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Carbon-loaded super-small-size precious metal nanoparticle catalyst and preparation method

A nanoparticle and precious metal technology, which is applied in the field of supporting extremely small particle size precious metal nanoparticle catalysts and its preparation, can solve the problems of not being able to guarantee full loading of precious metal nanoparticles, increasing the preparation cost, and increasing production links, etc., and achieves excellent catalytic ability, high Effective catalytic active area, low cost effect

Inactive Publication Date: 2019-05-14
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the liquid-phase reduction process, an excess of reducing agent is usually added, such as hydrazine hydrate, polyol, sodium borohydride, etc., to reduce the noble metal precursor on the surface of the C material, and at the same time, a surfactant is added to control the concentration of the noble metal nanoparticles on the C surface. Particle size; in this process, excessive reducing agent can not ensure that the noble metal nanoparticles are fully loaded on the surface of C material, and the use of a large amount of surfactants will easily pollute the surface of nanoparticles and inhibit their catalytic performance, on the other hand, it will also Increased preparation costs and poses a potential threat to the environment
In addition, in the existing patented technology, it is necessary to pretreat the C material during the synthesis process, such as pickling or alkali washing, and adjusting the pH of the reaction system, etc., which increases the production process and increases the production cost.

Method used

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  • Carbon-loaded super-small-size precious metal nanoparticle catalyst and preparation method
  • Carbon-loaded super-small-size precious metal nanoparticle catalyst and preparation method
  • Carbon-loaded super-small-size precious metal nanoparticle catalyst and preparation method

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preparation example Construction

[0040] A kind of preparation method of the catalyst of activated carbon surface loading ultra-small size noble metal of the present invention, comprises the following steps:

[0041]1) First, commercial activated carbon is mixed with a noble metal precursor, and the noble metal contained in the noble metal precursor is one or any two of Pt, Pd, Ru or Rh (the mass ratio of the two noble metals is any ratio); the added The mass ratio of the noble metal contained in the noble metal precursor to the activated carbon is (0.5-5):100. The corresponding soluble noble metal salts are chloroplatinic acid (H 2 PtCl 6 ·nH 2 O), potassium chloroplatinite (K 2 PtCl 4 ), potassium chloroplatinate (K 2 PtCl 6 ); Potassium chloropalladate (K 2 PdCl 4 ), palladium nitrate (Pd(NO 3 ) 2 ·nH 2 O), potassium chloropalladate (K 2 PdCl 6 ), palladium chloride (PdCl 2 ), sodium tetrachloropalladate (Na 2 PdCl 4 ); ammonium chlororuthenate ((NH 4 ) 2 RuCl 6 ), ruthenium trichloride (...

Embodiment 1

[0045] First, weigh 50 g of commercial activated carbon and noble metal precursor potassium chloropalladate (K 2 PdCl 4 ) mixed, the mass ratio of noble metal palladium (Pd) contained in the added noble metal precursor to commercial activated carbon is 0.5:100. Then add water and ethanol according to the mass ratio of the mixture of commercial activated carbon and noble metal precursor to water and ethanol 10:45:45 to form a suspension containing 10% solids. After fully ultrasonically dispersed, pass it into the spray dryer. Keep the flow rate of the suspension at 200ml / h, set the drying temperature range of the dryer at 100°C, perform rapid atomization drying, and collect the powdery solid precursor. Subsequently, the obtained solid precursor was placed in a muffle furnace, and calcined at 5°C / min to 450°C for 3 hours in a mixture of hydrogen and argon with a mixing ratio of 5:95. The calcined product is C- Pd catalyst.

[0046] figure 1 It is a transmission electron micr...

Embodiment 2

[0048] First, weigh 50 g of commercial activated carbon and noble metal precursor chloroplatinic acid (H 2 PtCl 6 ·nH 2 O) mixing, the mass ratio of noble metal platinum (Pt) contained in the added noble metal precursor to activated carbon is 1:100. Then add water and ethanol according to the mass ratio of the mixture of activated carbon and noble metal precursor to water and ethanol 10:45:45 to form a suspension containing 10% solids. After fully ultrasonically dispersed, pass it into a spray dryer and keep The flow rate of the suspension is 100ml / h, and the drying temperature of the dryer is set at 140°C for rapid atomization and drying to collect the powdery solid precursor. Subsequently, the obtained solid precursor was placed in a muffle furnace, and calcined at 5°C / min to 300°C for 7 hours in a mixture of hydrogen and nitrogen with a mixing ratio of 5:95, and the calcined product was C-Pt catalyst.

[0049] image 3 It is a transmission electron microscope image of ...

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Abstract

The invention discloses a carbon-loaded super-small-size precious metal nanoparticle catalyst and a preparation method. The preparation method comprises the following steps: firstly enabling commercial active carbon to be mixed with a precious metal precursor, wherein precious metal contained in the precious metal precursor is one or any two of Pt, Pd, Ru or Rh; then adding water and ethyl alcohol, and forming turbid liquid; and adequately ultrasonic-dispersing, rapidly atomizing and drying in a high temperature, finally acquiring a solid powder-like precursor; calcining the solid powder-likeprecursor in a reducing atmosphere, enabling precious metal ions adsorbed on the surface thereof to be nucleated in situ and forming super-small-size precious metal nanoparticles which are loaded on the surface of a commercial active carbon carrier, to obtain the catalyst. The method is pollution-free, and low in cost. An average diameter of the loaded precious metal nanoparticles does not exceed3 nm, and the precious metal nanoparticles are uniformly loaded on the surface of the active carbon carrier. The catalyst has a higher effective catalytic activity area and excellent catalytic capacity.

Description

technical field [0001] The present invention relates to a carbon-supported ultra-small size noble metal M (M=Pt, Pd, Ru, Rh, Rh / Pt, Pd / Rh, Pt / Ru, Rh / Ru, Ru / Pd, Pt / Pd) nanoparticles The catalyst and its preparation method particularly relate to a highly evenly dispersed catalyst on the surface of commercial activated carbon loaded with extremely small diameter noble metal nanoparticles and its preparation method. Background technique [0002] Supported nano-noble metal / carbon materials, such as Pd / C, Pt / C, Ru / C, etc., have good catalytic properties and can be widely used in alkenes, alkynes, oximes, nitriles, aromatic and aliphatic aldehydes, nitro Aromatic compounds, aromatic nitriles, hydrazones, amines, ketones, aromatic heterocyclic compounds, cyclopentane and other compounds, etc., are widely used in fine chemical industries such as pharmaceutical industry, petrochemical industry, dyes, liquid crystals, pesticides, polymer materials, etc. important application. However...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/42B01J23/46B01J23/44B82Y30/00B82Y40/00
Inventor 王斌蔡海蕊刘博杨生春
Owner XI AN JIAOTONG UNIV
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