CN106512930A - Preparation method and application of durian skin based biomass charcoal material - Google Patents
Preparation method and application of durian skin based biomass charcoal material Download PDFInfo
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- CN106512930A CN106512930A CN201610897895.2A CN201610897895A CN106512930A CN 106512930 A CN106512930 A CN 106512930A CN 201610897895 A CN201610897895 A CN 201610897895A CN 106512930 A CN106512930 A CN 106512930A
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- 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
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- 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
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- 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
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Abstract
The invention discloses a method for preparing a biomass charcoal material by utilizing waste durian skin and an application of the biomass charcoal material in adsorbing oils and organic substances. The preparation method specifically comprises the following steps of removing hard outer skin of the durian skin, performing thorough washing, performing dicing, and sequentially performing treatment such as hydrothermal treatment, hot-water-bath soaking, freeze-drying, high-temperature pyrolysis in a nitrogen-gas atmosphere and the like, thereby obtaining the durian skin based biomass charcoal material. After the durian skin based biomass charcoal material is soaked into oil or organic solvents to conduct static and sufficient adsorption, a blocky adsorbent is taken out, so that separation can be realized. Besides, regeneration of the adsorbent can be realized through a method of evaporating the solvent.
Description
Technical field
The present invention relates to a kind of preparation method of durian peel based biomass Carbon Materials and its absorption oils and organic matter should
With, belong to biomass carbon sorbing material prepare and water pollution process field.
Background technology
In recent years, each type organic incident of leakage for taking place frequently further has increased earth water resources crisis, and to natural ring
Border and human health cause serious harm.The method of traditional process organic wastewater includes chemical method (such as dispersion method, original
Position combustion method and coacervation), Physical (separating organic matter and water by Large Oil moisture disembarkation and common felt etc.) and bioanalysis.
Chemical method typically easily causes secondary pollution;Physical is often related to complex device, high cost, low separation efficiency;Bioanalysis is adopted
Microorganism often have selective, i.e., a kind of microorganism is typically only capable to process a kind of organic matter, high cost.At present, physics or
The equipment and instrument that the absorption method of chemistry is related to is simple, and treatment technology is easy, therefore advantage of lower cost, therefore widely closed
Note.Developing inexpensive efficient adsorbent has become a big study hotspot for processing organic wastewater.
All kinds of Carbon Materials are to study more Adsorption of Organic agent at present.Traditional carbon/carbonaceous class material such as activated carbon, its
Main component is carbon, and surface functional group enriches, and hole is flourishing, and specific surface area is generally up to 500~1200m2/ g, to organic
Thing has certain suction-operated, but its adsorption efficiency is relatively low, expensive, and regeneration is complicated, separates difficulty, therefore its application is limited
System.It is in order to overcome the shortcomings of traditional Carbon Materials, various new with graphite, Graphene, CNT and shitosan etc. as raw material
The Carbon Materials of oil suction and organic solvent are successfully prepared out.For example, the Graphene raw material of wood-charcoal of the high-strength light that Xu etc. is prepared
Material shows excellent super-hydrophobicity and super-oleophilic, and the adsorption capacity up to 100 to various oils for testing and organic matter~
260g/g(L.Xu,G.Xiao,et al.Superhydrophobic and superoleophilicgraphene aerogel
prepared by facile chemical reduction[J].J.Mater.Chem.A,2015,3,7498-7504.);
S.Kabiri etc. has gone out the graphene-carbon nano tube aeroge with tridimensional network by Material synthesis of graphite, as a result table
The bright aeroge prepared is preferable to various oil products, fat and organic solvent adsorption effect, particularly under vacuum
Persistently adsorb, adsorbable 28L oil (S.Kabiri, D.N.H.Tran, the et al.Outstanding of every gram of adsorbent
adsorption performance of graphene–carbon nanotube aerogels for continuous
oil removal[J].Carbon,2014,80,523-533.).Although these novel charcoal materials are to various oils and organic matter
Pollution entering the water shows good absorption property, but the most still prices of its preparing raw material are higher, and synthetic method is loaded down with trivial details, is also easy to produce
Secondary pollution.Therefore, some researchers are from from raw material with low cost and to simplify carbon Carbon Materials preparation technologies two big
Aspect is started with, and has inquired into the preparation method of carbon/Carbon Materials, and has achieved certain progress.Some common biological materials such as west
Melon, wax gourd, sugarcane etc. are used for preparing Carbon Materials, on the one hand considerably reduce cost of material, another aspect plant biomass
Material contains the macromolecular substances of the special constructions such as a large amount of celluloses rich in carbon, hemicellulose and lignin, and inorganic matter contains
Low, compound with regular structure is measured, the structure for the tridimensional network of Carbon Materials provides excellent presoma.But report at present
Biomass carbon material is also little, and has certain economic worth the raw material for utilizing more, therefore its cost needs further to be reduced.
