CN115028160B - Method for preparing hollow carbon nano cake by utilizing water micro-plastic coagulation floc and application thereof - Google Patents
Method for preparing hollow carbon nano cake by utilizing water micro-plastic coagulation floc and application thereof Download PDFInfo
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- CN115028160B CN115028160B CN202210697572.4A CN202210697572A CN115028160B CN 115028160 B CN115028160 B CN 115028160B CN 202210697572 A CN202210697572 A CN 202210697572A CN 115028160 B CN115028160 B CN 115028160B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 33
- 229920003023 plastic Polymers 0.000 title claims abstract description 32
- 239000004033 plastic Substances 0.000 title claims abstract description 32
- 230000015271 coagulation Effects 0.000 title claims abstract description 19
- 238000005345 coagulation Methods 0.000 title claims abstract description 19
- 238000000197 pyrolysis Methods 0.000 claims abstract description 27
- 239000000701 coagulant Substances 0.000 claims abstract description 17
- 229920000426 Microplastic Polymers 0.000 claims abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims abstract description 9
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 239000000919 ceramic Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 230000001112 coagulating effect Effects 0.000 claims abstract description 4
- 230000001681 protective effect Effects 0.000 claims abstract description 4
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 10
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 7
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000005868 electrolysis reaction Methods 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical compound OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 claims description 2
- 229920001732 Lignosulfonate Polymers 0.000 claims description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 2
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- 239000003463 adsorbent Substances 0.000 claims description 2
- 229940037003 alum Drugs 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 239000000413 hydrolysate Substances 0.000 claims description 2
- 229910001416 lithium ion Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 239000003990 capacitor Substances 0.000 claims 1
- 238000011161 development Methods 0.000 abstract description 2
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- 229920000915 polyvinyl chloride Polymers 0.000 description 15
- 239000004800 polyvinyl chloride Substances 0.000 description 15
- 239000000047 product Substances 0.000 description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 238000004064 recycling Methods 0.000 description 5
- 229940043267 rhodamine b Drugs 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 239000000571 coke Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000004098 Tetracycline Substances 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 230000037406 food intake Effects 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229960002180 tetracycline Drugs 0.000 description 1
- 229930101283 tetracycline Natural products 0.000 description 1
- 235000019364 tetracycline Nutrition 0.000 description 1
- 150000003522 tetracyclines Chemical class 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000002110 toxicologic effect Effects 0.000 description 1
- 231100000759 toxicological effect Toxicity 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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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
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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
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
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- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- 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
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Abstract
The invention discloses a method for preparing a hollow carbon nano cake by utilizing water micro-plastic coagulation flocs, which comprises the following steps: by mixing the water body: coagulant aid: inorganic coagulant: the organic flocculant is prepared from the following components in percentage by mass: (10-200): (1-10): (5-50) coagulating the water body containing the micro plastics to obtain micro plastics coagulated flocs; placing a ceramic crucible into a tubular furnace for pyrolysis, raising the temperature to a target temperature at a specific heating speed, and pyrolyzing for a certain time at a constant temperature, wherein inert gas is used as protective gas; cooling the tubular furnace to room temperature, and grinding and crushing the sample to obtain a hollow carbon nano cake; the prepared hollow carbon nano cake HCNC is a carbon nano cake containing iron element, the diameter range is 200-500 nm, the thickness is 20-100 nm, and the iron atom content is 20-50%. The method is easy to operate, good in repeatability and extremely good in application prospect, and provides a new direction for development and application of sustainable wastewater treatment technology.
Description
Technical Field
The invention belongs to the technical field of sewage treatment and recycling, and particularly relates to a method for preparing a hollow carbon nano cake by utilizing water micro-plastic coagulated flocs and application thereof.
Background
Microplastic is widely found in marine ecosystems, freshwater ecosystems, soil and sediment, even in drinking water, human feces, polar environments. It not only can produce physical injury to living beings through ingestion, can also release or adsorb toxic and harmful pollutants, and has direct or indirect toxicological effect on ecological environment. Flocculation sedimentation is a commonly used technology for removing microplastic at present, and the surface property of the microplastic can be changed by adding a flocculating agent into sewage, so that attraction energy between the microplastic is larger than repulsion energy, and the microplastic is aggregated into a large-block flocculation to be removed by sedimentation. However, a large amount of flocculent sludge is inevitably generated in the disposal process, so that secondary pollution is very easy to cause, but no better solution exists at present.
As is well known, the pyrolysis process is one of the important means for recycling waste plastics at the present stage, and can be used for preparing coke, pyrolysis oil and pyrolysis gas. The pyrolysis process technology provides a new idea for recycling the micro-plastic coagulation flocs. However, the micro plastic coagulated flocs have more impurities, so that the oil and gas production efficiency is very low. Meanwhile, the uncertain component composition of the micro-plastic coagulated floc enables the morphology and the pores of the pyrolytic coke to be uncontrollable, so that the recycling industrialization prospect of the micro-plastic coagulated floc is not clear.
