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Preparation method of highly homogeneous Pd-loaded diatomite composite material

A composite material and diatomite technology are applied in the field of impregnation-thermal decomposition preparation of palladium-loaded diatomite composite materials, which can solve the problems of uneven adsorption and distribution of palladium salt, material performance degradation, long preparation period, etc. Pulverizing performance, low cost, and the effect of improving the loading of palladium

Inactive Publication Date: 2015-05-27
GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has high utilization rate, less dosage, and low cost of raw materials, but the amount of one-time impregnation is small, multiple impregnations are required, the preparation cycle is long, the adsorption distribution of palladium salt is uneven and mainly adsorbed on the surface of the carrier, and hydrogen absorption and desorption cycles are repeated. Afterwards, it is easy to fall off and pulverize, causing material performance degradation and blocking the separation system

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Diatomite particles with a particle size of 20-100 mesh and a porosity of not less than 85% are heat-treated at 850°C for 2 hours and then placed in the impregnation chamber. Palladium acetylacetonate (Pd(AcAc) 2 ) is the precursor, chloroform is the palladium salt solvent, and the concentration of the impregnation solution is 0.3 g / mL. The impregnation parameters of diatomite are: the impregnation temperature is 0°C; the selection rate of the impregnation chamber is 10rpm; the vacuum degree in the impregnation chamber is 0.099MPa. After the vacuum degree in the impregnation chamber is stable, open the liquid inlet valve of the impregnation chamber, and the impregnation liquid will be sucked into the impregnation chamber under the action of negative pressure. The volume of the impregnation liquid accounts for 50% of the loose volume of diatomite in the impregnation chamber; , the impregnation chamber is heated to 40°C, as the solvent in the impregnation liquid is rotov...

Embodiment 2

[0030] Diatomite particles with a particle size of 20-100 mesh and a porosity of not less than 85% are heat-treated at 850°C for 2 hours and then placed in the impregnation chamber. Palladium acetylacetonate (Pd(AcAc) 2) is the precursor, chloroform is the palladium salt solvent, and the concentration of the impregnation solution is 0.05 g / mL. The impregnation parameters of diatomite are: the impregnation temperature is 30°C; the selection rate of the impregnation chamber is 90rpm; the vacuum degree in the impregnation chamber is 0.01MPa. After the vacuum degree in the impregnation chamber is stable, open the liquid inlet valve of the impregnation chamber, and the impregnation liquid will be sucked into the impregnation chamber under the action of negative pressure. , the impregnation chamber is heated to 95°C, as the solvent in the impregnation solution is rotatably evaporated, and after being cooled by the condensation tower, all of it is recovered to the collection bottle,...

Embodiment 3

[0033] Diatomite particles with a particle size of 20-100 mesh and a porosity of not less than 85% are heat-treated at 800°C for 2 hours and then put into the impregnation chamber. Using PdCl 2 is the precursor, water is the palladium salt solvent, and the concentration of the impregnating solution is 0.1 g / mL. The impregnation parameters of diatomite are as follows: the impregnation temperature is 50°C; the selection rate of the impregnation chamber is 70rpm; the vacuum degree in the impregnation chamber is 0.06MPa. After the vacuum degree in the impregnation chamber is stable, open the liquid inlet valve of the impregnation chamber, and the impregnation liquid will be sucked into the impregnation chamber under the action of negative pressure. , the impregnation chamber is heated to 150°C, as the solvent in the impregnation liquid is rotatively evaporated, and after being cooled by the condensation tower, all of it is recovered to the collection bottle, and the impregnation ...

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Abstract

The invention relates to a preparation method of a highly homogeneous Pd-loaded diatomite composite material. The preparation method comprises the following steps: (1) putting diatomaceous support particles into a rotary impregnation bottle, and vacuumizing; (2) adding a palladium salt impregnation liquid, carrying out rotation impregnation for more than 5 min, and heating the impregnation bottle to form a palladium salt / diatomite particle intermediate; and (3) carrying out high-temperature heating decomposition on the obtained intermediate to obtain the Pd-loaded diatomite composite material. The Pd-loaded diatomite composite material obtained by the above method has advantages of high palladium load capacity, uniform adsorption, performance consistency, high stability of batches and the like.

Description

technical field [0001] The invention relates to a preparation method of a high-uniform palladium-loaded diatomite composite material, in particular to a preparation method of impregnation-thermal decomposition of a palladium-loaded diatomite composite material, and the obtained palladium-loaded diatomite composite material can be used for hydrogen isotope Separation can also be used for hydrogen purification. Background technique [0002] The hydrides of palladium and its alloys have a very significant isotope effect. Palladium is the hydrogen storage metal with the highest hydrogen isotope separation factor at room temperature. At the same time, palladium also has the advantages of easy activation, fast hydrogen absorption and desorption, and high displacement efficiency. Therefore, palladium has been widely studied and applied as a hydrogen isotope storage and separation material. In recent years, it has been widely used in fusion fuel cycle and tritium treatment process....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/14B01J20/32B01D59/26
CPCB01J20/14B01D59/26B01J20/0225B01J20/3204B01J20/3214B01J2220/42
Inventor 雷洋刘晓鹏李帅何迪张超王树茂蒋利军
Owner GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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