CN115672267A - Nitrogen-doped carbon material, preparation thereof and application thereof in heavy metal ion adsorption - Google Patents
Nitrogen-doped carbon material, preparation thereof and application thereof in heavy metal ion adsorption Download PDFInfo
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- CN115672267A CN115672267A CN202110848500.0A CN202110848500A CN115672267A CN 115672267 A CN115672267 A CN 115672267A CN 202110848500 A CN202110848500 A CN 202110848500A CN 115672267 A CN115672267 A CN 115672267A
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- nitrogen
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- hydrochloride
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 43
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 19
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 20
- 150000002500 ions Chemical class 0.000 claims abstract description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 5
- 239000012298 atmosphere Substances 0.000 claims abstract description 4
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 238000006467 substitution reaction Methods 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 8
- 239000003463 adsorbent Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- RKMFFOLUBJFMBQ-UHFFFAOYSA-N (4-amino-2-azaniumylphenyl)azanium;dichloride Chemical group Cl.Cl.NC1=CC=C(N)C(N)=C1 RKMFFOLUBJFMBQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003929 acidic solution Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000005530 etching Methods 0.000 abstract description 3
- 125000003277 amino group Chemical group 0.000 abstract description 2
- 239000005416 organic matter Substances 0.000 abstract description 2
- ZPHQBFRCXUIIAZ-UHFFFAOYSA-N benzene;hydrochloride Chemical compound Cl.C1=CC=CC=C1 ZPHQBFRCXUIIAZ-UHFFFAOYSA-N 0.000 abstract 1
- -1 lead ions Chemical class 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 7
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 3
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000005381 potential energy Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention relates to a nitrogen-doped carbon material and preparation and application thereof in heavy metal ion adsorption, wherein the preparation method comprises the steps of mixing polyamino benzene hydrochloride and ferric trichloride, calcining in an inert gas atmosphere, and carrying out post-treatment to obtain the nitrogen-doped carbon material; wherein the substitution number of amino groups in the polyaminobenzene hydrochloride is 3-5; the prepared nitrogen-doped carbon material can be used for adsorbing lead ions in water. Compared with the prior art, the porous nitrogen-doped carbon material is prepared by directly calcining the nitrogen-containing organic matter in one step without a template agent and an additional etching step, the method is simple and easy to amplify, and the prepared porous nitrogen-doped carbon material has high adsorption capacity to heavy metal ions, particularly lead ions, and has good application significance.
Description
Technical Field
The invention belongs to the technical field of heavy metal ion adsorption, and relates to a nitrogen-doped carbon material, and preparation and application thereof in heavy metal ion adsorption.
Background
The porous carbon material has high specific surface area and porosity, very stable physical property and chemical property, low cost, easy preparation and simple regeneration process, and is widely applied in the fields of gas phase and liquid phase adsorption, catalyst carriers and electrode materials of super capacitors. Hetero atoms such as nitrogen and phosphorus are introduced into the porous carbon material, so that lattice parameters, surface chemical potential energy and surface hydrophilicity of the carbon material can be changed, and the adsorption capacity of the carbon material on specific ions is enhanced. Nitrogen doping is often carried out by two ways, one of which is calcining the carbon material in an ammonia atmosphere after its preparation, or calcining it together with other nitrogen-containing materials, to prepare a nitrogen-doped carbon material. The other method is to use a nitrogen-containing substance as a precursor to prepare the nitrogen-doped carbon material by a one-step method. The second method has the characteristics of simple preparation method, low energy consumption and the like.
One important application of carbon materials is the adsorption of heavy metal ions. With the development of economy, environmental problems such as heavy metal pollution increasingly affect the lives of people. The pollution of heavy metals to water and soil seriously affects the health of human beings, aquatic animals and plants. The heavy metal ions can be quickly removed from the water through the specific adsorption capacity of the adsorbent to the special ions, the operation is simple, and the cost is low. Chinese patent application CN2019113029335 discloses a method for preparing a nitrogen-oxygen co-doped porous carbon material by calcining a mixture of oxygen-containing organic matters and nitrogen-containing organic matters, wherein the nitrogen-oxygen co-doped porous carbon material containing 5-25% of nitrogen and oxygen is prepared, and the removal rate of the material on nickel ions can reach more than 99%. In the method, the nano oxide is used as a template agent, so that the cost is high, and in addition, after the calcination, an additional etching step is required to remove the nano oxide, so that the environmental protection risk and the production cost are increased.
