CN110152608A - A kind of nitrogen-atoms auto-dope chicken feather charcoal adsorbent material and preparation method thereof - Google Patents
A kind of nitrogen-atoms auto-dope chicken feather charcoal adsorbent material and preparation method thereof Download PDFInfo
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- CN110152608A CN110152608A CN201910383649.9A CN201910383649A CN110152608A CN 110152608 A CN110152608 A CN 110152608A CN 201910383649 A CN201910383649 A CN 201910383649A CN 110152608 A CN110152608 A CN 110152608A
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- 241000287828 Gallus gallus Species 0.000 title claims abstract description 48
- 210000003746 feather Anatomy 0.000 title claims abstract description 48
- 239000003610 charcoal Substances 0.000 title claims abstract description 44
- 239000000463 material Substances 0.000 title claims abstract description 38
- 239000003463 adsorbent Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 125000004433 nitrogen atom Chemical group N* 0.000 title claims abstract description 24
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 13
- 125000003118 aryl group Chemical group 0.000 claims abstract description 9
- 125000000524 functional group Chemical group 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 238000005087 graphitization Methods 0.000 claims abstract description 6
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 6
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 230000001681 protective effect Effects 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000004321 preservation Methods 0.000 claims description 15
- 238000010792 warming Methods 0.000 claims description 15
- 239000002028 Biomass Substances 0.000 claims description 13
- 239000012300 argon atmosphere Substances 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 30
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 23
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 10
- 229910052793 cadmium Inorganic materials 0.000 abstract description 7
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract description 7
- 229960002135 sulfadimidine Drugs 0.000 abstract description 5
- ASWVTGNCAZCNNR-UHFFFAOYSA-N sulfamethazine Chemical compound CC1=CC(C)=NC(NS(=O)(=O)C=2C=CC(N)=CC=2)=N1 ASWVTGNCAZCNNR-UHFFFAOYSA-N 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 15
- 238000010521 absorption reaction Methods 0.000 description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- FDDDEECHVMSUSB-UHFFFAOYSA-N sulfanilamide Chemical compound NC1=CC=C(S(N)(=O)=O)C=C1 FDDDEECHVMSUSB-UHFFFAOYSA-N 0.000 description 6
- 229940124530 sulfonamide Drugs 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 241000446313 Lamella Species 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 241000234295 Musa Species 0.000 description 2
- 235000018290 Musa x paradisiaca Nutrition 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 150000003230 pyrimidines Chemical class 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 230000035508 accumulation Effects 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 235000004252 protein component Nutrition 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 230000009919 sequestration Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0259—Compounds of N, P, As, Sb, Bi
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0262—Compounds of O, S, Se, Te
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0262—Compounds of O, S, Se, Te
- B01J20/0266—Compounds of S
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
Abstract
The present invention discloses a kind of nitrogen-atoms auto-dope chicken feather charcoal adsorbent material and preparation method thereof, the adsorbent material has stratiform cross-linked structure, rich in N, S, O activated adoption structure of functional groups and aromatic ring structure is contained, preparation method is to clean chicken feather with clear water, be dried for standby；By the chicken feather of drying crosslinked at low temperature in a nitrogen atmosphere, medium temperature charing high temperature graphitization again, is ground up, sieved, obtains nitrogen-atoms auto-dope chicken feather charcoal adsorbent material under protective atmosphere；Nitrogen-atoms auto-dope chicken feather charcoal adsorbent material of the present invention has the characteristics that adsorption rate capacity is high, it respectively reaches 389.5mg/g and 107.5mg/g to the adsorption capacity of heavy metal cadmium and organic pollutant sulfamethazine, is heavy metal and the Adsorption of Organic agent of a kind of function admirable.
Description
Technical field
It is recycled the invention belongs to biomass castoff and environmental functional new material technology field, in particular to a kind of nitrogen is former
Sub- auto-dope chicken feather charcoal adsorbent material (NSD-CFB) and preparation method.
Background technique
Charcoal is that biomass is carbonized through cracking under limit oxygen or oxygen free condition, a kind of phosphorus content height of generation, flourishing hole
Gap structure, the chemical stability of height, thermal stability, biologically inert and strong characterization of adsorption solid matter.Therefore, charcoal exists
The fields such as agricultural, material and environment possess huge application potential, especially adsorb locking field in soil carbon sequestration and pollutant
And heavy metal ions in sewage and the Adsorption of organic pollutant etc..
