Preparation method of Ni/C core-shell material

A core-shell, solid product technology, applied in catalyst activation/preparation, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of high energy consumption, easy introduction of impurities, catalyst particle size, unevenness, etc.

Inactive Publication Date: 2018-10-16
QIDONG XIANGRUI CONSTR CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods generally have disadvantages such as expensive equipment, high energy consumption, and easy introduction of impurities, and most of the prepared cataly

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A method for preparing a Ni / C core-shell material, comprising the steps of: dissolving 15 parts of nickel acetate tetrahydrate in 55 parts of deionized water, stirring until dissolved; dissolving 8 parts of DHTP in 40 parts of THF, and mixing the above two The solution was fully mixed in a hydrothermal kettle and sealed, kept in an oven at 102°C for 4 days, cooled to room temperature, the resulting solid product was filtered, washed with THF and methanol, and replaced with methanol for four days, and the filtered solid product was vacuum-dried at 110°C for 14 hours , to get Ni-MOF-74; put Ni-MOF-74 in a quartz boat, put it in a tube furnace, and raise the temperature at 12°C / min to 230°C, then raise the temperature at 5°C / min to 385°C for 7.5 hours, then cool naturally to room temperature; all raw materials are in parts by weight.

Embodiment 2

[0017] A method for preparing a Ni / C core-shell material, comprising the steps of: dissolving 10 parts of nickel acetate tetrahydrate in 50 parts of deionized water, stirring until dissolved; dissolving 5 parts of DHTP in 35 parts of THF, and mixing the above two The solution is fully mixed in a hydrothermal kettle and sealed, kept in an oven at 100°C for 3.5 days, cooled to room temperature, the resulting solid product is filtered, washed with THF and methanol and replaced with methanol for four days, and the solid product is filtered and dried in vacuum at 105°C 13h, Ni-MOF-74 was obtained; put Ni-MOF-74 in a quartz boat, put it in a tube furnace, and raise the temperature at 12°C / min under the condition of argon gas with a gas flow rate of 5.6L / h to 220°C, then raised to 380°C at a rate of 5°C / min for 7 hours, and then naturally cooled to room temperature; all raw materials are in parts by weight.

Embodiment 3

[0019] A method for preparing a Ni / C core-shell material, comprising the steps of: dissolving 20 parts of nickel acetate tetrahydrate in 60 parts of deionized water, stirring until dissolved; dissolving 10 parts of DHTP in 45 parts of THF, and mixing the above two The solution was fully mixed in a hydrothermal kettle and sealed, kept in an oven at 105°C for 4.5 days, cooled to room temperature, the resulting solid product was filtered, washed with THF and methanol and replaced with methanol for four days, and the solid product was filtered and dried in vacuum at 115°C 15h to get Ni-MOF-74; put Ni-MOF-74 in a quartz boat, put it in a tube furnace, and raise the temperature at 12°C / min under the condition of argon gas with a gas flow rate of 5.8L / h to 240°C, then raised to 390°C at a rate of 5°C / min and kept at constant temperature for 8 hours, and then naturally cooled to room temperature; all raw materials are in parts by weight.

[0020] The method is simple, fast, and easy t...

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PUM

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Abstract

The invention discloses a preparation method of a Ni/C core-shell material. The preparation method of the Ni/C core-shell material comprises the following steps: adding nickel acetate tetrahydrate into deionized water, and carrying out stirring until the nickel acetate tetrahydrate is dissolved so as to obtain a solution; dissolving DHTP in THF so as to obtain a solution; fully mixing the two solutions so as to obtain a mixture, sealing the mixture in a hydrothermal kettle, and performing thermal insulation at 100-105 DEG C in an oven for 3.5-4.5 days; carrying out cooling so as to obtain a solid product, filtrating the obtained solid product, washing the filtered solid product with THF and methanol, and carrying out replacement with methanol for four days; carrying out filtrating so as toobtain a solid product, and performing vacuum drying on the solid product so as to obtain Ni-MOF-74; placing the Ni-MOF-74 in a quartz boat, putting the quartz boat into a tubular furnace, carrying out heating in the presence of argon at a heating rate of 12 DEG C/minute until the temperature reaches 220-240 DEG C, maintaining the temperature for 7-8 hours, carrying out heating at a heating rateof 5 DEG C/minute until the temperature reaches 380-390 DEG C, and maintaining the temperature for 7-8 hours; and then, carrying out cooling so as to obtain the Ni/C core-shell material. The preparation method of the Ni/C core-shell material is simple, convenient, easy to operate, and capable of successfully preparing a nano-Ni/C core-shell catalyst which is abundant in mesoporous structure, uniform in size and excellent in catalytic activity.

Description

technical field [0001] The invention relates to a preparation method of a Ni / C core-shell material. Background technique [0002] Styrene (ST) is an important monomer for the production of polymer materials such as polystyrene (PS), ABS resin and styrene-butadiene rubber. Aromatic compound impurities in industrial styrene will affect the degree of polymerization and performance of the product, especially the presence of phenylacetylene (PA), which will not only increase the catalyst consumption during styrene polymerization, affect the chain length and polymerization speed, but also cause polyphenylene The performance of ethylene deteriorates, such as discoloration, odor, degradation, release of odor, etc. Therefore, styrene purification is a very important link in industrial applications. Due to the similar chemical structure and polarity of PA and ST, the interaction between the two and the extractive distillation solvent is also similar, and the traditional extractive d...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J35/00B01J35/02B01J35/10B01J37/08
CPCB01J37/086B01J23/755B01J35/0073B01J35/026B01J35/1052
Inventor 不公告发明人
Owner QIDONG XIANGRUI CONSTR CO LTD
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