Durian peel is a kind of fruit accessory substance, and aboundresources, easily regeneration have the advantages that biomass, i.e. microstructure rule
It is whole, rich in compositions such as cellulose, hemicellulose and lignin, it is a kind of desirable feedstock for preparing Carbon Materials.Even so, daily
In life, durian peel is more by as a kind of discarded object, discard processing.As its yield is huge, smell is unique, therefore causes more
The serious wasting of resources and environmental pollution.Therefore, the process of durian peel and recycling problem also result in the highest attention of people.
The content of the invention
It is an object of the invention to discarded durian peel as raw material, there is provided a kind of system of durian peel based biomass Carbon Materials
Preparation Method and its application in terms of oils and organic wastewater process, further reduce the preparation cost of biomass carbon material,
And propose the thinking of the recycling of a discarded durian peel.
Technical scheme is as follows:
A kind of preparation method of durian peel based biomass Carbon Materials, it is characterised in that utilize discarded durian peel to be three dimensional network
Shape structure charcoal material precursor, and it is related to that the hydro-thermal of durian peel is tentatively carbonized, freeze-drying keeps high in pattern and nitrogen atmosphere
Temperature three big processes of carbonization.Comprise the following steps that:The discarded durian peel collected is removed into the hard barbed epidermis of yellow green, is cleaned, stripping and slicing,
10~24h of hydro-thermal process at a temperature of 150~220 DEG C, immersion in hot bath remove soluble impurity.Then, will be soaked
Durian peel is freezed, and -80 DEG C of freeze-drying 24-48h in vacuum freezing drying oven;Finally, by material 800 in nitrogen atmosphere
DEG C pyrolysis 1~5h, obtain final product durian peel based biomass Carbon Materials.
The adsorbent for preparing according to the method described above is used for the field of waste water treatment containing oils or organic liquid by the present invention, and
Achieve preferable adsorption effect.Described oils and organic liquid include:Pump oil, castor oil, N,N-dimethylformamide
(DMF), ethanol, acetone, paraxylene (PX), normal heptane, toluene, methyl alcohol, formic acid, 1-METHYLPYRROLIDONE (NMP) etc..This
Outward, the durian peel based biomass Carbon Materials that prepared by the present invention can realize regeneration by the method for evaporation solvent.
Compared with prior art, it is an advantage of the current invention that:
1. durian peel is a kind of fruit accessory substance, and substantially without economic worth, yield is huge, is often dropped, or even causes tight
The environmental pollution of weight.Adsorbent is prepared from durian peel for raw material, not only reduce further absorption cost, be also beneficial to realize
The recycling of discarded durian peel.Simultaneously to contain a large amount of celluloses rich in carbon, hemicellulose and lignin etc. special for durian peel
The macromolecular substances of structure, inorganic content are low, compound with regular structure, for the tridimensional network of Carbon Materials structure provide it is excellent
Presoma.
2. the present invention has prepared light porous, high-specific surface area by steps such as hydro-thermal, freeze-drying and pyrolysis, and inhales
The durian peel based biomass Carbon Materials of attached excellent performance.The preparation method equipment is relatively easy, and energy consumption is relatively low, pollution-free produce
Raw, environmental protection is easy.