Although enriching extensive biomass castoff in world wide provides sufficient raw material for the preparation of charcoal, more
The precursor substance of kind multiplicity also meets the preparation of different application purpose charcoal.However, the challenge in the preparation of charcoal exists
In how selecting specific precursor substance and specific preparation method to realize the preparation of the charcoal of required function.For current
Heavy metal and organic matter cooperate with pollution problem in environmental pollution, how to realize the collaboration removal of heavy metal and organic pollutant simultaneously
Refer to an important directions for causing the design of object carbon structure.
The type of existing charcoal is more, such as patent CN109046244A discloses a kind of cow dung charcoal, granular absorption
The adsorbent of the preparation method and application of agent, this method preparation all have good purification adsorption effect to phosphorus polluted-water, and
Technique is relatively easy easy, mild condition, there is the potentiality of industrialized production.Patent CN109046247A discloses a kind of reinforcing suction
Modification biological charcoal of attached organic dyestuff and preparation method thereof is adsorbed through the modified charcoal of iron chloride with stronger organic dyestuff
Ability.
Be modified to biomass is also research field more popular now, W.J. Liu and H. Jiang
[Environmental Science & Technology, 51 (2017) 10081-10089.] etc. be prepared for magnesia and repair
The N element of decorations adulterates charcoal adsorbent material, and changing adsorbent can reach flat to the absorption of the lead ion in water body in 10min
Weighing apparatus, maximum adsorption capacity is up to 893mg/g.Z. Zhou [Bioresource Technology, 232 (2017) 204-
210.] etc. using fresh and dehydration banana skin as raw material, using a step hydro-thermal charring, it is prepared for biological carbon adsorbent, is used
In the Adsorption of heavy metal lead.The adsorbent surface contains a large amount of hydroxyl and carboxyl, prepared by dehydration and fresh banana skin
Charcoal is respectively 359mg/g and 193mg/g to the maximum adsorption capacity of heavy metal lead.
From it is existing research from the point of view of, using biomass castoff as raw material, prepare by simple method efficiently, can adsorb simultaneously
The stratiform cross-linked porous charcoal adsorbent material of organic pollutant and heavy metal still needs further to be studied.Chicken feather is most commonly seen
One of biomass castoff can only be reprocessed into high level product on a small quantity, and existing most of chicken feather is handled as waste,
It is not fully used.
Summary of the invention
The primary purpose of the present invention is that a kind of nitrogen-atoms auto-dope chicken feather charcoal adsorbent material (NSD-CFB) is provided,
Be prepared by chicken feather biomass, which has stratiform cross-linked structure, rich in containing N, S, O activated adoption structure of functional groups and
Aromatic ring structure.
Another object of the present invention is to provide the system of the nitrogen-atoms auto-dope chicken feather charcoal adsorbent material (NSD-CFB)
Preparation Method, comprising the following steps:
(1) chicken feather cleaned with clear water, be dried for standby；
(2) by the chicken feather crosslinked at low temperature in a nitrogen atmosphere of step (1) drying, medium temperature charing pyrographite again under protective atmosphere
Change, is ground up, sieved, obtains nitrogen-atoms auto-dope chicken feather charcoal (NSD-CFB).
Step (1) drying temperature is 60~100 DEG C.
Step (2) crosslinked at low temperature be warming up to the heating rate of 5~15 DEG C/min 200~240 DEG C heat preservation 120~
240min。
Step (2) medium temperature charing be warming up to the heating rate of 5~15 DEG C/min 400~500 DEG C heat preservation 60~
120min。
Step (2) high temperature graphitization be warming up to the heating rate of 5~15 DEG C/min 600~1000 DEG C heat preservation 30~
90min。
Step (2) protective atmosphere is argon atmosphere or nitrogen atmosphere.
Step (2) sieving is 60~100 meshes.
Nitrogen-atoms auto-dope chicken feather charcoal adsorbent material (NSD-CFB) is repaired field in environmental improvement to apply,
Especially suitable for remediating heavy metal and organic pollution, such as heavy metal and Adsorption of Organic field.
