CN103272558A - Nitrogen doped carbon xerogel material for absorbing heavy metal ions from water, and preparation method - Google Patents
Nitrogen doped carbon xerogel material for absorbing heavy metal ions from water, and preparation method Download PDFInfo
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- CN103272558A CN103272558A CN201310142901XA CN201310142901A CN103272558A CN 103272558 A CN103272558 A CN 103272558A CN 201310142901X A CN201310142901X A CN 201310142901XA CN 201310142901 A CN201310142901 A CN 201310142901A CN 103272558 A CN103272558 A CN 103272558A
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Abstract
The invention discloses a nitrogen doped carbon xerogel material for absorbing heavy metal ions from water, and a preparation method. The nitrogen doped carbon xerogel material comprises, by mass, 20.97%-21.49% of resorcinol, 32.69%-33.50% of formaldehyde, 0.10%-0.20% of sodium carbonate, 2.36%-4.61% of melamine and 41.52%-42.55% of water. Sodium carbonate is used as a catalyst to initiate a reaction of resorcinol and melamine with formaldehyde; an organic gel with a three-dimensional network structure is produced after polymerization; the organic gel is extracted by a solvent, dried and then carbonized in a tube furnace under the protection of nitrogen, and thus the nitrogen doped carbon xerogel material is obtained. Nitrogen-containing polymerization monomers are added in raw materials for conventional carbon gel synthesis, so that the nitrogen doped carbon xerogel material has relatively many surface functional groups. The nitrogen doped carbon xerogel material synthesized by the method has relatively good mechanical strength and adsorption capacity of the heavy metal ions.
Description
Technical field
The present invention relates to relate to a kind of nitrogen doping charcoal xerogel material and preparation method for absorbing heavy metal ions in water, belong to environmental protection technical field.
Background technology
The treatment of heavy metal ions technology has multiple, mainly comprises chemical method, physics method and bioanalysis.Absorption method has obtained extensive use as a kind of efficient cheap method.In numerous sorbing materials, the raw material of wood-charcoal material especially is widely used.
The charcoal gel has obtained extensive concern as a kind of novel porous nanometer material at recent two decades.The charcoal gel is synthetic by the Pekala of U.S. Lawrence Livemore National Laboratory the earliest, afterwards numerous scholar's research control the synthetic technology of its pore passage structure character.The charcoal gel is big because of its specific area, and the duct is abundant to be beneficial to mass transfer, and the chemical stability height is applied to the pollutant adsorbing domain.
The charcoal xerogel is also fewer for heavy metal ion adsorbed research, and its main cause is that material surface functional group is less, and adsorption capacity also has the very big rising space.Adopting melamine to add in the reaction raw materials can allow the charcoal xerogel of modification have more functional group, this nitrogen-containing functional group can be with heavy metal ion generation ion-exchange and complexing (shown in equation, wherein X is the body construction of charcoal xerogel, the M representation metal ion), thus improve the charcoal xerogel to the adsorption capacity of heavy metal ion.In addition, the structure of melamine hexatomic ring has good heat endurance, and is less through the carbonization process structural change.
2(X-OH)?+?M
2+→?(X-O)
2M?+?2H
+
2(X-NH)
++?M
2+?→?(X-N)
2M?+?2H
+
X-N+M
2+→?[M→N-X]
2+。
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of nitrogen doping charcoal xerogel material and preparation method for absorbing heavy metal ions in water is provided.
The nitrogen doping charcoal xerogel material that is used for absorbing heavy metal ions in water is by percentage to the quality, resorcinol 20.97% ~ 21.49%, formaldehyde 32.69% ~ 33.50%, sodium carbonate 0.10% ~ 0.20%, melamine 2.36% ~ 4.61%, water 41.52% ~ 42.55%; It by sodium carbonate as catalyst; cause resorcinol and the same formolite reaction of melamine; generate the organogel with tridimensional network after the polymerization, after organogel process solvent extraction and the drying, charing obtains nitrogen doping charcoal xerogel material in tube furnace under nitrogen protection.
The nitrogen doping charcoal xerogel material preparation method that is used for absorbing heavy metal ions in water is: add resorcinol 9.09 grams in beaker successively, sodium carbonate 0.0438～0.0876 gram, melamine 1～2 gram, water 18 grams are heated to 80 ℃, mix, add formaldehyde 14.17 grams again, wait to obtain to pour in the glass tube behind the yellow settled solution, put into baking oven and carry out drying, first following dry 3 days at 85 ℃; Descended dry 3 days at 100 ℃ again, through acetone extract, 800 ℃ of following charings, obtain nitrogen doping charcoal xerogel material then.