3. the durian peel based biomass Carbon Materials absorption oils and the method for organic solvent that the present invention is provided easily is implemented, and adsorbs
Speed is fast, and adsorption efficiency is high, and lock out operation is convenient, and cycle performance is excellent, and is capable of achieving absorption by simple evaporation solvent
Regeneration.
Description of the drawings
In conjunction with the following drawings, the embodiment of the present invention or technical scheme of the prior art is specifically illustrated, but is retouched below
Accompanying drawing for the present invention in stating is only some embodiments of the present invention, rather than limits the scope of the present invention.
Fig. 1 is the SEM figures of sample 1 (1a), sample 2 (1b) and sample 3 (1c) prepared by embodiment 1.
Fig. 2 is the N of sample 3 prepared by embodiment 12Adsorption desorption curve.
Fig. 3 is the pore diameter distribution figure of sample 3 prepared by embodiment 1.
Fig. 4 is the FTIR spectrograms of sample 1, sample 2 and sample 3 prepared by embodiment 1.
Fig. 5 is the Raman spectrograms of sample 1, sample 2 and sample 3 prepared by embodiment 1.
Fig. 6 is the XRD spectra of sample 1, sample 2 and sample 3 prepared by embodiment 1.
Fig. 7 is the durian peel based biomass Carbon Materials that measure of embodiment 2 to common oils and the adsorption effect figure of organic matter.
Fig. 8 is suction-de-adsorption cycle design sketch of the durian peel based biomass Carbon Materials that measure of embodiment 3 to acetone solvent.
Specific embodiment
Be expanded on further the present invention with reference to specifically embodiment, but these embodiments be merely to illustrate the present invention and
It is not used in restriction the scope of the present invention.
Embodiment 1
The present invention prepares durian peel based biomass Carbon Materials by following methods, and which is characterized.
Fresh durian peel removes the hard barbed epidermis of yellow green, respectively with running water and distillation water washing 3 times, stripping and slicing, Yu Bing
- 20 DEG C of freezing 24h in case, and -80 DEG C of freeze-drying 48h in vacuum freezing drying oven, obtain sample 1.
Fresh durian peel removes the hard barbed epidermis of yellow green, and respectively with running water and distillation water washing 3 times, stripping and slicing is put into water
In thermal response kettle, 180 DEG C of hydro-thermal reactions 10h in air dry oven are placed in preliminary carbonization durian peel in 70 DEG C of hot baths and soak
Bubble 2 days.Then, soaked durian peel is placed in in refrigerator -20 DEG C of freezing 24h, and in vacuum freezing drying oven -80 DEG C it is cold
Dry 48h is freezed, sample 2 is obtained.
Fresh durian peel removes the hard barbed epidermis of yellow green, and respectively with running water and distillation water washing 3 times, stripping and slicing is put into water
In thermal response kettle, 180 DEG C of hydro-thermal reactions 10h in air dry oven are placed in preliminary carbonization durian peel in 70 DEG C of hot baths and soak
Bubble 2 days, removes soluble impurity.Then, soaked durian peel is placed in into -20 DEG C of freezing 24h in refrigerator, and in vacuum refrigeration
- 80 DEG C of freeze-drying 48h in drying box.Finally, material is pyrolyzed into 1h for 800 DEG C in nitrogen atmosphere, obtains sample 3, i.e. durian peel
Based biomass Carbon Materials.