The present invention formed cross-linked network to chicken feather fibers crosslinked at low temperature before this, and the lamella for being conducive to subsequent product is handed over
Connection, and be conducive to its capture to heavy metal contaminants；Then medium temperature carbonizes, and forms stratiform and is crosslinked lamella；Final high temperature graphite
Change, produces porous structure, increase the specific surface area and pore volume of active carbon, and increase aromaticity, be conducive to it to aromatic series
The absorption of organic pollutant.
The present invention using chicken feather as raw material, make full use of in chicken feather fibers polymer and protein component abundant to be easily crosslinked,
Structure is strong and the characteristic of hollow tube, in the case where not adding external source dopant, so as to contain a large amount of activity nitrogenous for charcoal
Functional group realizes the recycling of waste while realizing the preparation of high-performance charcoal.
Chicken feather of the present invention is a kind of biomass castoff rich in protein, have it is from a wealth of sources, cheap, be rich in N
The advantages that with the adsorption activities functional group such as S and adsorption site, no pollution to the environment, as adsorbent material for heavy metal and
Adsorption of Organic is taken naturally, recurrence realizes the recycling of biomass castoff in natural process.
The present invention passes through the adsorbent material that a step programmed temperature method is calcined, and specific surface area and pore volume are big, and tie
Contain a large amount of aromatic structures and nitrogen-containing functional group in structure, provides physical absorption sky simultaneously for the absorption of heavy metal and organic pollutant
Between and chemisorption active site, greatly improve the absorption property of adsorbent material, have adsorption rate capacity high, absorption combines
The features such as ability is strong, thus it has good cost advantage and application prospect in heavy metal adsorption field, can be widely applied to
In environmental improvement reparation field, especially suitable for remediating heavy metal and organic pollution.
Adsorbent material of the invention has combined physical absorption and chemisorption in adsorption process, adsorption rate capacity
Height, adsorption binding energy are strong.Adsorbent material of the present invention is applied in heavy metal adsorption, heavy metal cadmium adsorption capacity is reached
389.5 mg/g are a kind of heavy metal absorbents of function admirable；It is phonetic to sulfanilamide (SN) dimethyl in Adsorption of Organic
The adsorption capacity of pyridine reaches 107.5 mg/g.
The method that the present invention uses is one-step method, and preparation process is simple, easy to operate, convenient for scale industrial production and is answered
With.
Detailed description of the invention
Fig. 1 is the infrared spectrogram for the NSD-CFB-800 that embodiment 1 is prepared；
Fig. 2 is the Raman spectrogram for the NSD-CFB-800 that embodiment 1 is prepared；
Fig. 3 is the specific surface area curve for the NSD-CFB-800 that embodiment 1 is prepared；
Fig. 4 is the pore size distribution curve for the NSD-CFB-800 that embodiment 1 is prepared；
The SEM figure that Fig. 5 is the NSD-CFB-800 that embodiment 1 is prepared；
Fig. 6 is the full spectrogram of XPS for the NSD-CFB-800 that embodiment 1 is prepared；
Fig. 7 is the absorption property of the heavy metal cadmium for the NSD-CFB-800 that embodiment 1 is prepared；
Fig. 8 is the absorption property of the organic pollutant sulfamethazine for the NSD-CFB-800 that embodiment 1 is prepared.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
The reagent that the following example uses can be obtained from commercial channel.
Embodiment 1
A kind of nitrogen-atoms auto-dope chicken feather charcoal adsorbent material (NSD-CFB), is prepared, the charcoal by chicken feather biomass
With stratiform cross-linked structure, rich in N, S, O activated adoption structure of functional groups and aromatic ring structure is contained, specific preparation method is wrapped
Include following steps:
(1) chicken feather that the market of farm produce is collected is cleaned with clear water, it is 24 hours dry in 80 DEG C of air dry ovens, it is dried for standby；
(2) in a nitrogen atmosphere by the chicken feather of step (1) drying, 220 DEG C of heat preservations are warming up to the heating rate of 10 DEG C/min
180min carries out crosslinked at low temperature, is then followed by a nitrogen atmosphere, is warming up to 450 DEG C of heat preservations with the heating rate of 10 DEG C/min
90min carries out medium temperature charing, is warming up to 800 DEG C of heat preservation 60min with the heating rate of 10 DEG C/min and carries out high temperature graphitization, is holding
Room temperature is cooled to the furnace under continuous nitrogen atmosphere, is ground, is crossed 80 meshes, obtains nitrogen-atoms auto-dope chicken feather charcoal (NSD-
CFB-800).
