CN112742348A - Waste plastic-based porous activated carbon composite material, preparation method thereof and application thereof in purification of VOCs (volatile organic compounds) - Google Patents
Waste plastic-based porous activated carbon composite material, preparation method thereof and application thereof in purification of VOCs (volatile organic compounds) Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 211
- 239000004033 plastic Substances 0.000 title claims abstract description 130
- 229920003023 plastic Polymers 0.000 title claims abstract description 130
- 239000002699 waste material Substances 0.000 title claims abstract description 124
- 239000002131 composite material Substances 0.000 title claims abstract description 111
- 239000012855 volatile organic compound Substances 0.000 title claims abstract description 32
- 238000000746 purification Methods 0.000 title claims abstract description 7
- 238000002360 preparation method Methods 0.000 title abstract description 14
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 20
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 16
- 238000001354 calcination Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 8
- 150000001621 bismuth Chemical class 0.000 claims description 5
- 150000001879 copper Chemical class 0.000 claims description 5
- 150000002751 molybdenum Chemical class 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000010815 organic waste Substances 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 45
- 239000002351 wastewater Substances 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 4
- 239000002910 solid waste Substances 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 30
- 239000007789 gas Substances 0.000 description 17
- 239000003463 adsorbent Substances 0.000 description 15
- 238000012360 testing method Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 10
- 239000012299 nitrogen atmosphere Substances 0.000 description 7
- 239000000571 coke Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical group [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 5
- 229940010552 ammonium molybdate Drugs 0.000 description 5
- 235000018660 ammonium molybdate Nutrition 0.000 description 5
- 239000011609 ammonium molybdate Substances 0.000 description 5
- 239000003575 carbonaceous material Substances 0.000 description 5
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical group [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 5
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical group Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 239000002912 waste gas Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000011067 equilibration Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N CuO Inorganic materials [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/027—Compounds of F, Cl, Br, I
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- B01J20/28019—Spherical, ellipsoidal or cylindrical
-
- 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
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
-
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/102—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
Abstract
The invention discloses a waste plastic-based porous activated carbon composite material, a preparation method thereof and application thereof in purifying VOCs (volatile organic compounds)3CuO and Bi2O3. According to the inventionThe waste plastic-based porous activated carbon composite material has good adsorption and purification effects on organic wastewater and VOCs, can be widely applied to the field of environmental protection, and is favorable for realizing recycling of solid waste of waste plastic solid waste.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a waste plastic-based porous activated carbon composite material and a preparation method and application thereof.
Background
The plastic product has the advantages of light weight, water resistance, durability, mature production technology and low cost, and is widely applied. In 1995, the yield of plastics in China is 519 ten thousand tons, the quantity of imported plastics is nearly 600 ten thousand tons, and the total consumption quantity of plastics in China is about 1100 ten thousand tons in the current year, wherein the quantity of plastics for packaging reaches 211 ten thousand tons. Most of the waste plastic products are in the form of waste films, plastic bags and foamed plastic tableware, and are discarded in the environment, so that the landscape is influenced, and the waste plastic products are difficult to degrade and cause potential harm to the ecological environment. Therefore, how to realize resource recycling of waste plastics is a problem to be solved at present.
The carbon material has the advantages of controllable structure, high specific surface area, low density, high mechanical stability, high thermal conductivity, easy large-scale production and the like, and is widely concerned by people. At present, one of the methods for harmlessly recycling waste plastics is to prepare carbon materials, and the prepared waste plastic-based carbon materials can be used for purifying organic wastewater such as printing and dyeing wastewater and Volatile Organic Compounds (VOCs). However, the single waste plastic-based carbon material has insufficient adsorption performance, and the use effect of the carbon material is limited.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a waste plastic-based porous activated carbon composite material, a preparation method thereof and application thereof in VOCs purification.
The invention provides a waste plastic-based porous activated carbon composite material which comprises the components of waste plastic-based porous activated carbon and MoO loaded on the waste plastic-based porous activated carbon3CuO and Bi2O3。
Preferably, the mass of the waste plastic-based porous activated carbon accounts for 60-80% of the total mass of the material; preferably, the mass of the waste plastic-based porous activated carbon accounts for 70% of the total mass of the material.
Preferably, the MoO3、CuO、Bi2O3In a molar ratio of (1-2): (1-2): (1-2); preferably, the MoO3、CuO、Bi2O3In a molar ratio of 1:1: 2.
Preferably, the mesh number of the waste plastic-based porous activated carbon is 48-800 meshes, and the specific surface area is 10-1000m2Per g, an average pore diameter of 20-300 μm, and a density of 0.35-0.56g/cm3The purity is more than or equal to 98 percent.
The waste plastic-based porous activated carbon can be prepared by a conventional method, and for example, may be:
(1) crushing and sieving the waste plastic to obtain waste plastic powder;
(2) deoiling the waste plastic powder, washing for 3-5 times by using hydrochloric acid, sulfuric acid or nitric acid with the concentration of 1-5mol/L to dissolve and remove powder attachments, and adjusting the pH value to 7-8.5 by using alkali liquor;
(3) and under the protection of inert atmosphere, heating at 600 ℃ for 3h, and then carrying out flotation, washing and drying to obtain the waste plastic-based porous activated carbon.