By SEM technologies, the microscopic appearance of sample 1, sample 2 and sample 3 is observed, as a result as shown in Figure 1.As can be seen that
Natural durian peel (sample 1) has cellular pore structure, and its (sample 2) after hydro-thermal process still remains raw material
Cellular pattern, only because carbonization causes frame sheet to become more loose, this explanation hydro-thermal process is to material morphology
Affect little.Sample 3 also remains the tridimensional network of raw material well, and the microcosmic shape of the tubular porous curled is presented
Looks, this should be caused by the cellular pore passage structure of durian peel is shunk during Pintsch process.This abundant loose structure makes
The specific surface area for obtaining the durian peel based biomass Carbon Materials of preparation of the present invention is up to 734.96m2/ g, and its bore dia integrated distribution
In 3.59nm, belong to mesoporous size range, Fig. 2 and Fig. 3 is the N of the sample 3 measured using BET methods respectively2Adsorption/desorption
Curve and graph of pore diameter distribution.Additionally, the durian peel based biomass Carbon Materials total pore volume that measures of BET method and average pore size are respectively
0.5063cm3/ g and 2.76nm.Therefore, the durian peel based biomass Carbon Materials that prepared by the present invention have abundant meso-hole structure,
Specific surface area is big, is conducive to oils and organic matter to be in contact with it, and is adsorbed.
Fig. 4 is the FTIR spectrograms of three kinds of samples.- OH is occurred in that in the FTIR spectrograms of natural durian peel (sample 1)
(3420cm-1And 1380cm-1Neighborhood), C=O (1740cm-1、1320cm-1、1110cm-1And 1060cm-1Neighborhood), fragrance
Race C=C (1640cm-1Neighborhood) and C-H (2920cm-1、777cm-1And 623cm-1Neighborhood) etc. group vibration adsorption peak,
Illustrate natural durian peel rich in functional groups such as hydroxyl, carbonyl, carboxyl, aromatic groups.In the spectrogram of sample 2,3420cm-1Place
- OH stretching vibration absworption peak remitted its furys, 1740cm-1, 1110cm-1And 1060cm-1Vicinity C=O absorption peak strength
Also the decrease of different amplitudes, or even disappearance, 2920cm-1Neighborhood C-H vibration absorption peak remitted its furys.In the spectrogram of sample 3, phase
The absworption peak of the groups such as-OH ,-COOH and C-H for closing further weakens.This is because glucide (the fiber that durian peel contains
Element etc.) the preliminary hydro-extraction carbonization in water-heat process, form the material such as furfural, then-the OH in high temperature pyrolysis, durian peel and-
The functional groups such as COOH and other macromolecule carbon chains further decompose, and carbonizing degree is deepened.Additionally, Fig. 5 is the Raman of three kinds of samples
Spectrogram.The Raman spectrograms of Carbon Materials have two common characteristic peak G peaks and D peaks, and which reflects the carbon atom in graphite linings respectively
Tangential vibrations and agraphitic carbon (or defect graphite-structure), and both integrated intensity ratio with Carbon Materials graphite linings it is orderly
Degree is related.As shown in Figure 5, with the intensification of processing procedure, the integrated intensity ratio at the G peaks and D peaks of the Raman spectrograms of three kinds of samples
Taper into, illustrate that the carbonizing degree of material is deepened, the sample 3 obtained through hydro-thermal and high temperature pyrolysis is agraphitic carbon structure,
This is almost consistent with the result of XRD spectrum (Fig. 6).Compared to sample 1 and 2, the biomass carbon aeroge (sample finally prepared
3) XRD spectra occurs in that two broad peaks near 23 ° and 43 °, that reflects the agraphitic carbon Rotating fields of material internal, may
It is that some remaining oxy radicals after pyrolysis in raw material are produced.
Embodiment 2
Adsorption rate test experiments:Take sample 3 (the durian peel based biomass Carbon Materials) title that 1 method of a piece of embodiment is prepared
Weight, is then immersed in standing adsorption 30s~5min in oils or organic liquid, takes out, weighs immediately, calculates the suction of adsorbent
Attached ability.
The computing formula of adsorbent power that the present invention is provided is:
Adsorption rate (%)=(m2-m1)/m1*100 (1)
Wherein, m1And m2Refer to adsorbent absorption oils or the quality before and after organic liquid respectively.
