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A kind of preparation method of palladium-loaded diatomite composite material

A technology of composite materials and diatomite, which is applied in the field of preparation of palladium-loaded diatomite composite materials, can solve the problems of reduced separation performance of Pd/K composite materials, easy destruction of diatomite structure, and lower thermal decomposition temperature. Promote and realize the effect of commercial application, short process flow and mild reaction

Active Publication Date: 2017-06-20
GRIMAT ENG INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method is the main method used in experiments and some applications at present, its precursors are all inorganic palladium salts. Because the thermal decomposition temperature is too high after impregnation, the reaction is violent, and the structure of diatomite is easily destroyed, and diatomite is pulverized. After that, it will cause the separation performance of Pd / K composite material to decrease and block the separation system
[0004] The inventor's research group reported the use of palladium acetylacetonate (Pd(acac) 2 ) as a precursor, the method of preparing Pd / K composites by natural impregnation with chloroform as a solvent reduces the thermal decomposition temperature, but Pd(acac) 2 Insoluble in water, organic solvents such as chloroform need to be introduced; and the processing cost is higher than that of PdCl 2 , is not conducive to industrialization; the key is Pd(acac) 2 The diffusion capacity of the molecule is less than that of PdCl 2 pd in the form of ions in solution 2+ The diffusion ability is not conducive to immersion into the pores of diatomite, resulting in uneven distribution of the adsorbed palladium salt, and it is easy to pulverize and fall off after multiple hydrogen absorption / desorption cycles

Method used

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  • A kind of preparation method of palladium-loaded diatomite composite material
  • A kind of preparation method of palladium-loaded diatomite composite material

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 8.33g (0.047mol) PdCl 2 Dissolve in 10 mL of 38% concentrated hydrochloric acid, heat the liquid to 40°C and stir for 10 min, then add 100 mL of deionized water to dilute after cooling down. Then add 5g of diatomite particles with a particle size of 20-80 mesh and a porosity of not less than 90% (loose volume is 14cm 3 ), stirred for 60min to allow it to be fully immersed in the solution. Then add 9.41g acetylacetone, and add NaOH to adjust the pH value of the solution to 7. At this time, all the inside and outside of the diatomite particles are soaked with PdCl 2 Yellow precipitates were produced in the solution, and after filtration and drying, Pd(acac) was loaded on the surface and inside the pores. 2 Diatomaceous earth granules 19.01g. The intermediate was thermally decomposed by heating to 600°C in a hydrogen atmosphere, the flow rate of hydrogen was 20 sccm, the temperature was kept for 60 minutes, and then the temperature was raised to 1300°C for sintering for...

Embodiment 2

[0031] 8.33g (0.047mol) PdCl 2 Dissolve in 19 mL of 37% concentrated hydrochloric acid, heat the liquid to 50°C and stir for 20 min, and add 80 mL of deionized water to dilute after cooling down. Then add 4g of diatomite particles with a particle size of 20-60 mesh and a porosity of not less than 90% (loose volume is 12cm 3 ), stirred for 90min to allow it to be fully immersed in the solution. Then add 9.41g acetylacetone, and add KOH to adjust the pH value of the solution to 7.5. 2 Yellow precipitates were produced in the solution, and after filtration and drying, Pd(acac) was loaded on the surface and inside the pores. 218.06g of diatomaceous earth particles. The intermediate was thermally decomposed by heating to 500°C in a hydrogen atmosphere, the flow rate of hydrogen was 50 sccm, the temperature was kept for 40 minutes, and then the temperature was raised to 1100°C for sintering for 90 minutes to obtain 8.79 g of the final Pd / K composite material with a palladium load...

Embodiment 3

[0033] 17.74g (0.1mol) PdCl 2 Dissolve in 30mL of 36% concentrated hydrochloric acid, heat the liquid to 60°C and stir for 15min, and add 180mL deionized water to dilute after cooling down. Then add 10g of diatomite particles with a particle size of 20-40 mesh and a porosity of not less than 90% (loose volume is 30cm 3 ), stirred for 120min to fully immerse it in the solution. Then add 20.04g acetylacetone, and add NaOH to adjust the pH value of the solution to 8. At this time, all the inside and outside of the diatomite particles are soaked with PdCl 2 Yellow precipitates were produced in the solution, and after filtration and drying, Pd(acac) was loaded on the surface and inside the pores. 2 40.08g of diatomaceous earth particles. The intermediate was thermally decomposed by heating to 350°C in a hydrogen atmosphere, the flow rate of hydrogen was 100 sccm, the temperature was kept for 30 minutes, and then the temperature was raised to 1200°C for sintering for 120 minutes ...

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Abstract

The invention discloses a preparation method for a palladium-loaded diatomite composite material. The method comprises the following steps: (1) dissolving a certain amount of PdCl2 in concentrated hydrochloric acid, and fully stirring and heating the solution to enable PdCl2 to be completely dissolved; (2) adding diatomite particles into the solution and carrying out uniform stirring to allow full impregnation; (3) adding an excess amount of acetylacetone and carrying out full stirring, adjusting the pH value of the obtained solution to be 7 to 9 by using NaOH or KOH such that a yellow precipitate Pd(acac)2 is generated at the surface and the interior of the diatomite, and subjecting the diatomite impregnated with the Pd(acac)2 to filtering and drying; and (4) finally, subjecting the obtained intermediate, i.e. the diatomite supporting Pd(acac)2, to medium-temperature heating and calcining so as to obtain the palladium-loaded diatomite composite material. The preparation method for the palladium-loaded diatomite composite material provided by the invention one-time completes two process steps of synthesis of Pd(acac)2 and impregnation of the diatomite in a traditional method, has the advantages of simple method, mild reaction, easy control and reliable technology, can be used for preparation of the high-performance palladium-loaded diatomite composite material, and can be applied in the fields of separation and extraction of hydrogen isotopes.

Description

technical field [0001] The invention relates to a preparation method of a palladium-loaded diatomite composite material. The synthesized palladium-loaded diatomite composite material can be used as a high-performance hydrogen isotope separation material and is applied in the technical field of hydrogen isotope purification, separation and extraction. Background technique [0002] Fusion energy is playing an increasingly important role due to the increasing shortage of fossil energy in the world. Among them, hydrogen isotope separation is one of the core technologies for utilizing deuterium-tritium fusion energy, and the performance of the separation material is the key factor determining the separation efficiency. Among many hydrogen isotope separation materials, palladium-supported diatomite (Pd / K) composite material has the advantages of large specific surface area and high palladium loading capacity, which can buffer the internal stress during the hydrogen absorption and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D59/00C01B4/00
Inventor 雷洋刘晓鹏
Owner GRIMAT ENG INST CO LTD