A kind of preparation method of palladium carbon catalyst

A palladium-carbon catalyst, carbon monoxide technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc. , the problem of easy loss of metal Pd, etc., to reduce the growth of palladium particles, solve the problems of palladium particles growing up, and the effect of palladium nanoparticles being small

Active Publication Date: 2019-11-01
厦门嘉氢科技有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

However, the preparation of the catalyst does not control the particle size of metal palladium, and organic solvents such as aromatic hydrocarbons are used, and the preparation process is relatively complicated.
[0004] Chinese patent CN100402144C discloses a kind of preparation method of Pd / C catalyst, adds complexing agent in Pd-containing solution, such as 8-hydroxyquinoline etc. and water are mixed with palladium mixed solution impregnating or spraying carrier activated carbon, complexing agent and Pd Produce stronger interaction and produce a kind of complex compound, the metal Pd of the catalyst prepared by this method is easy to lose during use, causes catalyst activity to decline
[0005] It can be seen that the traditional catalyst preparation technology can not meet the requirements of industrial application, it is necessary to improve the preparation method of the catalyst, and find a kind of high stability palladium carbon catalyst synthesis technology, so as to be convenient for industrial application

Method used

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  • A kind of preparation method of palladium carbon catalyst

Examples

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Effect test

Embodiment 1

[0024] 50g high specific surface coconut shell activated carbon (specific surface area 1300~1400m 2 / g -1 ) after pretreatment in a drying oven at 100°C, disperse in 300mL water, measure 10mL of 1mol / L chloropalladium acid (H 2 PdCl 4 ) and slowly added dropwise to the above dispersion, stirring and impregnating for 10h. The loaded mixed solution was suction-filtered and washed until neutral, and then dried at 60°C to constant weight. Dry the above-mentioned carrier at 200°C, N 2 Roasting is carried out under atmosphere, then pass into the mixed gas of high-purity carbon monoxide and water vapor to reduce at 60 ℃, obtain the high-stability palladium-carbon catalyst of the present invention, figure 1 It is a transmission electron microscope image of the highly stable palladium-carbon catalyst prepared in Example 1 of the present invention, and the average particle size of the catalyst is about 3nm.

Embodiment 2

[0026] 50g high specific surface coconut shell activated carbon (specific surface area 1300~1400m 2 / g -1 ) was pretreated in a drying oven at 120°C, dispersed in 300mL water, and 25mL of 1mol / L chloropalladium acid (H 2 PdCl 4 ) and slowly added dropwise to the above dispersion, stirring and impregnating for 20h. The loaded mixed solution was suction-filtered and washed until neutral, and then dried at 80°C to constant weight. Dry the above-mentioned carrier at 300°C, N 2 Calcination is carried out under the atmosphere, and then a mixed gas of high-purity carbon monoxide and water vapor is passed through for reduction at 80° C. to obtain the high-stability palladium-carbon catalyst of the present invention.

Embodiment 3

[0028] 100g high specific surface coconut shell activated carbon (specific surface area 1200~1300m 2 / g -1 ) after pretreatment in a drying oven at 110°C, disperse in 300mL water, measure 10mL of 1mol / L chloropalladium acid (H 2 PdCl 4 ) and slowly added dropwise to the above dispersion, stirring and impregnating for 12h. The loaded mixed solution was suction filtered and washed to neutral, and then dried at 70°C to constant weight. Dry the above-mentioned carrier at 250°C, N 2 Roasting under the atmosphere, and then reducing at 70°C by introducing a mixture of carbon monoxide, nitrogen (volume ratio 5:95) and water vapor to obtain the high-stability palladium-carbon catalyst of the present invention.

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Abstract

The invention relates to a preparation method of a palladium-carbon catalyst, and belongs to the field of noble metal catalysts. The preparation method comprises the following steps: performing high-temperature pretreatment on a carbon support with a high specific surface area, and dispersing in a water phase; dropwisely adding a prepared palladium precursor solution into the carbon support dispersion solution, and stirring and impregnating for some time; performing vacuum filtration on the loaded dispersion solution, washing, and drying; and roasting the dried carbon support in a nitrogen protective atmosphere, and reducing with mixed gas of nitrogen / argon, carbon monoxide and vapor to obtain the palladium-carbon catalyst. In the prepared palladium-carbon catalyst, the active carbon with a high specific surface area is used as the support, and the noble metal Pd is loaded; and the content of the metal Pd in the palladium-carbon catalyst based on mass percent is 0.5-10%.

Description

technical field [0001] The invention belongs to the field of noble metal catalysts, in particular to a preparation method of a palladium carbon catalyst. Background technique [0002] Palladium carbon catalyst is a commonly used hydrogenation catalyst, widely used in carbonyl hydrogenation, olefin hydrogenation, nitro and nitroso hydrogenation and other fields. The main factors affecting catalyst activity are the content of active metal, particle size and dispersion, catalyst surface structure and so on. The influencing factors are mainly related to the type of carrier, pretreatment method, impregnation method, reduction method and temperature. [0003] Traditional palladium-carbon catalysts mostly adopt wet reduction method. Due to the weak force between the active component and the carrier, the catalyst obtained by this method has the phenomenon of growth and loss of palladium particles during the reaction process, which leads to a decrease in the dispersion of the cataly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44
CPCB01J23/44
Inventor 郑南峰江春珂刘圣杰
Owner 厦门嘉氢科技有限公司
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