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Preparation method and application of Pd-Ni bimetallic catalyst supported by N-doped acid-activated sepiolite

A bimetallic catalyst, sepiolite technology, applied in physical/chemical process catalysts, chemical instruments and methods, oxime preparation, etc., can solve the problems of low utilization rate of reaction resources, unsuitable for large-scale production, and high catalyst cost, and meet the conditions Mild, increasing electronegativity, reducing the effect of metal particle size

Active Publication Date: 2016-10-26
XIANGTAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the existing hydrogenation process, the catalytic effect is good when noble metals are used, but the catalyst cost is high, which is not suitable for large-scale industrial production; when non-noble metals are used, the utilization rate of reaction resources is low and the product quality is not high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Weigh 20g of sepiolite, put it in a 1000mL single-necked flask, add 400mL of 1moL / L hydrochloric acid solution according to the solid-to-liquid mass ratio of 1:20, put it into a magnet, and place it in an oil bath with a constant temperature of 75°C Vigorously stirred for 24 hours, the suspension was filtered with suction, washed with distilled water, neutralized, and dried at 100°C for 2 hours to obtain the desired acid-modified sepiolite. Weigh the above 10g of acid-modified sepiolite and place it in a 100mL single-necked flask, add 20ml of deionized water, 10g of melamine, and 20ml of formaldehyde solution, and put it into a 75°C water bath and stir vigorously, while stirring at a stirring rate of 1000rpm During the process, add 0.5Mol / L NaOH solution to adjust the pH to 12.5, and stir for 60 minutes; cool the above mixture to room temperature, add a small amount of 36% acetic acid solution to adjust the pH to 6, and stir at 1000rpm Stir for 12 hours, centrifuge, fil...

Embodiment 2

[0036] Weigh 0.15 grams of the 1%Pd-20%Ni / N-AAS catalyst obtained in Example 1 and place it in a 50mL lining of a high-temperature reactor, add 5.5 grams of ethylenediamine, 0.5 grams of nitrocyclohexane, and put the magneton , seal the autoclave, replace the air in the autoclave with nitrogen for 4 times, evacuate the autoclave to vacuum with a vacuum pump, and then place the autoclave in an oil bath. After rising to the set reaction temperature of 60°C, hydrogen was introduced to pressurize to 0.5 MPa, magnetic stirring was started, and the reaction timing started. After reacting for 8 hours, the reaction mixture was filtered, and the content of each substance in the filtrate was analyzed by gas chromatography. The conversion rate of nitrocyclohexane was 91.63%, and the selectivity of cyclohexanone oxime was 71.21%.

Embodiment 3

[0038] Weigh 0.15 grams of the 1%Pd-20%Ni / N-AAS catalyst obtained in Example 1 and place it in a 50mL lining of a high-temperature reactor, add 5.5 grams of ethylenediamine, 0.5 grams of nitrocyclohexane, and put the magneton , seal the autoclave, replace the air in the autoclave with nitrogen for 4 times, evacuate the autoclave to vacuum with a vacuum pump, and then place the autoclave in an oil bath. After rising to the set reaction temperature of 70°C, hydrogen was introduced to pressurize to 0.5 MPa, magnetic stirring was started, and the reaction timing started. After reacting for 8 hours, the reaction mixture was filtered, and the content of each substance in the filtrate was analyzed by gas chromatography. The conversion rate of nitrocyclohexane was 98.63%, and the selectivity of cyclohexanone oxime was 82.56%.

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Abstract

The invention discloses a preparation method and an application of a Pd-Ni bimetallic catalyst supported by N-doped acid-activated sepiolite. The preparation method comprises the following steps: sepiolite is subjected to acid activation or acid modification firstly, then subjected to N-doping treatment and subjected to impregnation to support Ni and Pd. Non-noble metal Ni is taken as a dominant active component and is modified with a small amount of Pd for preparation of the Pd-Ni bimetallic catalyst, so that noble metal is prevented from being used as the only active component, the cost of the catalyst is reduced greatly, a technology for preparing cyclohexanone-oxime from nitrocyclohexane through liquid-phase hydrogenation is enabled to be more environment-friendly by means of the catalyst, the technology is simple, conditions are mild, and quite high nitrocyclohexane conversion rate and cyclohexanone-oxime with high selectivity can be obtained by optimizing the reaction conditions and preparing the catalyst.

Description

technical field [0001] The invention relates to the fields of material preparation and chemical engineering, in particular to a preparation method and application of a nitrogen-doped acid-activated sepiolite-loaded Pd-Ni bimetallic catalyst. Background technique [0002] The hydrogenation of nitrocyclohexane mainly produces cyclohexanone oxime and cyclohexylamine, and the rearrangement of cyclohexanone oxime produces caprolactam. Caprolactam is one of the important organic chemical raw materials and is mainly used to synthesize nylon-6 fiber and nylon-6 engineering. plastic. Due to its excellent thermal stability, high mechanical strength, chemical corrosion resistance and processability, caprolactam has a wide range of applications, mainly in the fields of automobiles, medical equipment, ships, electronic appliances, and daily necessities. The current industrial production methods mainly include toluene method, cyclohexanone-hydroxylamine method, photonitrosation method an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C07C249/10C07C251/44
CPCB01J27/24C07C249/10C07C251/44
Inventor 刘平乐吕扬郝芳罗和安
Owner XIANGTAN UNIV
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