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Hydrothermal preparation method of magnetic carbon micro-spheres

A carbon microsphere and hydrothermal technology, applied in the direction of microsphere preparation, microcapsule preparation, chemical instruments and methods, etc., can solve the problems of long reaction cycle, etc., and achieve the effects of low production cost, convenient reuse and high yield

Inactive Publication Date: 2015-03-25
NORTHEAST FORESTRY UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reaction is usually carried out in multiple steps, the reaction cycle is long and usually involves reagents such as strong acid and strong base, which inhibits large-scale commercial application

Method used

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  • Hydrothermal preparation method of magnetic carbon micro-spheres
  • Hydrothermal preparation method of magnetic carbon micro-spheres
  • Hydrothermal preparation method of magnetic carbon micro-spheres

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Add 1.5g microcrystalline cellulose to 45mL aqueous solution, use nickel acetate tetrahydrate as the nickel source, the concentration is 0.1mol / L, put it into a polytetrafluoroethylene-lined hydrothermal reaction kettle, and ensure that the volume of the solution and the volume of the kettle are 13:20, put it into a high-temperature reactor, heat up to the target temperature of 230°C at a rate of 10°C / min, keep the temperature for 14 hours, cool down to room temperature, and centrifuge twice at a speed of 9000r / min to obtain a brown solid product. It was washed with distilled water and absolute ethanol three times successively, and vacuum-dried at 100°C for 6 hours to obtain a nickel-doped hydrothermal carbon product precursor. Put the dried carbon sample into a tubular resistance furnace, raise the temperature at 5°C / min to the target temperature of 950°C, and keep the temperature constant for 2 hours to obtain carbon microspheres with a well-developed pore structure. ...

Embodiment 2

[0029]Add 2.5g microcrystalline cellulose to 40mL aqueous solution, use nickel acetate tetrahydrate as the nickel source, the concentration is 0.2mol / L, put it into a polytetrafluoroethylene-lined hydrothermal reaction kettle, and ensure that the volume of the solution and the volume of the kettle are 6:7, put it into a high-temperature reactor, raise the temperature to the target temperature of 250°C at a rate of 10°C / min, keep the temperature for 11 hours, cool down to room temperature, and centrifuge twice at a speed of 12000r / min to obtain a brown solid product. It was washed with distilled water and absolute ethanol three times successively, and vacuum-dried at 80°C for 6 hours to obtain a nickel-doped hydrothermal carbon product precursor. Put the dried carbon sample into a tubular resistance furnace, raise the temperature at 5°C / min to the target temperature of 850°C, and keep the temperature constant for 2 hours to obtain carbon microspheres with well-developed pore str...

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Abstract

The invention provides a hydrothermal preparation method of magnetic carbon micro-spheres. The hydrothermal preparation method is characterized by comprising the following steps: with microcrystalline cellulose as a raw material, distilled water as a solvent and nickel acetate tetrahydrate as a nickel source, carrying out high-temperature and high-pressure hydrothermal treatment; then centrifugally separating to obtain a dark brown solid product; and drying the dark brown solid product at a constant temperature and carrying out high-temperature activation and carbonization on the obtained product under the protection of nitrogen gas to obtain the magnetic micro-spheres which are doped with metal nickel and have an ordered developed pore structure and a good paramagnetic property. The operation process has the main characteristics that the cheap microcrystalline cellulose is used as the raw material; and after high-temperature activation treatment, nickel exists in a stable form of coexistence of metal nickel and nickel oxide, and the paramagnetic carbon micro-spheres with high specific surface area and the developed pore structure are generated. A prepared sample has a relatively high adsorption capability on Cd<2+> in wastewater, and the carbon micro-spheres can be recycled from a solution by a magnet, so that the carbon micro-spheres are suitable for a solution system; and meanwhile, the preparation method is simple and the performance of the carbon micro-spheres is excellent.

Description

Technical field: [0001] The invention relates to the field of nanomaterial preparation, in particular to a hydrothermal preparation method of magnetic carbon microspheres. Background technique: [0002] Water pollution caused by heavy metal ions is a severe environmental problem facing the world, among which cadmium and lead are usually the highest in content and most harmful to human health. According to the World Health Organization standard, the maximum content of cadmium and lead in drinking water should not be higher than 0.003 and 0.01mg / g. As a class of materials with high specific surface area and pore volume and pore size, carbon materials have a rich pore structure. The physical adsorption caused by the van der Waals force through the pore structure can effectively remove pigments, toxic substances, and heavy metal ions in purified water, overcoming traditional methods. However, most of the carbon materials involved are powder or solid particles, which are difficu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/20B01J20/28B01J20/30B01J13/02C02F1/28C02F1/62
CPCB01J20/02B01J20/06B01J20/20B01J20/28009B01J20/28019B01J20/28054C02F1/281C02F1/283C02F1/288C02F2101/20
Inventor 刘守新李伟吴琼黄占华代林林吴艳姣
Owner NORTHEAST FORESTRY UNIVERSITY
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