Disclosure of Invention
The invention aims to provide a nitrogen-doped carbon material, a preparation method thereof and application thereof in heavy metal ion adsorption, and aims to solve the problems of complicated preparation method, high environmental hazard risk and high production cost of the conventional nitrogen-oxygen co-doped porous carbon material type lead ion adsorbent.
The purpose of the invention can be realized by the following technical scheme:
a method of making a nitrogen-doped carbon material, comprising: mixing polyaminobenzene hydrochloride with ferric trichloride, calcining in an inert gas atmosphere, and performing post-treatment to obtain the nitrogen-doped carbon material;
wherein, in the polyaminobenzene hydrochloride, the substitution number of amino groups is 3-5, and more preferably, the polyaminobenzene hydrochloride is 1,2, 4-triaminobenzene dihydrochloride.
Further, the mixing is ball milling mixing, the used ball grinding material is zirconia balls with the diameter of 3-8mm, the ball milling rotating speed is 50-200rpm, and the ball milling time is 20-30h.
Furthermore, in the calcination, the calcination temperature is 600-1000 ℃, and the calcination time is 1-10h.
Furthermore, the mixing mass ratio of the polyaminobenzene hydrochloride to the ferric trichloride is (1-10): 1.
Further, the post-treatment sequentially comprises acid solution washing, deionized water washing and drying.
Further, in the acidic solution washing, the acidic solution used comprises 0.5-1.5M hydrochloric acid.
The nitrogen-doped carbon material is prepared by the method, can be preferably used as an adsorbent and is used for adsorbing heavy metal ions in a water body.
Further, the nitrogen-doped carbon material is used as an adsorbent for adsorbing lead ions.
Compared with the prior art, the invention has the following characteristics:
1) According to the invention, the porous nitrogen-doped carbon material is directly prepared by one-step calcination of the nitrogen-containing organic matter, a template agent and an additional etching step are not needed, and the method is simple and easy to amplify;
2) The porous nitrogen-doped carbon material prepared by the invention has higher adsorption capacity to heavy metal ions, especially lead ions, and has better application significance.
Drawings
FIG. 1 is a scanning electron micrograph of a nitrogen-doped carbon material prepared in example 1;
fig. 2 is a scanning electron micrograph of the nitrogen-doped carbon material prepared in example 4.
Detailed Description
The invention is described in detail below with reference to the figures and the specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
The embodiment is as follows:
a nitrogen-doped carbon material and a preparation method thereof comprise the following steps:
1) Ferric chloride hexahydrate (FeCl) 3 ·6H 2 O), 1,2, 4-triaminobenzene dihydrochloride and 60g of zirconia balls with the diameter of 3-8mm are respectively added into a ball milling tank, and then ball milling is carried out for 24 hours at the rotating speed of 100rpm, so that ferric trichloride hexahydrate and 1,2, 4-triaminobenzene dihydrochloride are uniformly mixed;
2) Transferring the ball-milled mixture into an alumina crucible, putting the alumina crucible into a tubular furnace, calcining for 4 hours at the normal pressure of 800 ℃ in the nitrogen atmosphere, and naturally cooling to room temperature to obtain a calcined product;
3) And washing the calcined product with 1M hydrochloric acid for three times and deionized water for three times in sequence to remove impurities in the product, and drying in a vacuum oven at 80 ℃ for 12 hours to obtain the nitrogen-doped carbon materials NC-1, NC-2, NC-3 and NC-4, wherein the scanning electron microscope images of NC-1 and NC-4 are respectively shown in figures 1 and 2.
The embodiment further comprises a lead ion adsorption test of the prepared nitrogen-doped carbon material, and the specific process is as follows: four 50mg/L lead nitrate solutions are prepared, each 100mL, 50mg of nitrogen-doped carbon materials NC-1, NC-2, NC-3 and NC-4 are respectively added into the solutions, the solutions are sealed and are vibrated and adsorbed in a constant-temperature water bath oscillator at 25 ℃ for 24 hours at the oscillation frequency of 100 rpm. After the oscillation is finished, filtering out powdery carbon materials, taking filtrate, analyzing the solution concentration by an inductively coupled plasma emission spectrum analyzer, and calculating the adsorption capacity according to the following formula:
Q t ＝(C 0 -C t )V/m
wherein Q t The lead ion adsorption capacity is unit mg/g; c 0 And C t The lead ion initial concentration and the concentration after adsorption are respectively, and the unit is mg/L; m is the mass of the adsorbent carbon material, unit g; v is the volume of the solution in L.
