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Preparation method of nitrogen and sulfur functionalized carbon foam magnetic microspheres

A magnetic microsphere, functionalized technology, applied in chemical instruments and methods, inorganic chemistry, alkali metal compounds, etc., can solve the problems of difficult separation and recovery, difficult to disperse, etc., to achieve high quality, easy to disperse, and to solve the problem of separation and recovery. Effect

Active Publication Date: 2015-11-04
德昭科技(上海)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the carbon foam prepared by this invention is a powder material, which is difficult to disperse and difficult to effectively separate and recycle during use.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Measured according to the mass ratio of resorcinol: formaldehyde solution: ethyl orthosilicate: L-cysteine: ammonia water: ethanol: water = 1: 1.5: 1.8: 1.0: 1.2: 28: 80. Add the formaldehyde solution dropwise to the mixed solution of the above substances, stir at 25°C for 30h, place it in a hydrothermal reaction kettle, and react at 100°C for 18h to obtain a SiO-containing 2 polymer microspheres. The microspheres were placed in a tube furnace, and under the protection of nitrogen, the temperature was raised to 550 °C for 4 h at a heating rate of 1 °C / min to obtain nitrogen and sulfur functionalized SiO 2 carbon foam microspheres. Use 3mol / L NaOH solution to remove SiO 2 (wherein NaOH and SiO 2 The mass ratio is 2:1) to obtain nitrogen and sulfur functionalized carbon foam microspheres. Measure according to the mass ratio of ferric nitrate nonahydrate: nitrogen, sulfur functionalized carbon foam microspheres: absolute ethanol = 0.25:1:20, mix evenly, shake at consta...

Embodiment 2

[0016] It is measured according to the mass ratio of resorcinol: formaldehyde solution: ethyl orthosilicate: L-cysteine: ammonia water: ethanol: water = 1:1.8:2.0:1.2:1.5:30:90. Add the formaldehyde solution dropwise to the mixed solution of the above substances, stir at 30°C for 18h, place it in a hydrothermal reaction kettle, and react at 100°C for 20h to obtain a SiO-containing 2 polymer microspheres. The microspheres were placed in a tube furnace, and under the protection of nitrogen, the temperature was raised to 550 °C for 4 h at a heating rate of 5 °C / min to obtain nitrogen and sulfur functionalized SiO 2 Carbon foam microspheres. Use 3mol / L NaOH solution to remove SiO 2 (wherein NaOH and SiO 2 The molar ratio of the substances is 2:1) to obtain nitrogen and sulfur functionalized carbon foam microspheres. Measure according to the mass ratio of ferric nitrate nonahydrate: nitrogen, sulfur functionalized carbon foam microspheres: absolute ethanol = 1.0:1:30, mix evenl...

Embodiment 3

[0018] It is measured according to the mass ratio of resorcinol: formaldehyde solution: ethyl orthosilicate: L-cysteine: ammonia water: ethanol: water = 1:2.0:2.2:1.5:1.7:34:120. Add the formaldehyde solution dropwise to the mixed solution of the above substances, stir at 30°C for 18h, place it in a hydrothermal reaction kettle, and react at 100°C for 24h to obtain a SiO-containing 2 polymer microspheres. The microspheres were placed in a tube furnace, and under the protection of nitrogen, the temperature was raised to 550 °C for 4 h at a heating rate of 10 °C / min to obtain nitrogen and sulfur functionalized SiO 2 carbon foam microspheres. Use 3mol / L NaOH solution to remove SiO 2 (wherein NaOH and SiO 2 The molar ratio of the substances is 2:1) to obtain nitrogen and sulfur functionalized carbon foam microspheres. Measure according to the mass ratio of ferric nitrate nonahydrate: nitrogen, sulfur functionalized carbon foam microspheres: anhydrous ethanol = 2.0:1:40, mix ev...

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Abstract

The invention relates to a preparation method of nitrogen and sulfur functionalized carbon foam magnetic microspheres. The method comprises the following steps: weighing resorcinol, a formaldehyde solution, ethyl orthosilicate, L-cysteine, ammonia water, ethanol and water according to a mass ratio of 1:1.5-2.0:1.8-2.2:1.0-1.5:1.2-1.7:28-34:80-120, mixing, stirring, putting the obtained mixture in a hydrothermal reaction kettle, and reacting for 18-24h to obtain SiO2-containing polymer microspheres; and putting the microspheres in a tubular furnace, heating at a heating rate of 1-10DEG C / min under the protection of nitrogen to 550DEG C, charring for 4h to obtain nitrogen and sulfur functionalized SiO2 carbon foam microspheres, removing SiO2 in the microspheres, weighing iron nitrate nonahydrate, the nitrogen and sulfur functionalized carbon foam microspheres and anhydrous ethanol according to a mass ratio of 0.25-2.0:1:20-40, uniformly mixing, carrying out constant temperature oscillation, placing the obtained mixture in the tubular furnace, heating at a heating rate of 1-10DEG C / min under the protection of nitrogen to 400DEG C, and carrying out heat treatment for 1h to obtain the nitrogen and sulfur functionalized carbon foam magnetic microspheres. The nitrogen and sulfur functionalized carbon foam magnetic microspheres have important application values in adsorption and removal of heavy metal mercury ions in wastewater.

Description

technical field [0001] The invention relates to a preparation method of nitrogen and sulfur functionalized carbon foam magnetic microspheres. Specifically, it refers to the use of silica nanoparticles as a template, resorcinol and formaldehyde as carbon sources, and L-cysteine ​​as a nitrogen- and sulfur-containing monomer. A method for preparing nitrogen and sulfur functionalized carbon foam magnetic microspheres. Background technique [0002] The survival and development of human beings are inseparable from the surrounding environment. In recent years, the continuous development of human society has also caused increasingly serious environmental problems. At present, the world's average annual emissions of about 15,000 tons of Hg, 3.4 million tons of Cu, 5 million tons of Pb, and 15 million tons of Mn have caused huge pollution to the environment. Therefore, heavy metal pollution is an urgent environmental problem to be solved. The adsorption method is an effective met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/20B01J20/28B01J20/30
Inventor 刘明贤邓祥祥甘礼华
Owner 德昭科技(上海)有限公司
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