Nitrogen doping charcoal xerogel material of the present invention is by melamine, and resorcinol forms with oxymethylene polymerization, has added nitrogenous polymerization single polymerization monomer in traditional charcoal gel synthesis material, has many relatively surface functional groups.The nitrogen doping charcoal xerogel material that synthesizes by the present invention has mechanical strength and heavy metal ion adsorbed capacity preferably.
The specific embodiment
The nitrogen doping charcoal xerogel material that is used for absorbing heavy metal ions in water is by percentage to the quality, resorcinol 20.97% ~ 21.49%, formaldehyde 32.69% ~ 33.50%, sodium carbonate 0.10% ~ 0.20%, melamine 2.36% ~ 4.61%, water 41.52% ~ 42.55%; It by sodium carbonate as catalyst; cause resorcinol and the same formolite reaction of melamine; generate the organogel with tridimensional network after the polymerization, after organogel process solvent extraction and the drying, charing obtains nitrogen doping charcoal xerogel material in tube furnace under nitrogen protection.
The nitrogen doping charcoal xerogel material preparation method that is used for absorbing heavy metal ions in water is: add resorcinol 9.09 grams in beaker successively, sodium carbonate 0.0438～0.0876 gram, melamine 1～2 gram, water 18 grams are heated to 80 ℃, mix, add formaldehyde 14.17 grams again, wait to obtain to pour in the glass tube behind the yellow settled solution, put into baking oven and carry out drying, first following dry 3 days at 85 ℃; Descended dry 3 days at 100 ℃ again, through acetone extract, 800 ℃ of following charings, obtain nitrogen doping charcoal xerogel material then.
Embodiment 1: with resorcinol 9.09 grams, sodium carbonate 0.0584 gram, melamine 2 grams, water 18 grams, be heated to 80 ℃, mix, under stirring condition, add formaldehyde 14.17 grams, obtain after polymerisation is finished pouring in the glass tube behind the yellow settled solution, put into baking oven and carry out drying (85 ℃ following 3 days; 100 ℃ are following 3 days), dry gained organogel obtains nitrogen doping charcoal gel rubber material through acetone extract and carbonization process (800 ℃), this material is soaked in the pb of 50mg/L
2+In the solution, be that this nitrogen doping charcoal gel rubber material is to pb under 4.5 the condition at pH
2+Adsorbance be 37.20mg/g.
Embodiment 2: with resorcinol 9.09 grams, sodium carbonate 0.0876 gram, melamine 2 grams, water 18 grams, be heated to 80 ℃, mix, under stirring condition, add formaldehyde 14.17 grams, obtain after polymerisation is finished pouring in the glass tube behind the yellow settled solution, put into baking oven and carry out drying (85 ℃ following 3 days; 100 ℃ are following 3 days), dry gained organogel obtains nitrogen doping charcoal gel rubber material through acetone extract and carbonization process (800 ℃), this material is soaked in the pb of 50mg/L
2+In the solution, be that this nitrogen doping charcoal gel rubber material is to pb under 4.5 the condition at pH
2+Adsorbance be 37.04mg/g.
Embodiment 3: with resorcinol 9.09 grams, sodium carbonate 0.0584 gram, melamine 1.5 grams, water 18 grams, be heated to 80 ℃, mix, under stirring condition, add formaldehyde 14.17 grams, obtain after polymerisation is finished pouring in the glass tube behind the yellow settled solution, put into baking oven and carry out drying (85 ℃ following 3 days; 100 ℃ are following 3 days), dry gained organogel obtains nitrogen doping charcoal gel rubber material through acetone extract and carbonization process (800 ℃), this material is soaked in the pb of 50mg/L
2+In the solution, be that this nitrogen doping charcoal gel rubber material is to pb under 4.5 the condition at pH
2+Adsorbance be 35.64mg/g.
Embodiment 4: with resorcinol 9.09 grams, sodium carbonate 0.0438 gram, melamine 2 grams, water 18 grams, be heated to 80 ℃, mix, under stirring condition, add formaldehyde 14.17 grams, obtain after polymerisation is finished pouring in the glass tube behind the yellow settled solution, put into baking oven and carry out drying (85 ℃ following 3 days; 100 ℃ are following 3 days), dry gained organogel obtains nitrogen doping charcoal gel rubber material through acetone extract and carbonization process (800 ℃), this material is soaked in the pb of 50mg/L
2+In the solution, be that this nitrogen doping charcoal gel rubber material is to pb under 4.5 the condition at pH
2+Adsorbance be 32.62mg/g.