Disclosure of Invention
The invention mainly aims at overcoming the defects of the prior art, and provides a method for preparing a hollow carbon nano cake by utilizing water micro-plastic coagulated flocs.
In a first aspect of the present invention, a method for preparing a hollow carbon nano-cake by using a water micro-plastic coagulation floc is provided, comprising the following steps:
s1, water (calculated by water density of 1 kg/L): coagulant aid: inorganic coagulant: the organic flocculant is prepared from the following components in percentage by mass: (10-200): (1-10): (5-50) coagulating the water body containing the micro plastics to obtain micro plastics coagulated flocs;
s2, placing the obtained micro-plastic coagulated flocs into a tubular furnace for pyrolysis by adopting a ceramic crucible, raising the temperature to a target temperature at a specific heating speed, and pyrolyzing for a certain time at a constant temperature, wherein inert gas is used as a protective gas;
and S3, cooling the tubular furnace to room temperature, and grinding and crushing the cooled sample to obtain the hollow carbon nano cake HCNC.
In some embodiments of the present invention, in step S1, the coagulant aid is a nano-micro electrolytic material, and the specific preparation method is shown in chinese patent No. CN201710247676.4, and is a preparation method of a nano-micro electrolytic material for removing tetracycline pollutants.
In some embodiments of the present invention, in step S1, the inorganic coagulant is selected from at least one of polymeric ferric sulfate PS, polymeric ferric chloride, polymeric aluminum sulfate, aluminum chloride, ferric sulfate, ferric chloride, alum.
In some embodiments of the present invention, in step S1, the organic flocculant is selected from at least one of polyacrylamide PAM, an alkaline hydrolysate of polyacrylamide, polyacrylic acid, sodium polyacrylate, calcium polyacrylate, styrene sulfonate, lignosulfonate, acrylic acid, methacrylic acid.
In some embodiments of the invention, in step S2, the specific heating rate is 5 to 15 ℃; the target temperature is 500-900 ℃; the pyrolysis is carried out for 0.5 to 4 hours.
In some embodiments of the present invention, in step S2, the inert atmosphere is at least one of nitrogen, argon, helium, or carbon dioxide gas.
In some embodiments of the present invention, in step S3, the hollow carbon nano-cake HCNC is a carbon nano-cake containing iron element, and has a diameter ranging from 200 to 500nm, a thickness ranging from 20 to 100nm, and an iron atom content ranging from 20 to 50%.
In a second aspect of the present invention, a hollow carbon nanocake is provided, which is the hollow carbon nanocake obtained by the above method.
In a third aspect of the present invention, the application of the hollow carbon nano-cake prepared by the method in a supercapacitor, an adsorbent, a catalyst or a lithium ion battery is provided.
Compared with the prior art, the invention has the following beneficial effects:
1) The invention takes a water body containing micro plastics as a raw material, and the water body (calculated by water density of 1 kg/L): coagulant aid: inorganic coagulant: the organic flocculant is used for coagulating the raw materials according to a specific mass compounding proportion to obtain micro-plastic coagulated flocs, and the micro-plastic coagulated flocs are pyrolyzed by adopting a specific pyrolysis process condition to prepare the hollow carbon nano cake HCNC which is a carbon nano cake containing iron element, wherein the diameter range is 200-500 nm, the thickness is 20-100 nm, and the iron atom content is 20-50%.
2) The preparation method not only realizes the harmless, reduction and recycling of the micro-plastic coagulation flocs, but also realizes the low-cost preparation of the hollow carbon nano cake HCNC with high added value. The method is easy to operate, good in repeatability and extremely good in application prospect, and provides a new direction for development and application of sustainable wastewater treatment technology.
Drawings
FIG. 1 is a scanning electron microscope image of a hollow carbon nano-cake HCNC at 500nm in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of hollow carbon nano-cake HCNC at 200nm in example 1 of the present invention.
FIG. 3 is a scanning electron microscope image of hollow carbon nano-cake HCNC at 2 μm in example 1 of the present invention.
FIG. 4 is a scanning electron microscope image of the PVC pyrolysis product in comparative example 3 of the present invention at 2. Mu.m.
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present invention based on the embodiments of the present invention.
