Preparation method of nitrogen and sulfur co-doping micropore-mesopore carbon microspheres

A technology of co-doping and mesoporous carbon, applied in the field of material science, can solve the problems of low nitrogen and sulfur content, low specific surface area of ​​carbon foam magnetic microspheres, and limited adsorption capacity, so as to increase specific surface area and improve adsorption capacity. , the effect of simple process

Inactive Publication Date: 2017-03-15
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the specific surface area of ​​carbon foam magnetic microspheres prepared by this invention is not high, and the content of nitrogen and sulfur is low, which limits the adsorption capacity of carbon materials for heavy metals

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Take 3-aminophenol, formaldehyde solution, L-cysteine, surfactant, silica sol, ethanol and water according to 1:1.2:0.5:0.5:1:32:40 parts by mass. Mix water and ethanol uniformly at 20°C, add surfactant, silica sol, L-cysteine, 3-aminophenol and formaldehyde solution in sequence with stirring, and after reaction for 24h, heat the above mixture at 100°C. For 24h, the product obtained was carbonized from room temperature to 600℃ at a heating rate of 2℃ / min in a nitrogen atmosphere, and then the SiO in the product was removed with NaOH solution 2 , The nitrogen and sulfur co-doped mesoporous carbon microspheres are obtained, and the amount of NaOH added is the SiO in the nitrogen and sulfur co-doped mesoporous carbon microspheres. 2 2 times the amount of substance. Take the obtained carbon microspheres, KOH and water in a quantity of 1:1:20 parts by mass, mix them evenly, dry them, and activate them in a nitrogen atmosphere from room temperature to 900°C at a heating rate of...

Embodiment 2

[0015] Take 3-aminophenol, formaldehyde solution, L-cysteine, surfactant, silica sol, ethanol and water according to 1:1.4:1:1:1:2:45:60 parts by mass. Mix water and ethanol uniformly at 30℃, add surfactant, silica sol, L-cysteine, 3-aminophenol and formaldehyde solution in sequence under stirring, and after reaction for 24h, heat the above mixture at 100℃ hydrothermally For 24h, the product obtained was carbonized from room temperature to 700℃ at a heating rate of 4℃ / min in a nitrogen atmosphere, and then the SiO in the product was removed with NaOH solution 2 , The nitrogen and sulfur co-doped mesoporous carbon microspheres are obtained, and the amount of NaOH added is the SiO 2 2 times the amount of substance. Take the obtained carbon microspheres, KOH and water according to the quantity of 1:2:30 parts by mass, mix them evenly, after drying, in a nitrogen atmosphere, heat up from room temperature to 800°C at a heating rate of 4°C / min for activation to obtain nitrogen and sul...

Embodiment 3

[0017] Take 3-aminophenol, formaldehyde solution, L-cysteine, surfactant, silica sol, ethanol and water according to 1:1.6:1.5:1.5:3:60:80 mass parts. Mix water and ethanol uniformly at 35°C, add surfactant, silica sol, L-cysteine, 3-aminophenol and formaldehyde solution in sequence under stirring, and after reaction for 24 hours, heat the above mixture at 100°C. For 24h, the product obtained was carbonized from room temperature to 800℃ at a heating rate of 8℃ / min in a nitrogen atmosphere, and then the SiO in the product was removed with NaOH solution 2 , The nitrogen and sulfur co-doped mesoporous carbon microspheres are obtained, and the amount of NaOH added is the SiO 2 2 times the amount of substance. Take the obtained carbon microspheres, KOH and water in a quantity of 1:3:40 parts by mass, mix them evenly, after drying, in a nitrogen atmosphere, heat up from room temperature to 700°C at a heating rate of 8°C / min for activation to obtain nitrogen and sulfur Co-doped microp...

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Abstract

The invention relates to a preparation method of nitrogen and sulfur co-doping micropore-mesopore carbon microspheres, and belongs to the scientific and technical field of materials. The method comprises the steps that 3-aminophenol, a formaldehyde solution, an L-cysteine, a surface active agent, silica soil, ethyl alcohol and water are taken on the basis of the mass ratio being 1:(1.2-1.8):(0.5-1.5):(0.5-1.5):(1-3):(32-82):(40-100); the water and ethyl alcohol are mixed to be uniform under the temperature of 20-35 DEG C, and the other raw materials are added into the mixture in sequence, the reaction is performed for 24 h, hydrothermal treatment is performed under the temperature of 100 DEG C for 24 h, under the nitrogen atmosphere, the room temperature is increased to 600-900 DEG C at the heating rate of 2-10 DEG C / min for carbonization, NaOH is used for removing SiO2, and nitrogen and sulfur co-doping mesoporous carbon microspheres are obtained. The obtained carbon microspheres, KOH and water are taken on the basis of the mass ratio being 1:(1-4):(20-50) and mixed to be uniform, after drying, in the nitrogen atmosphere, the room temperature is increased to 600-900 DEG C at the heating speed of 2-10 DEG C / min for activation, and the nitrogen and sulfur co-doping micropore-mesopore carbon microspheres are obtained. The technology is simple, the obtained nitrogen and sulfur co-doping micropore-mesopore carbon microspheres are wide in application prospect on the aspect of adsorption and removal of heavy metal ions in wastewater.

Description

Technical field [0001] The invention relates to a method for preparing nitrogen and sulfur co-doped microporous-mesoporous carbon microspheres, and belongs to the technical field of materials science. Background technique [0002] Groundwater and surface water in most areas of my country are polluted by heavy metal ions to varying degrees. Heavy metal wastewater (containing chromium, cadmium, copper, mercury, nickel, zinc and other heavy metal ions) produced in industrial production processes such as mining and metallurgy, machinery manufacturing, chemicals, electronics, and instrumentation is the industry that pollutes the most water bodies and harms humans the most One of waste water. The method of using adsorbents to remove heavy metal ions in water is widely used for its advantages of simplicity, high efficiency, economy, and good selectivity. Carbon materials are considered to be one of the good adsorbents. It has a wide range of raw materials and can be designed with diff...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/20B01J20/30C02F1/28C02F101/20
CPCB01J20/20B01J20/02C02F1/283C02F2101/20
Inventor 刘明贤张冰洁甘礼华
Owner TONGJI UNIV
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