Embodiment 5: with resorcinol 9.09 grams, sodium carbonate 0.0584 gram, melamine 1 gram, water 18 grams, be heated to 80 ℃, mix, under stirring condition, add formaldehyde 14.17 grams, obtain after polymerisation is finished pouring in the glass tube behind the yellow settled solution, put into baking oven and carry out drying (85 ℃ following 3 days; 100 ℃ are following 3 days), dry gained organogel obtains nitrogen doping charcoal gel rubber material through acetone extract and carbonization process (800 ℃), this material is soaked in the pb of 50mg/L
2+In the solution, be that this nitrogen doping charcoal gel rubber material is to pb under 4.5 the condition at pH
2+Adsorbance be 32.14mg/g.
Embodiment 6: with resorcinol 9.09 grams, sodium carbonate 0.0584 gram, melamine 2 grams, water 18 grams, be heated to 80 ℃, mix, under stirring condition, add formaldehyde 14.17 grams, obtain after polymerisation is finished pouring in the glass tube behind the yellow settled solution, put into baking oven and carry out drying (85 ℃ following 3 days; 100 ℃ are following 3 days), dry gained organogel obtains nitrogen doping charcoal gel rubber material through acetone extract and carbonization process (800 ℃), this material is soaked in the Cu of 50mg/L
2+In the solution, be that this nitrogen doping charcoal gel rubber material is to Cu under 5.5 the condition at pH
2+Adsorbance be 41.57mg/g.
Embodiment 7: with resorcinol 9.09 grams, sodium carbonate 0.0876 gram, melamine 2 grams, water 18 grams, be heated to 80 ℃, mix, under stirring condition, add formaldehyde 14.17 grams, obtain after polymerisation is finished pouring in the glass tube behind the yellow settled solution, put into baking oven and carry out drying (85 ℃ following 3 days; 100 ℃ are following 3 days), dry gained organogel obtains nitrogen doping charcoal gel rubber material through acetone extract and carbonization process (800 ℃), this material is soaked in the Cu of 50mg/L
2+In the solution, be that this nitrogen doping charcoal gel rubber material is to Cu under 5.5 the condition at pH
2+Adsorbance be 40.82mg/g.
Embodiment 8: with resorcinol 9.09 grams, sodium carbonate 0.0584 gram, melamine 1.5 grams, water 18 grams, be heated to 80 ℃, mix, under stirring condition, add formaldehyde 14.17 grams, obtain after polymerisation is finished pouring in the glass tube behind the yellow settled solution, put into baking oven and carry out drying (85 ℃ following 3 days; 100 ℃ are following 3 days), dry gained organogel obtains nitrogen doping charcoal gel rubber material through acetone extract and carbonization process (800 ℃), this material is soaked in the Cu of 50mg/L
2+In the solution, be that this nitrogen doping charcoal gel rubber material is to Cu under 5.5 the condition at pH
2+Adsorbance be 40.09mg/g.
Embodiment 9: with resorcinol 9.09 grams, sodium carbonate 0.0438 gram, melamine 2 grams, water 18 grams, be heated to 80 ℃, mix, under stirring condition, add formaldehyde 14.17 grams, obtain after polymerisation is finished pouring in the glass tube behind the yellow settled solution, put into baking oven and carry out drying (85 ℃ following 3 days; 100 ℃ are following 3 days), dry gained organogel obtains nitrogen doping charcoal gel rubber material through acetone extract and carbonization process (800 ℃), this material is soaked in the Cu of 50mg/L
2+In the solution, be that this nitrogen doping charcoal gel rubber material is to Cu under 5.5 the condition at pH
2+Adsorbance be 38.78mg/g.
Embodiment 10: with resorcinol 9.09 grams, sodium carbonate 0.0584 gram, melamine 1 gram, water 18 grams, be heated to 80 ℃, mix, under stirring condition, add formaldehyde 14.17 grams, obtain after polymerisation is finished pouring in the glass tube behind the yellow settled solution, put into baking oven and carry out drying (85 ℃ following 3 days; 100 ℃ are following 3 days), dry gained organogel obtains nitrogen doping charcoal gel rubber material through acetone extract and carbonization process (800 ℃), this material is soaked in the Cu of 50mg/L
2+In the solution, be that this nitrogen doping charcoal gel rubber material is to Cu under 5.5 the condition at pH
2+Adsorbance be 36.59mg/g.