Test standard or method of each performance index:
test standard or method for iron atom content of hollow carbon nano cake HCNC: an X-ray energy spectroscopy (EDS) analysis;
test standard or method for diameter of hollow carbon nano-cake HCNC: scanning Electron Microscope (SEM) measurements;
test standard or method for the thickness of hollow carbon nanocakes HCNC: scanning Electron Microscope (SEM) measurements;
test standard or method for specific surface area of hollow carbon nano cake HCNC: a specific surface area tester measurement method;
test standard or method for removing effect of hollow carbon nano cake HCNC on 100mL rhodamine b dye with 5mg/L under the same condition: ultraviolet-visible spectrophotometry.
Example 1
A method for preparing a hollow carbon nano cake by utilizing water micro-plastic coagulation flocs comprises the following steps:
s1, calculating the water mass (calculated by water density of 1 kg/L): coagulant aid nano micro-electrolysis material mass: mass of the polymerized ferric sulfate PS: polyacrylamide PAM mass = 1,000,000:50:5:20, carrying out coagulation on the simulated polyvinyl chloride micro-plastic water body containing 100 mu m to obtain micro-plastic coagulated flocs;
s2, placing the obtained microplastic coagulated flocs into a GSL-1600X tubular furnace by adopting a zirconia ceramic crucible for pyrolysis; in the pyrolysis process, a tube furnace (GSL-1600X) is raised to 800 ℃ at a speed of 10 ℃/min, and pyrolyzed at a constant temperature of 800 ℃ for 3 hours, using N 2 As a shielding gas;
and S3, cooling the tubular furnace to room temperature, and grinding and crushing the cooled sample to obtain the hollow carbon nano cake HCNC.
The diameter range of the prepared hollow carbon nano cake HCNC is 200-500 nm, the thickness is 50-100 nm, and the iron atom content is 25-50%; and the specific surface area of the prepared hollow carbon nano cake HCNC (54.37 m 2 /g) is much greater than that of the PVC pyrolysis product (1.53 m 2 Per g), which is 5.5 times more effective at removing 100mL of 5mg/L rhodamine b dye than PVC pyrolysis product under equivalent conditions.
Example 2
A method for preparing a hollow carbon nano cake by utilizing water micro-plastic coagulation flocs comprises the following steps:
s1, calculating the water mass (calculated by water density of 1 kg/L): coagulant aid nano micro-electrolysis material mass: iron sulfate mass: sodium polyacrylate mass = 1,000,000:200:10:50, carrying out coagulation on the simulated polyvinyl chloride micro-plastic water body containing 100 mu m to obtain micro-plastic coagulated flocs;
s2, placing the obtained microplastic coagulated flocs into a GSL-1600X tubular furnace by adopting a zirconia ceramic crucible for pyrolysis; in the pyrolysis process, a tube furnace (GSL-1600X) is raised to 700 ℃ at a rate of 10 ℃/min, and pyrolyzed at constant temperature for 4 hours, using N 2 As a shielding gas;
and S3, cooling the tubular furnace to room temperature, and grinding and crushing the cooled sample to obtain the hollow carbon nano cake HCNC.
The diameter range of the prepared hollow carbon nano cake HCNC is 250-500 nm, the thickness is 50-100 nm, and the iron atom content is 25-50%; and the specific surface area (64.11 m) 2 /g) is much greater than that of the PVC pyrolysis product (1.53 m 2 Per g), which has a 5mg/L removal effect on 100mL of rhodamine b dye at equal conditions of 5.8 times higher than the PVC pyrolysis product.
Example 3
A method for preparing a hollow carbon nano cake by utilizing water micro-plastic coagulation flocs comprises the following steps:
s1, calculating the water mass (calculated by water density of 1 kg/L): coagulant aid nano micro-electrolysis material mass: mass of polyaluminum sulfate: calcium polyacrylate mass = 1,000,000:10:1:5, carrying out coagulation on the simulated polyvinyl chloride micro-plastic water body containing 100 mu m to obtain micro-plastic coagulated flocs;
s2, putting the obtained flocs into a GSL-1600X tubular furnace by adopting a zirconia ceramic crucible for pyrolysis; in the pyrolysis process, a tube furnace (GSL-1600X) is raised to 600 ℃ at a speed of 15 ℃/min, and pyrolyzed for 2 hours at a constant temperature, and argon is used as a protective gas;
and S3, cooling the tubular furnace to room temperature, and grinding and crushing the cooled sample to obtain the hollow carbon nano cake HCNC.
The diameter range of the prepared hollow carbon nano cake HCNC is 200-400 nm, the thickness is 50-90 nm, and the iron atom content is 25-60%; and the specific surface area of the prepared hollow carbon nano cake HCNC (59.37 m 2 /g) is much greater than that of the PVC pyrolysis product (1.53 m 2 Per g), which is 5.6 times more effective than PVC pyrolysis product in removing 100mL of rhodamine b dye at 5mg/L under the same conditions.