Fig. 1 is the infrared spectrogram of NSD-CFB-800 that the present embodiment is prepared, in figure, in 2090cm-1~
3450cm-1The broad peak at place is the characteristic peak of c h bond and O-H key, 1560cm-1The characteristic peak at place represents stretching for C-C key on carbon skeleton
Contracting vibration, 1121cm-1The broad peak at place is aromatic rings characteristic peak.
Fig. 2 is the Raman spectrogram of NSD-CFB-800 that the present embodiment is prepared, in figure, 1338cm-1Peak be D
Peak represents unordered or defective atomic structure of carbon；1590cm-1Peak be the peak G, represent in the form of sp2 hydridization formed stone
Inkization carbon atom；2796cm-1Width be the peak 2D, represent there are the accumulations of Multi-layer graphite lamella.
Fig. 3 is the specific surface area curve for the NSD-CFB-800 that the present embodiment is prepared；As can be seen from the figure material
Specific surface area is 11.3m2/g。
Fig. 4 is the pore size distribution curve for the NSD-CFB-800 that the present embodiment is prepared；As can be seen from the figure pore volume
For 0.016cm3/ g, aperture 6.20nm.
The SEM figure that Fig. 5 is the NSD-CFB-800 that the present embodiment is prepared；As can be seen from the figure lamellar structure and
Lamella packing phenomenon.
Fig. 6 is the full spectrogram of XPS for the NSD-CFB-800 that the present embodiment is prepared；It can be seen from the figure that NSD-CFB-
The N element of high level is contained on 800 surfaces, and N element content is greater than 10%, it was demonstrated that high N element doping.
The adsorption experiment of heavy metal cadmium, initial Cd are carried out using the material that the present embodiment is prepared2+Concentration is 400mg/L
(ppm), pH value is the original solution that 5.5(does not add any soda acid), liquor capacity 200mL, the suction that the present embodiment is prepared
Attached dose of dosage is 100mg, and in 298K, revolving speed is stir process under 150rpm, as shown in fig. 7, absorption 5min, 10min,
0.5h, 2h, 4h, 6h, 10h and 12h, NSD-CFB-800 is to the adsorption capacity of heavy metal cadmium up to 389.5mg/g, adsorption reaction
It can reach balance at 12 hours.
The adsorption experiment of organic pollutant sulfamethazine is carried out using the material that the present embodiment is prepared, initially
Sulfamethazine concentration is 200mg/L(ppm), pH value is the original solution that 6.0(does not add any soda acid), liquor capacity is
200mL, adsorbent dosage are 100mg, and in 298K, revolving speed is stir process under 150rpm, as shown in figure 8, absorption 5min,
10min, 0.5h, 2h, 4h, 6h, 10h and 12h, NSD-CFB-800 are reachable to the adsorption capacity of sulfamethazine
107.5mg/g, adsorption reaction can reach balance at 12 hours.
Embodiment 2
A kind of nitrogen-atoms auto-dope chicken feather charcoal adsorbent material (NSD-CFB), is prepared, the charcoal by chicken feather biomass
With stratiform cross-linked structure, rich in N, S, O activated adoption structure of functional groups and aromatic ring structure is contained, specific preparation method is wrapped
Include following steps:
(1) chicken feather that the market of farm produce is collected is cleaned with clear water, it is 24 hours dry in 60 DEG C of air dry ovens, it is dried for standby；
(2) in a nitrogen atmosphere by the chicken feather of step (1) drying, 200 DEG C of heat preservations are warming up to the heating rate of 5 DEG C/min
240min carries out crosslinked at low temperature, is then followed by a nitrogen atmosphere, is warming up to 400 DEG C of heat preservations with the heating rate of 5 DEG C/min
120min carries out medium temperature charing, under continuing nitrogen atmosphere, is warming up to 600 DEG C of heat preservation 90min progress with the heating rate of 5 DEG C/min
High temperature graphitization cools to room temperature with the furnace under continuing nitrogen atmosphere, grinds, crosses 60 meshes, obtains nitrogen-atoms auto-dope
Chicken feather charcoal (NSD-CFB-600).