Embodiment 11: with resorcinol 9.09 grams, sodium carbonate 0.0584 gram, melamine 2 grams, water 18 grams, be heated to 80 ℃, mix, under stirring condition, add formaldehyde 14.17 grams, obtain after polymerisation is finished pouring in the glass tube behind the yellow settled solution, put into baking oven and carry out drying (85 ℃ following 3 days; 100 ℃ are following 3 days), dry gained organogel obtains nitrogen doping charcoal gel rubber material through acetone extract and carbonization process (800 ℃), this material is soaked in the Zn of 50mg/L
2+In the solution, be that this nitrogen doping charcoal gel rubber material is to Zn under 5.5 the condition at pH
2+Adsorbance be 40.13mg/g.
Embodiment 12: with resorcinol 9.09 grams, sodium carbonate 0.0876 gram, melamine 2 grams, water 18 grams, be heated to 80 ℃, mix, under stirring condition, add formaldehyde 14.17 grams, obtain after polymerisation is finished pouring in the glass tube behind the yellow settled solution, put into baking oven and carry out drying (85 ℃ following 3 days; 100 ℃ are following 3 days), dry gained organogel obtains nitrogen doping charcoal gel rubber material through acetone extract and carbonization process (800 ℃), this material is soaked in the Zn of 50mg/L
2+In the solution, be that this nitrogen doping charcoal gel rubber material is to Zn under 5.5 the condition at pH
2+Adsorbance be 39.45mg/g.
Embodiment 13: with resorcinol 9.09 grams, sodium carbonate 0.0584 gram, melamine 1.5 grams, water 18 grams, be heated to 80 ℃, mix, under stirring condition, add formaldehyde 14.17 grams, obtain after polymerisation is finished pouring in the glass tube behind the yellow settled solution, put into baking oven and carry out drying (85 ℃ following 3 days; 100 ℃ are following 3 days), dry gained organogel obtains nitrogen doping charcoal gel rubber material through acetone extract and carbonization process (800 ℃), this material is soaked in the Zn of 50mg/L
2+In the solution, be that this nitrogen doping charcoal gel rubber material is to Zn under 5.5 the condition at pH
2+Adsorbance be 35.94mg/g.
Embodiment 14: with resorcinol 9.09 grams, sodium carbonate 0.0438 gram, melamine 2 grams, water 18 grams, be heated to 80 ℃, mix, under stirring condition, add formaldehyde 14.17 grams, obtain after polymerisation is finished pouring in the glass tube behind the yellow settled solution, put into baking oven and carry out drying (85 ℃ following 3 days; 100 ℃ are following 3 days), dry gained organogel obtains nitrogen doping charcoal gel rubber material through acetone extract and carbonization process (800 ℃), this material is soaked in the Zn of 50mg/L
2+In the solution, be that this nitrogen doping charcoal gel rubber material is to Zn under 5.5 the condition at pH
2+Adsorbance be 35.87mg/g.
Embodiment 15: with resorcinol 9.09 grams, sodium carbonate 0.0584 gram, melamine 1 gram, water 18 grams, be heated to 80 ℃, mix, under stirring condition, add formaldehyde 14.17 grams, obtain after polymerisation is finished pouring in the glass tube behind the yellow settled solution, put into baking oven and carry out drying (85 ℃ following 3 days; 100 ℃ are following 3 days), dry gained organogel obtains nitrogen doping charcoal gel rubber material through acetone extract and carbonization process (800 ℃), this material is soaked in the Zn of 50mg/L
2+In the solution, be that this nitrogen doping charcoal gel rubber material is to Zn under 5.5 the condition at pH
2+Adsorbance be 34.41mg/g.
Claims (2)
1. a nitrogen doping charcoal xerogel material that is used for absorbing heavy metal ions in water is characterized in that by percentage to the quality resorcinol 20.97% ~ 21.49%, formaldehyde 32.69% ~ 33.50%, sodium carbonate 0.10% ~ 0.20%, melamine 2.36% ~ 4.61%, water 41.52% ~ 42.55%; It by sodium carbonate as catalyst; cause resorcinol and the same formolite reaction of melamine; generate the organogel with tridimensional network after the polymerization, after organogel process solvent extraction and the drying, charing obtains nitrogen doping charcoal xerogel material in tube furnace under nitrogen protection.