The preparation method of the waste plastic-based porous activated carbon composite material comprises the following steps:
s1, dissolving molybdenum salt, copper salt and bismuth salt in a dilute nitric acid solution, and then adding waste plastic-based porous activated carbon and uniformly stirring to obtain a mixed solution;
s2, adjusting the pH value of the mixed solution to 7-13, and uniformly stirring to obtain composite gel;
s3, performing microwave treatment on the composite gel to obtain composite powder;
and S4, drying the composite powder, and calcining in an inert atmosphere to obtain the waste plastic-based porous activated carbon composite material.
Preferably, in the step S3, the microwave treatment condition is 800-; preferably, the microwave treatment is performed under 1000W for 30 min.
Preferably, in the step S4, the drying condition is 100-120 ℃ for 0.5-1.5h, and the calcining condition is 350-450 ℃ for 1-6 h; preferably, the drying conditions are 110 ℃ for 1h, and the calcining conditions are 400 ℃ for 3 h.
Preferably, in the step S1, the concentration of the dilute nitric acid solution is 0.1-0.2 mol/L.
Preferably, in the mixed solution, the concentration of the molybdenum salt is 0.1-0.5mol/L, the concentration of the copper salt is 0.05-0.5mol/L, and the concentration of the bismuth salt is 0.05-0.25 mol/L.
Preferably, the molybdenum salt is ammonium molybdate, the copper salt is copper nitrate, and the bismuth salt is bismuth nitrate.
The application of the waste plastic-based porous activated carbon composite material in organic wastewater treatment.
The application of the waste plastic-based porous activated carbon composite material in VOCs purification.
The invention has the following beneficial effects:
the MoO is prepared by a microwave calcination reaction method3-CuO-Bi2O3Modified waste plastic based porous active carbon composite material has a mixed structure of spherical shape and flaky shape, the microstructure presents multistage and multiscale, and the modified waste plastic based porous active carbon composite material has good adsorption and purification effects on organic wastewater and VOCs (volatile organic compounds), has high adsorption quantity and high adsorption speed, can be widely applied to the field of environmental protection, and is favorable for realizing the realization of the environment-friendly effectRecycling and reusing the solid waste of the waste plastic solid waste.
Drawings
Fig. 1 is an XRD image of the waste plastic-based porous activated carbon composite material of the present invention.
Fig. 2 is an SEM image of the waste plastic-based porous activated carbon composite material of the present invention.
FIG. 3 shows the adsorption removal rate of the waste plastic-based porous activated carbon composite material on phenol in organic wastewater.
FIG. 4 shows the adsorption amount of phenol in organic wastewater by the waste plastic-based porous activated carbon composite material of the present invention.
FIGS. 5-8 are graphs of breakthrough data for adsorption of VOCs by the waste plastic-based porous activated carbon composite material of the present invention.
FIG. 9 is a schematic diagram of an apparatus for testing adsorption of VOCs.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
In the following examples and comparative examples, the used waste plastic-based porous activated carbon had a mesh number of 48 to 800 mesh and a specific surface area of 10 to 1000m2Per g, an average pore diameter of 20-300 μm, and a density of 0.35-0.56g/cm3The purity is more than or equal to 98 percent.
Example 1
The composition of the composite material comprises the waste plastic-based porous activated carbon and MoO loaded on the waste plastic-based porous activated carbon3CuO and Bi2O3(ii) a Wherein the mass of the waste plastic based porous activated carbon accounts for 60-80% of the total mass of the material, and MoO3、CuO、Bi2O3In a molar ratio of (1-2): (1-2): (1-2).
The preparation method of the waste plastic-based porous activated carbon composite material comprises the following steps:
s1, dissolving molybdenum salt, copper salt and bismuth salt in a dilute nitric acid solution with the concentration of 0.1-0.2mol/L, and then adding waste plastic-based porous activated carbon and stirring uniformly to obtain a mixed solution;
s2, adjusting the pH value of the mixed solution to 7-13, and uniformly stirring to obtain composite gel;
s3, performing microwave treatment on the composite gel for 20-60min under the conditions of 800-1500W to obtain composite powder;
s4, drying the composite powder at the temperature of 100-120 ℃ for 0.5-1.5h, and then calcining the composite powder at the temperature of 350-450 ℃ for 1-6h in an inert atmosphere to obtain the waste plastic-based porous activated carbon composite material.
Example 2
The preparation method of the waste plastic-based porous activated carbon composite material comprises the following steps:
s1, dissolving ammonium molybdate, copper nitrate and bismuth nitrate in a dilute nitric acid solution with the concentration of 0.15mol/L, and then adding waste plastic-based porous activated carbon and uniformly stirring to obtain a mixed solution;
s2, adjusting the pH value of the mixed solution to 7-13, and uniformly stirring to obtain composite gel;
s3, performing microwave treatment on the composite gel for 30min under the condition of 1000W to obtain composite powder;
s4, drying the composite powder at 110 ℃ for 1h, and then calcining the dried composite powder at 400 ℃ for 3h in a nitrogen atmosphere to obtain the waste plastic-based porous activated carbon composite material, wherein the waste plastic-based porous activated carbon composite material comprises the waste plastic-based porous activated carbon and MoO loaded on the waste plastic-based porous activated carbon3CuO and Bi2O3Wherein the mass of the waste plastic-based porous activated carbon accounts for 70 percent of the total mass of the material, and MoO3、CuO、Bi2O3In a molar ratio of (1-2): (1-2): (1-2).