Comparative example 1
A method for preparing a hollow carbon nano cake by utilizing water micro-plastic coagulation flocs comprises the following steps:
s1, calculating the water mass (calculated by water density of 1 kg/L): coagulant aid nano micro-electrolysis material mass: mass of the polymerized ferric sulfate PS: polyacrylamide PAM mass = 1,000,000:50:5:2, carrying out coagulation on the simulated polyvinyl chloride micro-plastic water body containing 100 mu m according to the mass ratio to obtain micro-plastic coagulation flocs; otherwise, the same as in example 1 was conducted.
The hollow carbon nano cake can not be prepared.
Comparative example 2
A method for preparing a hollow carbon nano cake by utilizing water micro-plastic coagulation flocs comprises the following steps:
s1, calculating the water mass (calculated by water density of 1 kg/L): coagulant aid nano micro-electrolysis material mass: mass of the polymerized ferric sulfate PS: polyacrylamide PAM mass = 1,000,000:50:5:70, carrying out coagulation on the simulated polyvinyl chloride micro-plastic water body containing 100 mu m to obtain micro-plastic coagulated flocs; otherwise, the same as in example 1 was conducted.
The hollow carbon nano cake can not be prepared.
Comparative example 3
The preparation method of the PVC pyrolysis product comprises the following steps: placing PVC microplastic into a GSL-1600X tubular furnace by adopting a zirconia ceramic crucible for pyrolysis; in the pyrolysis process, a tube furnace (GSL-1600X) was raised to 800℃at a rate of 10℃per minute, and pyrolyzed at constant temperature for 4 hours, using N 2 As a shielding gasA body;
after the tube furnace is cooled to room temperature, the cooled sample is ground and crushed, the obtained PVC pyrolysis product cannot have a hollow carbon nano cake structure (shown in figure 3), and the specific surface area is only 1.53m 2 Per gram, the removal effect of 100mL of 5mg/L rhodamine b dye under the same condition is 13.1 percent.
The foregoing is a further detailed description of the invention in connection with specific/preferred embodiments, and it is not intended that the invention be limited to such description. It will be apparent to those skilled in the art that several alternatives or modifications can be made to the described embodiments without departing from the spirit of the invention, and these alternatives or modifications should be considered to be within the scope of the invention. In the description of the present specification, reference to the terms "one embodiment," "some embodiments," "preferred embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Those skilled in the art may combine and combine the features of the different embodiments or examples described in this specification and of the different embodiments or examples without contradiction. Although embodiments of the present invention and their advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made herein without departing from the scope of the invention as defined by the appended claims.
Claims (4)
1. The method for preparing the hollow carbon nano cake by utilizing the water body micro-plastic coagulation floc is characterized by comprising the following steps of:
s1, water (calculated by water density of 1 kg/L): coagulant aid: inorganic coagulant: the organic flocculant is prepared from the following components in percentage by mass: (10-200): (1-10): (5-50) coagulating the water body containing the micro plastics to obtain micro plastics coagulated flocs;
s2, placing the obtained micro-plastic coagulated flocs into a tubular furnace for pyrolysis by adopting a ceramic crucible, raising the temperature to a target temperature at a specific heating speed, and pyrolyzing for a certain time at a constant temperature, wherein inert gas is used as a protective gas;
s3, cooling the tubular furnace to room temperature, and grinding and crushing the cooled sample to obtain a hollow carbon nano cake HCNC;
in the step S1, the coagulant aid is a nano micro-electrolysis material;
the inorganic coagulant is at least one selected from polymeric ferric sulfate, polymeric ferric chloride, polymeric aluminum sulfate, aluminum chloride, ferric sulfate, ferric chloride and alum;
the organic flocculant is at least one selected from polyacrylamide PAM, alkali-added hydrolysate of polyacrylamide, polyacrylic acid, sodium polyacrylate, calcium polyacrylate, styrene sulfonate, lignosulfonate, acrylic acid and methacrylic acid;
in the step S2, the specific heating speed is 10-15 ℃; the target temperature is 500-900 ℃; the pyrolysis is carried out for 0.5 to 4 hours;
in the step S3, the hollow carbon nano cake HCNC is a carbon nano cake containing iron element, the diameter range is 200-500 nm, the thickness is 20-100 nm, and the iron atom content is 20-50%.
2. The method for preparing hollow carbon nano-cakes by utilizing water micro-plastic coagulation flocs according to claim 1, wherein in the step S2, the inert atmosphere is at least one of nitrogen, argon, helium or carbon dioxide.
3. A hollow carbon nanocake characterized by being obtained by the method of any one of claims 1 to 2.
4. Use of the hollow carbon nano-cake prepared by the method according to any one of claims 1-2 in super capacitors, adsorbents, catalysts or lithium ion batteries.
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