CN115028160A - Method for preparing hollow carbon nano-cake by using water body micro-plastic coagulated flocs and application thereof - Google Patents
Method for preparing hollow carbon nano-cake by using water body micro-plastic coagulated flocs and application thereof Download PDFInfo
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- CN115028160A CN115028160A CN202210697572.4A CN202210697572A CN115028160A CN 115028160 A CN115028160 A CN 115028160A CN 202210697572 A CN202210697572 A CN 202210697572A CN 115028160 A CN115028160 A CN 115028160A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 55
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229920003023 plastic Polymers 0.000 title claims abstract description 39
- 239000004033 plastic Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000000197 pyrolysis Methods 0.000 claims abstract description 27
- 239000000701 coagulant Substances 0.000 claims abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007789 gas Substances 0.000 claims abstract description 9
- 230000001112 coagulating effect Effects 0.000 claims abstract description 8
- 239000000919 ceramic Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 229910052742 iron Inorganic materials 0.000 claims abstract description 5
- 230000001681 protective effect Effects 0.000 claims abstract description 4
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 229920000426 Microplastic Polymers 0.000 claims description 13
- 229920002401 polyacrylamide Polymers 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 238000005868 electrolysis reaction Methods 0.000 claims description 9
- 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 8
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 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
- 239000003344 environmental pollutant Substances 0.000 claims description 3
- 231100000719 pollutant Toxicity 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
- 239000004098 Tetracycline Substances 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
- 239000003990 capacitor Substances 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
- 229960002180 tetracycline Drugs 0.000 claims description 2
- 229930101283 tetracycline Natural products 0.000 claims description 2
- 235000019364 tetracycline Nutrition 0.000 claims description 2
- 150000003522 tetracyclines Chemical class 0.000 claims description 2
- 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
- 229940043267 rhodamine b Drugs 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 238000004064 recycling Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 239000000571 coke Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 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
- 230000004075 alteration Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000013329 compounding Methods 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
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 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
- 238000004519 manufacturing process 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
- 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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- C—CHEMISTRY; METALLURGY
- 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
-
- 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
-
- 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
-
- 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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- B01J35/23—
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- B01J35/613—
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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
-
- 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
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
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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
- C02F1/54—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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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
Abstract
The invention discloses a method for preparing hollow carbon nano-cakes by utilizing water body micro-plastic coagulated flocs, which comprises the following steps: by mixing a water body: coagulant aid: inorganic coagulant: the organic flocculant is prepared from the following components in a mass ratio of 1,000,000: (10-200): (1-10): (5-50) coagulating the water body containing the micro-plastics to obtain micro-plastic coagulated flocs; putting a ceramic crucible into a tubular furnace for pyrolysis, raising the temperature to a target temperature at a specific heating speed, pyrolyzing for a certain time at a constant temperature, and using inert gas as protective gas; cooling the tube furnace to room temperature, grinding and crushing the sample to obtain a hollow carbon nano cake; the hollow carbon nano-cake HCNC is a carbon nano-cake containing iron elements, the diameter range is 200-500 nm, the thickness is 20-100 nm, and the content of iron atoms is 20-50%. The method is easy to operate, has good repeatability and great application prospect, and provides a new direction for the development and application of a 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 hollow carbon nano-cakes by utilizing water body micro-plastic coagulated flocs and application thereof.
Background
Micro-plastics are widely found in marine ecosystems, freshwater ecosystems, soils and sediments, even in drinking water, human feces, polar environments. It can not only cause biological physiological damage through ingestion, but also release or adsorb toxic and harmful pollutants, and produce direct or indirect toxicological effects on the ecological environment. The flocculation sedimentation is a common micro-plastic removal technology at present, and the surface properties of micro-plastics can be changed by adding a flocculating agent into sewage, so that the attraction energy among the micro-plastics is greater than the repulsion energy, and the micro-plastics are aggregated into large floccules to be removed through sedimentation. However, a large amount of flocculent sludge is inevitably generated in the disposal process, which is very easy to cause secondary pollution, but no better solution is provided at present.
As is well known, the pyrolysis process is one of the important means for recycling waste plastics at present stage, and can be used for preparing coke, pyrolysis oil and pyrolysis gas. The pyrolysis technology provides a new idea for recycling the micro plastic coagulated flocs. But the micro plastic coagulation flocs have a lot of impurities, so that the oil and gas production efficiency is very low. Meanwhile, the appearance and the pores of the pyrolytic coke are uncontrollable due to uncertain component composition of the micro plastic coagulated flocs, so that the prospect of recycling industrialization of the micro plastic coagulated flocs is unknown.
