Preparation method of aza-carbon-coated cobalt catalyst and unsaturated compound catalytic transfer hydrogenation method based on catalyst

A cobalt catalyst, transfer hydrogenation technology, applied in the preparation of organic compounds, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of harsh reaction conditions, expensive precious metals, long reaction time, etc., and achieve fast reaction speed , raw materials are cheap and easy to obtain, and the preparation method is simple

Inactive Publication Date: 2017-08-18
HUBEI UNIV
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  • Application Information

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Problems solved by technology

[0003] The existing unsaturated compound catalytic hydrogenation reaction conditions are relatively harsh, high temperature, high hydrogen pressure to be used, and high catalyst cost, all of which affect the utilization of biomass oil to a certain extent
For example, the Chinese patent with the application number 201410280751.3 discloses a method entitled "a method for preparing a carbon-nitrogen material-supported nano-metal catalyst", which mainly uses a carbon-nitrogen material-supported nano-metal catalyst, and the supported nano-precious metals are rhodium, ruthenium, Iridium, the catalyst can catalyze amine compounds, the selectivity is high, and the catalyst can be recycled many times, but the active center is more expensive to use noble metals, and the production cost is high
The Chinese patent with the application number 201610566647.X discloses a method entitled "a carbon-nitrogen material-supported cobalt catalyst and a met

Method used

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  • Preparation method of aza-carbon-coated cobalt catalyst and unsaturated compound catalytic transfer hydrogenation method based on catalyst
  • Preparation method of aza-carbon-coated cobalt catalyst and unsaturated compound catalytic transfer hydrogenation method based on catalyst
  • Preparation method of aza-carbon-coated cobalt catalyst and unsaturated compound catalytic transfer hydrogenation method based on catalyst

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preparation example Construction

[0028] The preparation method of azacarbon-coated cobalt catalyst comprises the following steps:

[0029] 1) Mixing: Mix carbon source, nitrogen source, cobalt salt and solvent according to the mass ratio of x:(6-x):(1~6):(1~10) and stir evenly, x is 0~6, carbon The source is one or a combination of glucose, sucrose, and fructose, the nitrogen source is one of melamine, dicyandiamide or urea, and the cobalt salt is one of cobalt chloride, cobalt acetate, cobalt nitrate, and cobalt sulfate. Kind, the solvent is deionized water;

[0030] 2) Drying and roasting: After drying the mixed mixture, place it in a vacuum tube furnace and roast in nitrogen. The roasting temperature is 500-800°C, the heating rate is 1-10°C / min, and the roasting time is 1-5h. ;

[0031] 3) Post-treatment: acidify the calcined mixture in dilute hydrochloric acid, dilute nitric acid or dilute phosphoric acid, then separate the solid from the liquid through filtration, wash and dry the solid several times t...

Embodiment 1

[0034] 3.0g glucose, 3.0g melamine, 3.0g cobalt chloride and 4.0g deionized water were mixed and stirred for 10min, transferred to a crucible, and placed in an oven at 80°C for 6h. Place the crucible in a vacuum tube furnace with N 2 As a protective gas, the temperature was raised to 500°C at a rate of 5°C / min, and roasted for 4h. After taking out the sample, soak it with 5% hydrochloric acid solution for 12h. Suction filtration, washing with deionized water, and drying to obtain Co@CN(1:1)-500 catalyst.

[0035] Take 50mg of the above-mentioned Co@CN(1:1)-500 catalyst, 76mg (0.5mmol) of vanillin, 10g of deionized water and 200mg of formic acid in the reactor, then tighten the reactor and fill it with N 2 Exhaust air, check airtightness, and fill with 0.5MPaN 2 For protective gas. Put the reaction kettle into a heater with a set temperature of 180°C, put the thermocouple in place, start stirring, and react for 4 hours. After the set reaction time, stop the reaction. The ...

Embodiment 2

[0037] 3.0g glucose, 3.0g melamine, 3.0g cobalt chloride and 4.0g deionized water were mixed and stirred for 10min, transferred to a crucible, and placed in an oven at 80°C for 6h. Place the crucible in a vacuum tube furnace with N 2 As a protective gas, the temperature was raised to 600°C at a rate of 5°C / min, and roasted for 4h. After taking out the sample, soak it with 10% hydrochloric acid solution for 12h. Suction filtration, washing with deionized water, and drying to obtain Co@CN(1:1)-600 catalyst.

[0038] According to the experimental procedure of Example 1, Co@CN(1:1)-600 was tested for activity. The experimental results show that the conversion rate of vanillin is 71.1%, and the selectivity of 2-methoxy-4-methylphenol is 100%.

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Abstract

The invention discloses a preparation method of an aza-carbon-coated cobalt catalyst. The preparation method comprises the following steps of uniformly mixing a carbon source, a nitrogen source, a cobalt salt and a solvent according to a mass ratio of x to (6-x) to (1 to 6) to (1 to 10), wherein x is an integer of 0 to 6; drying an obtained mixture, and roasting the mixture in a vacuum tubular furnace in inert gas; acidifying the roasted mixture in diluted acid, separating solid and liquid, and washing and drying the solid, so as to obtain the aza-carbon-coated cobalt catalyst. The invention also discloses a method using the catalyst prepared by the method for the catalytic transfer hydrogenation of unsaturated compounds, especially vanilline, benzaldehyde, cinnamyl aldehyde or quinoline. The preparation method has the advantages that the preparation method is simple, the cost of the raw materials is low, and the obtaining is easy; cobalt is coated into aza-carbon, so that while the high activity is maintained, the acid-resistant property and anti-CO (carbon monoxide) toxicity property of the catalyst are improved; formic acid is used as a hydrogen source to replace high-pressure hydrogen in a catalytic reduction reaction of the unsaturated compounds, the environment-friendly and economic effects are realized, the selectivity of a target product is high, and the generation of byproducts is avoided.

Description

technical field [0001] The invention relates to a composite material catalyst, in particular to a preparation method of an azacarbon-coated cobalt catalyst and a method for catalytic transfer hydrogenation of an unsaturated compound based on the catalyst. Background technique [0002] The rapid economic development is accompanied by a large amount of energy consumption, and the stock of traditional renewable energy is gradually becoming scarce. Finding renewable energy is one of the important issues for the sustainable development of human society. Biomass oil is a mixture of various degradation products of cellulose, hemicellulose and lignin, which contains a large number of unsaturated compounds such as aldehydes, aromatic rings, ketones, phenols, etc., the highest oxygen content It can be as much as half, and too high oxygen content will easily lead to poor chemical stability and low calorific value of the oil, which is extremely unfavorable for its application. Commonly...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J23/75C07C41/18C07C43/23C07D215/06
CPCB01J23/75B01J27/24B01J35/0086C07C41/18C07D215/06C07C43/23
Inventor 聂仁峰杨环环喻小龙夏清华
Owner HUBEI UNIV
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