The test results are shown in Table 1, fromAs can be seen from the table, the nitrogen-doped carbon materials prepared in this example all exhibited excellent Pb, compared to the non-nitrogen-doped porous activated carbon material (adsorption amount is usually less than 30 mg/g) 2+ And (4) adsorption effect.
TABLE 1
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A method for preparing a nitrogen-doped carbon material, the method comprising: mixing polyaminobenzene hydrochloride with ferric trichloride, calcining in an inert gas atmosphere, and performing post-treatment to obtain the nitrogen-doped carbon material;
wherein, in the polyaminobenzene hydrochloride, the substitution number of amino is 3-5.
2. The method of claim 1, wherein the polyaminobenzene hydrochloride is 1,2, 4-triaminobenzene dihydrochloride.
3. The method for preparing nitrogen-doped carbon material according to claim 2, wherein the mixing is ball milling mixing, the ball grinding material is zirconia balls with the diameter of 3-8mm, the ball milling speed is 50-200rpm, and the ball milling time is 20-30h.
4. The method of claim 1, wherein the calcination is carried out at a temperature of 600-1000 ℃ for 1-10 hours.
5. The method for preparing a nitrogen-doped carbon material according to claim 1, wherein the mixing mass ratio of the polyaminobenzene hydrochloride to the ferric trichloride is (1-10): 1.
6. The method as claimed in claim 1, wherein the post-treatment comprises washing with an acidic solution, washing with deionized water, and drying.
7. The method of claim 6, wherein the acidic solution used in the washing step comprises 0.5-1.5M hydrochloric acid.
8. A nitrogen doped carbon material produced by the method of any one of claims 1 to 7.
9. The use of a nitrogen-doped carbon material according to claim 8, as an adsorbent for the adsorption of heavy metal ions in a body of water.
10. The use of a nitrogen-doped carbon material as claimed in claim 9, wherein said nitrogen-doped carbon material is used as an adsorbent for adsorbing lead ions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110848500.0A CN115672267B (en) | 2021-07-27 | Nitrogen-doped carbon material, preparation method thereof and application thereof in heavy metal ion adsorption |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110848500.0A CN115672267B (en) | 2021-07-27 | Nitrogen-doped carbon material, preparation method thereof and application thereof in heavy metal ion adsorption |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115672267A true CN115672267A (en) | 2023-02-03 |
| CN115672267B CN115672267B (en) | 2024-05-17 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011001772A1 (en) * | 2009-07-03 | 2011-01-06 | 日清紡ホールディングス株式会社 | Oxidation catalyst, reduction catalyst, and catalyst for purging exhaust gas |
| CN102923688A (en) * | 2012-11-01 | 2013-02-13 | 中国科学院长春应用化学研究所 | Preparation method and application of nitrogen-doped carbon material |
| CN106915735A (en) * | 2017-01-25 | 2017-07-04 | 广西大学 | A kind of preparation method of nitrogen or metal-doped carbon material |
| CN109012565A (en) * | 2018-08-07 | 2018-12-18 | 华南理工大学 | A kind of method of the magnetic carbon material Adsorption heavy metal ions in wastewater of nitrating |
| CN109012590A (en) * | 2018-08-24 | 2018-12-18 | 华南理工大学 | A kind of lignin-base transition metal-nitrogen-doped carbon material and its preparation and application |
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011001772A1 (en) * | 2009-07-03 | 2011-01-06 | 日清紡ホールディングス株式会社 | Oxidation catalyst, reduction catalyst, and catalyst for purging exhaust gas |
| CN102923688A (en) * | 2012-11-01 | 2013-02-13 | 中国科学院长春应用化学研究所 | Preparation method and application of nitrogen-doped carbon material |
| CN106915735A (en) * | 2017-01-25 | 2017-07-04 | 广西大学 | A kind of preparation method of nitrogen or metal-doped carbon material |
| CN109012565A (en) * | 2018-08-07 | 2018-12-18 | 华南理工大学 | A kind of method of the magnetic carbon material Adsorption heavy metal ions in wastewater of nitrating |
| CN109012590A (en) * | 2018-08-24 | 2018-12-18 | 华南理工大学 | A kind of lignin-base transition metal-nitrogen-doped carbon material and its preparation and application |
Non-Patent Citations (1)
| Title |
|---|
| 杨晓洁等: "N掺杂有序介孔碳材料的研究进展", 浙江化工, vol. 48, no. 01, pages 26 - 32 * |
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