It is detected using the material that the method for embodiment 1 obtains embodiment 2, it is available same as Example 1
As a result；Heavy metal cadmium and organic pollutant sulfanilamide (SN) diformazan are carried out to the material that embodiment 2 obtains using the method for embodiment 1 respectively
The adsorption experiment of yl pyrimidines shows good absorption property.
Embodiment 3
A kind of nitrogen-atoms auto-dope chicken feather charcoal adsorbent material (NSD-CFB), is prepared, the charcoal by chicken feather biomass
With stratiform cross-linked structure, rich in N, S, O activated adoption structure of functional groups and aromatic ring structure is contained, specific preparation method is wrapped
Include following steps:
(1) chicken feather that the market of farm produce is collected is cleaned with clear water, it is 24 hours dry in 100 DEG C of air dry ovens, it is dried for standby；
(2) in a nitrogen atmosphere by the chicken feather of step (1) drying, 240 DEG C of heat preservations are warming up to the heating rate of 15 DEG C/min
120min carries out crosslinked at low temperature, is then followed by under an argon atmosphere, is warming up to 500 DEG C of heat preservations with the heating rate of 15 DEG C/min
60min carry out medium temperature charing, continue argon atmosphere under, with the heating rate of 15 DEG C/min be warming up to 1000 DEG C of heat preservation 30min into
Row high temperature graphitization cools to room temperature with the furnace under lasting argon atmosphere, grinds, crushes, sieves with 100 mesh sieve, and obtains nitrogen-atoms certainly
It adulterates chicken feather charcoal (NSD-CFB-1000).
It is detected using the material that the method for embodiment 1 obtains embodiment 3, it is available same as Example 1
As a result；Heavy metal cadmium and organic pollutant sulfanilamide (SN) diformazan are carried out to the material that embodiment 3 obtains using the method for embodiment 1 respectively
The adsorption experiment of yl pyrimidines shows good absorption property.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (8)
1. a kind of nitrogen-atoms auto-dope chicken feather charcoal adsorbent material, which is characterized in that be prepared by chicken feather biomass, the life
Object charcoal has stratiform cross-linked structure, rich in containing N, S, O activated adoption structure of functional groups and aromatic ring structure.
2. the preparation method of nitrogen-atoms auto-dope chicken feather charcoal adsorbent material described in claim 1, which is characterized in that including with
Lower step:
(1) chicken feather cleaned with clear water, be dried for standby；
(2) by the chicken feather crosslinked at low temperature in a nitrogen atmosphere of step (1) drying, medium temperature charing pyrographite again under protective atmosphere
Change, is ground up, sieved, obtains nitrogen-atoms auto-dope chicken feather charcoal adsorbent material.
3. the preparation method of nitrogen-atoms auto-dope chicken feather charcoal adsorbent material according to claim 2, which is characterized in that step
Suddenly (1) drying temperature is 60~100 DEG C.
4. the preparation method of nitrogen-atoms auto-dope chicken feather charcoal adsorbent material according to claim 2, which is characterized in that step
Suddenly (2) crosslinked at low temperature is that 200~240 DEG C of 120~240min of heat preservation are warming up to the heating rate of 5~15 DEG C/min.
5. the preparation method of nitrogen-atoms auto-dope chicken feather charcoal adsorbent material according to claim 2, which is characterized in that step
Suddenly (2) medium temperature charing is that 400~500 DEG C of 60~120min of heat preservation are warming up to the heating rate of 5~15 DEG C/min.
6. the preparation method of nitrogen-atoms auto-dope chicken feather charcoal adsorbent material according to claim 2, which is characterized in that step
Suddenly (2) high temperature graphitization is that 600~1000 DEG C of 30~90min of heat preservation are warming up to the heating rate of 5~15 DEG C/min.
7. the preparation method of nitrogen-atoms auto-dope chicken feather charcoal adsorbent material according to claim 2, which is characterized in that step
Suddenly (2) protective atmosphere is argon atmosphere or nitrogen atmosphere.
8. the preparation method of nitrogen-atoms auto-dope chicken feather charcoal adsorbent material according to claim 2, which is characterized in that step
Suddenly (2) sieving is 60~100 meshes.
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