Preparation method and application of CuNi-based catalyst

A technology of catalysts and additives, applied in the field of preparation of CuNi-based catalysts, can solve problems such as difficulty in application

Inactive Publication Date: 2018-09-07
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although now for CO 2 、H 2 The research on the synthesis of DMF with dimethylamine has been in-depth, but because most of them use noble metal catalysts, it is difficult to apply them to actual production.
The latest research by Han et al. showed that the Cu/ZnO cata

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  • Preparation method and application of CuNi-based catalyst

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[0029] The present invention provides a kind of preparation method and application of CuNi base catalyst, such as figure 1 Shown, described preparation method comprises at least:

[0030] S1, mixing urea, or concentrated ammonia water, or a mixture of urea and concentrated ammonia water, with copper salt and nickel salt to make a mixed solution;

[0031] S2, adding a carrier or an auxiliary agent into the mixed solution to make a material to be aged;

[0032] S3, pouring the material to be aged into a reflux oil bath reactor, and generating a precipitate through ammonia distillation reflux reaction;

[0033] S4, preparing the CuNi-based catalyst by successively centrifuging, washing, drying, calcining and reducing the precipitate.

[0034] In addition, the present invention also provides the application of a CuNi-based catalyst for CO 2 and HN(CH 3 ) 2 In the reaction of hydrogenation reaction to synthesize DMF, the reaction adopts a high-pressure reactor, and the reaction ...

Embodiment 1

[0037] Take an appropriate amount of copper nitrate, nickel nitrate, 40% Wt% silica sol and concentrated ammonia water according to Cu:Ni=1:1, SiO 2 : Ni = 10: 1, concentrated ammonia water: (Cu+Ni) = 15: 1 (molar ratio) to prepare a 1M mixed material. Put the mixed material in a three-necked flask with a condensing reflux tube, under the heating of an oil bath, reflux and age at 80°C for 16 hours, centrifuge the reaction solution, wash, and dry to obtain a solid precipitate, and heat up at 1°C / min The rate was raised to 500°C and fired for 6 hours to obtain a metal oxide precursor. Weigh 0.20g of the metal oxide precursor and put it into the reduction tube. 2 Reduction under the atmosphere, the reduction conditions are: increase the temperature at a rate of 1°C / min to 500°C, reduce for 3h, H 2 Flow velocity 20ml / min, obtain CuNi base catalyst after reduction, wherein this CuNi base catalyst comprises CuOWt%: 28.5%, NiOWt%: 24.3%, SiO 2 Wt%: 47.2%.

[0038] Put 0.2g of the...

Embodiment 2

[0040] Take appropriate amount of copper nitrate, nickel nitrate, 40%wt% silica sol and urea according to Cu:Ni=3:1, SiO 2 : Ni=10:1, urea: (Cu+Ni)=8:1 (molar ratio) prepared into a 1.5M mixed material. Put the mixed material in a three-necked flask with a condensing reflux tube, under the heating of an oil bath, reflux and age at 80°C for 16 hours, centrifuge the reaction solution, wash, and dry to obtain a solid precipitate, and heat up at 1°C / min Raise the rate to 600°C, and bake for 3 hours to obtain a metal oxide precursor. Weigh 0.20g of the metal oxide precursor and put it into the reduction tube. 2 Reduction under the atmosphere, the reduction conditions are: increase the temperature at a rate of 1°C / min to 600°C, reduce for 3h, H 2 Flow rate 20ml / min, obtain CuNi base catalyst after reduction, wherein this CuNi base catalyst comprises CuOWt%: 30.5%, NiOWt%: 9.8%, SiO 2 Wt%: 59.7%.

[0041] Put 0.2 g of the above-mentioned reduced CuNi-based catalyst into the autoc...

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Abstract

The invention provides a preparation method and application of a CuNi-based catalyst. The preparation method comprises the following steps: uniformly mixing urea or concentrated ammonia or a mixture of urea and concentrated ammonia with a copper salt, a nickel salt and a carrier or auxiliary agent in a reflux device under stirring; carrying out ammonia distillation to obtain a metal precipitate; and then successively carrying out centrifugation, washing, drying, calcination and reduction so as to obtain the CuNi-based catalyst. The CuNi-based catalyst comprises, by mass, 30-50% of CuO, 5-25% of NiO and 30-60% of a carrier or auxiliary agent. The CuNi-based catalyst prepared in the invention is free of active component loss and stable in catalytic performance; when the CuNi-based catalyst is applied to CO2 hydrogenation and HN(CH3)2(DMA) reaction for synthesis of DMF, the yield of DMF is high, and required raw materials are cheap and easily available; and the preparation method is simple in process, easy to operate, low in process cost and high in repetitive rate, and thus has good application prospects.

Description

technical field [0001] The invention belongs to the field of inorganic chemistry and relates to a preparation method and application of a catalyst, in particular to a preparation method of a CuNi-based catalyst and its application in CO 2 The application of hydrogenation and dimethylamine in the synthesis of DMF. Background technique [0002] CO 2 Carbon oxides are abundant, readily available, cheap, non-toxic, and renewable in nature. Converting them into valuable chemicals or fuels can not only alleviate energy shortage, but also solve the problem of greenhouse gas control. . in CO 2 Among the many conversion pathways of hydrogenation, the hydrogenation reaction plays an important role. Through the hydrogenation reaction, various fuels and chemicals such as formic acid, formate and its derivatives, methanol, dimethyl ether, carbon monoxide, and methane can be produced. [0003] N,N-Dimethylformamide (DMF), is a colorless, high-boiling, hygroscopic, fishy-smelling liqui...

Claims

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Application Information

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IPC IPC(8): B01J23/755C07C231/10C07C233/03
CPCB01J23/002B01J23/755B01J2523/00C07C231/10B01J2523/17B01J2523/847B01J2523/41B01J2523/31C07C233/03
Inventor 王慧夏林张建明钟良枢魏伟孙予罕
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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