Durian peel based biomass Carbon Materials are calculated to pump oil, castor oil, N,N-dimethylformamide using formula (1)
(DMF), the oils such as ethanol, acetone, paraxylene (PX), normal heptane, toluene, methyl alcohol, formic acid, 1-METHYLPYRROLIDONE (NMP)
Or the adsorption rate of organic matter, as a result as shown in Figure 7.Various oils and organic solvent of the durian peel based biomass Carbon Materials to test
Show preferably absorption property, the i.e. rate of adsorption very fast, 30s or so can reach saturation absorption, and adsorption rate is high, keeps
In the range of 324%~1843%.
Embodiment 3
Cycle performance test experiments:Take the sample 3 (durian peel based biomass Carbon Materials) that 1 method of a piece of embodiment is prepared
Weigh, be then immersed in standing adsorption 30s~5min in acetone, take out, weigh immediately, calculate the first time circulation of adsorbent
Adsorption rate.Then, the adsorbent after absorption is placed in surface plate, is placed in air dry oven, 100 DEG C of dryings are to constant weight
(20min), complete first time adsorption-desorption-regeneration cycle experiment.
According to step described above, 5 adsorption-desorption-regeneration cycle experiments are carried out, as shown in figure 8, structure shows durian
Scytoblastema biomass carbon material has good regeneration cycle performance, the 5th adsorption-desorption-regeneration cycle mistake to acetone solvent
The adsorption rate of journey is the 95% of the adsorption rate of the 1st cyclic process.Furthermore, it is possible to be realized by the method for simple evaporation solvent
The regeneration of adsorbent.
Claims (6)
1. a kind of preparation method of durian peel based biomass Carbon Materials, it is characterised in that:With resourceful discarded object durian peel
For raw material, successively durian peel hydro-thermal is tentatively carbonized, height in soluble impurity, freeze-drying holding pattern and nitrogen atmosphere is removed
Temperature carbonization, obtains durian peel based biomass charcoal material sorbent.
2. the preparation method of a kind of durian peel based biomass Carbon Materials according to claim 1, it is characterised in that:To collect
Discarded durian peel remove the hard barbed epidermis of yellow green, clean, stripping and slicing, 10~24h of hydro-thermal process at a temperature of 150~220 DEG C,
In hot bath, immersion removes soluble impurity;Then, soaked durian peel is freezed, and -80 in vacuum freezing drying oven
DEG C freeze-drying 24-48h;Finally, material is pyrolyzed into 1~5h for 800 DEG C in nitrogen atmosphere, obtains final product durian peel based biomass raw material of wood-charcoal
Material.
3. the preparation method of a kind of durian peel based biomass Carbon Materials according to claim 1, it is characterised in that:The pomegranate
Lotus scytoblastema biomass carbon material be bulk material, hole enrich, the aperture size that BET method is measured belongs to macropore range.
4. the durian peel based biomass Carbon Materials that according to claim 1 prepared by preparation method be used for adsorbing in waste water oils and
The purposes of organic liquid.
5. purposes according to claim 4, it is characterised in that described oils and organic liquid include:Pump oil, castor-oil plant
Oil, N,N-dimethylformamide (DMF), ethanol, acetone, paraxylene (PX), normal heptane, toluene, methyl alcohol, formic acid and N- methyl
Pyrrolidones (NMP).
6. purposes according to claim 4, it is characterised in that:Durian peel based biomass Carbon Materials can be by evaporation solvent
Mode realizes adsorbent reactivation.