Disclosure of Invention
The invention mainly aims to provide a method for preparing hollow carbon nano-cakes by utilizing water body micro-plastic coagulated flocs aiming at the defects of the prior art.
The invention provides a method for preparing hollow carbon nano-cake by utilizing water body micro-plastic coagulated floc, which comprises the following steps:
s1, by mixing the water body (calculated by the water density of 1 kg/L): coagulant aid: inorganic coagulant: the organic flocculant is prepared from the following components in a mass ratio of 1,000,000: (10-200): (1-10): (5-50) coagulating the water body containing the micro-plastics to obtain micro-plastic coagulated flocs;
s2, putting the obtained micro plastic coagulated flocs into a tubular furnace by adopting a ceramic crucible for pyrolysis, raising the temperature to a target temperature at a specific heating speed, pyrolyzing for a certain time at a constant temperature, and using inert gas as protective gas;
and S3, cooling the tube furnace to room temperature, grinding and crushing the sample cooled to room temperature 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-electrolysis material, and the specific preparation method is described in chinese patent No. CN201710247676.4, and the preparation method of the nano micro-electrolysis material for removing tetracycline pollutants.
In some embodiments of the 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, and alum.
In some embodiments of the present invention, in step S1, 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 some embodiments of the present invention, in step S2, the specific heating rate is 5 to 15 ℃; the target temperature is 500-900 ℃; the pyrolysis is carried out for a certain time of 0.5 h-4 h.
In some embodiments of the invention, in step S2, the inert atmosphere is at least one of nitrogen, argon, helium or carbon dioxide.
In some embodiments of the invention, in step S3, the hollow carbon nanocake HCNC is a carbon nanocake containing iron element, the diameter is 200 to 500nm, the thickness is 20 to 100nm, and the iron atom content is 20 to 50%.
In a second aspect of the invention, a hollow carbon nano-cake is provided, which is obtained by the method.
In a third aspect of the invention, the application of the hollow carbon nano cake prepared by the method in a super capacitor, 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 water containing micro-plastics as raw material, and the water (calculated by water density 1 kg/L): coagulant aid: inorganic coagulant: the raw materials are coagulated by an organic flocculant according to a specific mass compounding ratio to obtain micro plastic coagulated flocs, and the micro plastic coagulated flocs are pyrolyzed by adopting a specific pyrolysis process condition to prepare hollow carbon nano-cake HCNC, wherein the hollow carbon nano-cake HCNC is a carbon nano-cake containing iron elements, the diameter range is 200-500 nm, the thickness is 20-100 nm, and the content of iron atoms is 20-50%.
2) The preparation method not only realizes the harmlessness, reduction and recycling of the micro-plastic coagulated 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 wide in application prospect, and provides a new direction for the development and application of a 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 a hollow carbon nano-cake HCNC at 200nm in example 1 of the present invention.
FIG. 3 is a scanning electron micrograph of a hollow carbon nanocompact HCNC at 2 μm in example 1 of the present invention.
FIG. 4 is a scanning electron micrograph of a PVC pyrolysis product at 2 μm in comparative example 3 of the present invention.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
The test standard or method of each performance index is as follows:
the test standard or method for the iron atom content of the hollow carbon nano cake HCNC comprises the following steps: x-ray energy spectroscopy (EDS) analysis;
test standards or methods for the diameter of hollow carbon nanofillers HCNC: scanning Electron Microscope (SEM) measurements;
test standard or method for thickness of hollow carbon nano-cake HCNC: scanning Electron Microscope (SEM) measurements;
test standards or methods for specific surface area of hollow carbon nanofillers HCNC: measuring by a specific surface area tester;
a test standard or method for the removal effect of the hollow carbon nano-cake HCNC on 100mL of 5mg/L rhodamine b dye under the same condition is as follows: ultraviolet-visible spectrophotometer measurement.