2. nitrogen doping charcoal xerogel material preparation method for absorbing heavy metal ions in water as claimed in claim 1, it is characterized in that: in beaker, add resorcinol 9.09 grams successively, sodium carbonate 0.0438～0.0876 gram, melamine 1～2 gram, water 18 grams, be heated to 80 ℃, mix, add formaldehyde 14.17 grams again, wait to obtain to pour in the glass tube behind the yellow settled solution, put into baking oven and carry out drying, first following dry 3 days at 85 ℃; Descended dry 3 days at 100 ℃ again, through acetone extract, 800 ℃ of following charings, obtain nitrogen doping charcoal xerogel material then.
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| CN104167296A (en) * | 2014-08-05 | 2014-11-26 | 郑州大学 | Method for preparing nanoelectrode material of super capacitor |
| CN104587918A (en) * | 2015-01-30 | 2015-05-06 | 河海大学 | Silver nano-particle modified carbon ball/graphene composite aero-gel material as well as preparation method and application of material |
| CN107115882A (en) * | 2017-05-09 | 2017-09-01 | 赵兴亚 | A kind of preparation method of photocatalyst crystals and its purposes in catalytic degradation organic wastewater |
| CN107824212A (en) * | 2017-10-31 | 2018-03-23 | 青岛大学 | Nitrogen-doped carbon cerium oxide composite and its preparation and application |
| CN112892483A (en) * | 2021-01-29 | 2021-06-04 | 武汉大学 | Nitrogen-doped carbon aerogel nano-microsphere as well as preparation method and application thereof |
| CN113903935A (en) * | 2020-07-07 | 2022-01-07 | 原子能与替代能源委员会 | Method for producing porous nitrogen-containing carbon materials with metal dopants, in particular for use as oxygen reduction (ORR) catalysts |
| CN117299091A (en) * | 2023-11-30 | 2023-12-29 | 同济大学 | Humic acid functionalized carbon submicron sphere, preparation method thereof and application thereof in heavy metal contaminated soil regeneration |
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| CN104167296A (en) * | 2014-08-05 | 2014-11-26 | 郑州大学 | Method for preparing nanoelectrode material of super capacitor |
| CN104167296B (en) * | 2014-08-05 | 2017-03-29 | 郑州大学 | A kind of preparation method of the nano-electrode material for ultracapacitor |
| CN104587918A (en) * | 2015-01-30 | 2015-05-06 | 河海大学 | Silver nano-particle modified carbon ball/graphene composite aero-gel material as well as preparation method and application of material |
| CN107115882A (en) * | 2017-05-09 | 2017-09-01 | 赵兴亚 | A kind of preparation method of photocatalyst crystals and its purposes in catalytic degradation organic wastewater |
| CN107115882B (en) * | 2017-05-09 | 2018-09-14 | 赣州安益宏科技有限公司 | The preparation method and its purposes in catalytic degradation organic wastewater of a kind of photocatalyst crystals |
| CN107824212A (en) * | 2017-10-31 | 2018-03-23 | 青岛大学 | Nitrogen-doped carbon cerium oxide composite and its preparation and application |
| CN107824212B (en) * | 2017-10-31 | 2020-06-09 | 青岛大学 | Nitrogen-doped carbon-cerium oxide composite material and preparation and application thereof |
| CN113903935A (en) * | 2020-07-07 | 2022-01-07 | 原子能与替代能源委员会 | Method for producing porous nitrogen-containing carbon materials with metal dopants, in particular for use as oxygen reduction (ORR) catalysts |
| CN112892483A (en) * | 2021-01-29 | 2021-06-04 | 武汉大学 | Nitrogen-doped carbon aerogel nano-microsphere as well as preparation method and application thereof |
| CN117299091A (en) * | 2023-11-30 | 2023-12-29 | 同济大学 | Humic acid functionalized carbon submicron sphere, preparation method thereof and application thereof in heavy metal contaminated soil regeneration |
| CN117299091B (en) * | 2023-11-30 | 2024-04-19 | 同济大学 | Humic acid functionalized carbon submicron sphere, preparation method thereof and application thereof in heavy metal contaminated soil regeneration |
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Application publication date: 20130904 |