of the nickel oxide additive is 2.5 wt%. According to the results of high-resolution electron microscopy (JEM-2100F), the particle size of Pd is 2-3nm.

[0089] Activity test for catalytic hydrogenation of benzonitrile: The 5Ni-Pd / C catalyst obtained above was pretreated before the reaction. Catalyst pretreatment: first in 10% O 2 / H...

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Abstract

The invention provides a method for preparing a catalyst for preparing secondary amines by liquid-phase catalytic hydrogenation of nitrile compounds, a catalyst product obtained by the method and an application of the catalyst product. The catalyst consists of 0.1-10 wt% of an active component Pd, 0.1-80 wt% of an auxiliary agent, Ni or an oxide of Ni, on the basis of Ni metal element, and the balance of a carrier. The method comprises supporting the active component and the auxiliary agent onto the carrier by an impregnation method, a coprecipitation method, a chemical vapor deposition method, an atomic layer deposition method or any combination of the methods so as to obtain the catalyst. The catalyst obtained by the method provided by the invention can be used to realize catalytic hydrogenation of different nitriles to prepare corresponding secondary amines under mild reaction conditions, wherein the preparation is high in conversion rate and selectivity; the catalyst has high stability and can be repeatedly used for a plurality of times; and in addition, the reaction has obvious advantages of less wastewater discharge, low toxicity and the like.

Description

technical field [0001] The invention relates to a preparation method of a catalyst used for liquid-phase catalytic hydrogenation of nitrile compounds to prepare secondary amines, and the obtained catalyst product and application. Background technique [0002] Secondary amine is an important fine chemical and organic synthesis intermediate, which has a very wide and large number of applications in dyestuff, pesticide, pharmaceutical, rubber and other industries. Taking the dibenzylamine involved in the present invention as an example, dibenzylamine is a special raw material for synthesizing efficient and nontoxic rubber vulcanization accelerator tetrabenzylthiuram disulfide (TBZTD) and zinc dibenzyldithiocarbamate (ZBEC) , It can also be used for the synthesis of penicillin, and the determination of cobalt, iron and cyanate. With the improvement of domestic rubber industry standards, the demand for replacing traditional additives with green additives TBZTD and ZBEC that do n...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C209/00C07C211/27C07C211/30C07C211/29C07C211/17C07C211/07C07C213/02C07C217/58C07D307/52
CPCB01J23/892C07C209/00C07C213/02C07D307/52C07C211/27C07C211/30C07C211/29C07C211/17C07C211/07C07C217/58
Inventor 路军岭王恒伟叶旭旭
Owner UNIV OF SCI & TECH OF CHINA
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