Example 1
A method for preparing hollow carbon nano-cakes by utilizing micro-plastic coagulated flocs in water comprises the following steps:
s1, obtaining the water body by calculating the mass of the water body (calculated by the water density of 1 kg/L): the coagulant aid nanometer micro-electrolysis material has the following quality: the mass of the polymerized ferric sulfate PS is as follows: polyacrylamide PAM mass 1,000,000: 50: 5: 20, coagulating a simulated polyvinyl chloride micro-plastic water body with the particle size of 100 mu m to obtain micro-plastic coagulated flocs;
s2, putting the obtained micro plastic coagulated flocs into a GSL-1600X tubular furnace by adopting a zirconia ceramic crucible for pyrolysis; during pyrolysis, a tube furnace (GSL-1600X) was ramped up to 800 ℃ at a rate of 10 ℃/min and pyrolyzed at a constant temperature of 800 ℃ for 3h using N 2 As a shielding gas;
and S3, cooling the tube furnace to room temperature, grinding and crushing the sample cooled to room temperature 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 content of iron atoms is 25-50%; and the specific surface area (54.37 m) of the hollow carbon nano-cake HCNC obtained by preparation 2 Per g) much greater than that of the pyrolysis product of PVC (1.53 m) 2 And/g) under the same conditions, the removal effect of the rhodamine B dye is 5.5 times higher than that of a PVC pyrolysis product on 100mL of 5mg/L rhodamine b dye.
Example 2
A method for preparing hollow carbon nano-cakes by utilizing micro-plastic coagulated flocs in water comprises the following steps:
s1, obtaining the water body by calculating the mass of the water body (calculated by the water density of 1 kg/L): the coagulant aid nanometer micro-electrolysis material has the following quality: and (3) the mass of ferric sulfate: sodium polyacrylate mass 1,000,000: 200: 10: coagulating a water body containing 100 mu m of simulated polyvinyl chloride micro-plastic in a proportion of 50 to obtain micro-plastic coagulated flocs;
s2, putting the obtained micro plastic coagulated flocs into a GSL-1600X tube furnace by adopting a zirconia ceramic crucible for pyrolysis; during pyrolysis, the tube furnace (GSL-1600X) was ramped up to 700 ℃ at a rate of 10 ℃/min and pyrolyzed at constant temperature for 4h using N 2 As a shielding gas;
and S3, cooling the tube furnace to room temperature, grinding and crushing the sample cooled to room temperature 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 content of iron atoms is 25-50%; and the specific surface area of the prepared hollow carbon nano-cake HCNC is (64.11 m) 2 /g) is much greater than POf VC pyrolysis product (1.53 m) 2 And/g) under the same conditions, the removal effect of the rhodamine B dye is 5.8 times higher than that of a PVC pyrolysis product on 100mL of 5mg/L rhodamine b dye.
Example 3
A method for preparing hollow carbon nano-cakes by utilizing water body micro-plastic coagulated flocs comprises the following steps:
s1, obtaining the water body by calculating the mass of the water body (calculated by the water density of 1 kg/L): the coagulant aid nanometer micro-electrolysis material has the following quality: the mass of the polyaluminium sulfate is as follows: calcium polyacrylate mass 1,000,000: 10: 1: 5, coagulating the water body containing the simulated polyvinyl chloride micro-plastics with the particle size of 100 mu m to obtain micro-plastic coagulated flocs;
s2, putting the obtained floc into a GSL-1600X tubular furnace by adopting a zirconia ceramic crucible for pyrolysis; in the pyrolysis process, the temperature of a tube furnace (GSL-1600X) is increased to 600 ℃ at the speed of 15 ℃/min, and the tube furnace is pyrolyzed for 2h at constant temperature, and argon is used as protective gas;
and S3, cooling the tube furnace to room temperature, grinding and crushing the sample cooled to room temperature 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 content of iron atoms is 25-60%; and the specific surface area (59.37 m) of the hollow carbon nano-cake HCNC obtained by preparation 2 Perg) much greater than that of PVC pyrolysis product (1.53 m) 2 And/g) under the same conditions, the removal effect of the rhodamine B dye is 5.6 times higher than that of a PVC pyrolysis product on 100mL of 5mg/L rhodamine b dye.
Comparative example 1
A method for preparing hollow carbon nano-cakes by utilizing water body micro-plastic coagulated flocs comprises the following steps:
s1, obtaining the water body by calculating the mass of the water body (calculated by the water density of 1 kg/L): the coagulant aid nanometer micro-electrolysis material has the following quality: the mass of the polymeric ferric sulfate PS is as follows: polyacrylamide PAM mass 1,000,000: 50: 5: 2, coagulating a simulated polyvinyl chloride micro-plastic water body containing 100 mu m of polyvinyl chloride according to the mass ratio to obtain a micro-plastic coagulated floc; the rest is the same as example 1.
Hollow carbon nano-cakes could not be prepared.