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Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107253720A (en) * | 2017-06-21 | 2017-10-17 | 中南大学 | A kind of high specific surface area and mesoporous activated carbon and preparation method thereof and the application in ultracapacitor |
CN107286884A (en) * | 2017-07-31 | 2017-10-24 | 安徽佳诺威木业有限公司 | A kind of preparation method of the plain aeroge Lauxite glue additive of manganese dioxide chitosan Carbon fibe |
CN107442062A (en) * | 2017-09-08 | 2017-12-08 | 安徽玄同工业设计有限公司 | A kind of preparation method of methylene blue adsorption number agent |
CN107486198A (en) * | 2017-08-02 | 2017-12-19 | 江苏大学 | A kind of Bi based on the modification of peach blossom biomass carbon2WO6The Preparation method and use of composite photo-catalyst |
CN107651687A (en) * | 2017-11-16 | 2018-02-02 | 湘潭大学 | A kind of preparation method and applications of the Carbon Materials rich in pyridine nitrogen |
CN111204831A (en) * | 2020-01-19 | 2020-05-29 | 陕西科技大学 | CNF-based homologous heterogeneous photothermal material for seawater desalination and preparation method thereof |
CN111785892A (en) * | 2019-04-03 | 2020-10-16 | 中南大学 | Preparation method of lithium-sulfur battery composite diaphragm |
CN111785912A (en) * | 2019-04-03 | 2020-10-16 | 中南大学 | Preparation method of novel porous carbon cathode lithium-sulfur battery |
CN111905694A (en) * | 2020-07-23 | 2020-11-10 | 江苏大学 | Preparation of copper-aluminum bimetal oxide modified durian shell biomass carbon fiber composite material and application of composite material in removing ammonia nitrogen in water |
CN113070044A (en) * | 2021-03-18 | 2021-07-06 | 武汉轻工大学 | Aflatoxin detoxication agent and preparation method and application thereof |
CN114192147A (en) * | 2021-11-30 | 2022-03-18 | 华中科技大学 | Method and system for preparing three-dimensional net-shaped Ni/CA catalyst by comprehensively treating fruit and vegetable waste and nickel plating wastewater |
CN115554979A (en) * | 2022-10-12 | 2023-01-03 | 云南中烟工业有限责任公司 | Method for adsorbing tobacco essence by using charcoal material |
CN116443849A (en) * | 2023-04-27 | 2023-07-18 | 安徽建筑大学 | Porous carbon material with high specific surface area and preparation method and application thereof |
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CN107486198B (en) * | 2017-08-02 | 2020-08-28 | 江苏大学 | Bi based on peach blossom biomass carbon modification2WO6Preparation method and application of composite photocatalyst |
CN107486198A (en) * | 2017-08-02 | 2017-12-19 | 江苏大学 | A kind of Bi based on the modification of peach blossom biomass carbon2WO6The Preparation method and use of composite photo-catalyst |
CN107442062A (en) * | 2017-09-08 | 2017-12-08 | 安徽玄同工业设计有限公司 | A kind of preparation method of methylene blue adsorption number agent |
CN107651687A (en) * | 2017-11-16 | 2018-02-02 | 湘潭大学 | A kind of preparation method and applications of the Carbon Materials rich in pyridine nitrogen |
CN111785892A (en) * | 2019-04-03 | 2020-10-16 | 中南大学 | Preparation method of lithium-sulfur battery composite diaphragm |
CN111785912A (en) * | 2019-04-03 | 2020-10-16 | 中南大学 | Preparation method of novel porous carbon cathode lithium-sulfur battery |
CN111204831A (en) * | 2020-01-19 | 2020-05-29 | 陕西科技大学 | CNF-based homologous heterogeneous photothermal material for seawater desalination and preparation method thereof |
CN111905694A (en) * | 2020-07-23 | 2020-11-10 | 江苏大学 | Preparation of copper-aluminum bimetal oxide modified durian shell biomass carbon fiber composite material and application of composite material in removing ammonia nitrogen in water |
CN113070044A (en) * | 2021-03-18 | 2021-07-06 | 武汉轻工大学 | Aflatoxin detoxication agent and preparation method and application thereof |
CN114192147A (en) * | 2021-11-30 | 2022-03-18 | 华中科技大学 | Method and system for preparing three-dimensional net-shaped Ni/CA catalyst by comprehensively treating fruit and vegetable waste and nickel plating wastewater |
CN115554979A (en) * | 2022-10-12 | 2023-01-03 | 云南中烟工业有限责任公司 | Method for adsorbing tobacco essence by using charcoal material |
CN116443849A (en) * | 2023-04-27 | 2023-07-18 | 安徽建筑大学 | Porous carbon material with high specific surface area and preparation method and application thereof |
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