Comparative example 2
A method for preparing hollow carbon nano-cakes by utilizing water body micro-plastic coagulated flocs comprises the following steps:
s1, obtaining the water body by calculating the mass of the water body (calculated by the water density of 1 kg/L): the coagulant aid nanometer micro-electrolysis material has the following quality: the mass of the polymeric ferric sulfate PS is as follows: polyacrylamide PAM mass 1,000,000: 50: 5: 70, coagulating a simulated polyvinyl chloride micro-plastic water body with the particle size of 100 mu m to obtain micro-plastic coagulated flocs; the rest is the same as example 1.
Hollow carbon nano-cakes could not be prepared.
Comparative example 3
The preparation method of the PVC pyrolysis product comprises the following steps: putting PVC micro plastic into a GSL-1600X tube furnace by adopting a zirconia ceramic crucible for pyrolysis; during pyrolysis, the tube furnace (GSL-1600X) was ramped up to 800 ℃ at a rate of 10 ℃/min and pyrolyzed at constant temperature for 4h using N 2 As a shielding gas;
after the tube furnace is cooled to the room temperature, the sample cooled to the room temperature is ground and crushed, and the obtained PVC pyrolysis product cannot have a hollow carbon nano cake structure (as shown in figure 3), and the specific surface area is only 1.53m 2 The removal effect of the rhodamine B dye on 100mL of 5mg/L under the same condition is 13.1 percent.
The foregoing is a more detailed description of the invention in connection with specific/preferred embodiments and is not intended to limit the practice of the invention to those descriptions. It will be apparent to those skilled in the art that various substitutions and modifications can be made to the described embodiments without departing from the spirit of the invention, and these substitutions and modifications should be considered to fall within the scope of the invention. In the description herein, references to the description of the term "one embodiment," "some embodiments," "preferred embodiments," "an example," "a specific example," or "some examples" or the like are intended to mean 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, the schematic representations of the terms used above are not necessarily intended to refer 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. Various embodiments or examples and features of various embodiments or examples described in this specification can be combined and combined by one skilled in the art 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 claims.
Claims (9)
1. A method for preparing hollow carbon nano-cakes by utilizing water body micro-plastic coagulated flocs is characterized by comprising the following steps:
s1, by mixing the water body (calculated by the water density of 1 kg/L): coagulant aid: inorganic coagulant: the organic flocculant is prepared from the following components in a mass ratio of 1,000,000: (10-200): (1-10): (5-50) coagulating the water body containing the micro-plastics to obtain micro-plastic coagulated flocs;
s2, putting the obtained micro plastic coagulated flocs into a tubular furnace by adopting a ceramic crucible for pyrolysis, raising the temperature to a target temperature at a specific heating speed, pyrolyzing for a certain time at a constant temperature, and using inert gas as protective gas;
and S3, cooling the tube furnace to room temperature, grinding and crushing the sample cooled to room temperature to obtain the hollow carbon nano-cake HCNC.
2. The method for preparing hollow carbon nano-cake by using water body micro-plastic coagulated flocs according to claim 1, wherein in step S1, the coagulant aid is a nano micro-electrolysis material, and the specific preparation method is described in Chinese patent No. CN201710247676.4, and the method for preparing the nano micro-electrolysis material for removing tetracycline pollutants.
3. The method for preparing hollow carbon nano-cake from the micro plastic coagulated flocs in water according to claim 1, wherein in step S1, the inorganic coagulant is at least one selected from the group consisting of polymeric ferric sulfate PS, polymeric ferric chloride, polymeric aluminum sulfate, aluminum chloride, ferric sulfate, ferric chloride and alum.
4. The method for preparing hollow carbon nano-cake from water body micro plastic coagulated flocs according to claim 1, wherein in step S1, 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.
5. The method for preparing hollow carbon nano-cake by using water body micro-plastic coagulated flocs according to claim 1, wherein in step S2, the specific heating speed is 5-15 ℃; the target temperature is 500-900 ℃; the pyrolysis is carried out for a certain time of 0.5 h-4 h.
6. The method for preparing hollow carbon nano-cakes according to claim 1, wherein in the step S2, the inert atmosphere is at least one of nitrogen, argon, helium or carbon dioxide.
7. The method for preparing hollow carbon nano-cakes through water body micro-plastic coagulated flocs according to claim 1, wherein in step S3, the hollow carbon nano-cake HCNC is a carbon nano-cake containing iron element, the diameter is 200-500 nm, the thickness is 20-100 nm, and the content of iron atom is 20-50%.
8. A hollow carbon nanocake, characterized in that it is obtained by the method according to any one of claims 1 to 7.
9. The application of the hollow carbon nano cake prepared by the method of any one of claims 1 to 7 in a super capacitor, an adsorbent, a catalyst or a lithium ion battery.
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