Samples 1-7, MoO in sample 1, were prepared by the method described above3、CuO、Bi2O3In a molar ratio of 1:1: MoO in sample 1, sample 23、CuO、Bi2O3In a molar ratio of 1:1:2, MoO in sample 33、CuO、 Bi2O3In a molar ratio of 1: 2: MoO in sample 4 13、CuO、Bi2O3In a molar ratio of 1: 2: 2, MoO in sample 53、CuO、Bi2O3In a molar ratio of 2: 1: MoO in sample 6 1, sample 63、CuO、Bi2O3In a molar ratio of 2: 1:2, MoO in sample 73、CuO、Bi2O3In a molar ratio of 2: 2: 1.
comparative example 1
The preparation method of the waste plastic-based porous activated carbon composite material comprises the following steps:
s1, dissolving ammonium molybdate in a dilute nitric acid solution with the concentration of 0.15mol/L, and then adding waste plastic-based porous activated carbon and uniformly stirring to obtain a mixed solution;
s2, adjusting the pH value of the mixed solution to 7-13, and uniformly stirring to obtain composite gel;
s3, performing microwave treatment on the composite gel for 30min under the condition of 1000W to obtain composite powder;
s4, drying the composite powder at 110 ℃ for 1h, and then calcining the dried composite powder at 400 ℃ for 3h in a nitrogen atmosphere to obtain the waste plastic-based porous activated carbon composite material, wherein the waste plastic-based porous activated carbon composite material comprises the waste plastic-based porous activated carbon and MoO loaded on the waste plastic-based porous activated carbon3Wherein the mass of the waste plastic-based porous activated carbon accounts for 70 percent of the total mass of the material.
Comparative example 2
The preparation method of the waste plastic-based porous activated carbon composite material comprises the following steps:
s1, dissolving copper nitrate in a dilute nitric acid solution with the concentration of 0.15mol/L, and then adding waste plastic-based porous activated carbon and uniformly stirring to obtain a mixed solution;
s2, adjusting the pH value of the mixed solution to 7-13, and uniformly stirring to obtain composite gel;
s3, performing microwave treatment on the composite gel for 30min under the condition of 1000W to obtain composite powder;
s4, drying the composite powder at 110 ℃ for 1h, and calcining the dried composite powder at 400 ℃ for 3h in a nitrogen atmosphere to obtain the waste plastic-based porous activated carbon composite material, wherein the waste plastic-based porous activated carbon composite material comprises the waste plastic-based porous activated carbon and CuO loaded on the waste plastic-based porous activated carbon, and the mass of the waste plastic-based porous activated carbon accounts for 70% of the total mass of the material.
Comparative example 3
The preparation method of the waste plastic-based porous activated carbon composite material comprises the following steps:
s1, dissolving bismuth nitrate in a dilute nitric acid solution with the concentration of 0.15mol/L, and then adding waste plastic-based porous activated carbon and uniformly stirring to obtain a mixed solution;
s2, adjusting the pH value of the mixed solution to 7-13, and uniformly stirring to obtain composite gel;
s3, performing microwave treatment on the composite gel for 30min under the condition of 1000W to obtain composite powder;
s4, drying the composite powder at 110 ℃ for 1h, and calcining the dried composite powder at 400 ℃ for 3h in a nitrogen atmosphere to obtain the waste plastic-based porous activated carbon composite material, wherein the waste plastic-based porous activated carbon composite material comprises the components of waste plastic-based porous activated carbon and Bi loaded on the waste plastic-based porous activated carbon2O3Wherein the mass of the waste plastic-based porous activated carbon accounts for 70 percent of the total mass of the material.
Comparative example 4
The preparation method of the waste plastic-based porous activated carbon composite material comprises the following steps:
s1, dissolving ammonium molybdate and copper nitrate in a dilute nitric acid solution with the concentration of 0.15mol/L, and then adding waste plastic-based porous activated carbon and uniformly stirring to obtain a mixed solution;
s2, adjusting the pH value of the mixed solution to 7-13, and uniformly stirring to obtain composite gel;
s3, performing microwave treatment on the composite gel for 30min under the condition of 1000W to obtain composite powder;
s4, drying the composite powder at 110 ℃ for 1h, and then calcining the dried composite powder at 400 ℃ for 3h in a nitrogen atmosphere to obtain the waste plastic-based porous activated carbon composite material, wherein the waste plastic-based porous activated carbon composite material comprises the waste plastic-based porous activated carbon and the waste plastic-based porous activated carbon loaded on the waste plastic-based porous activated carbonOf MoO3And CuO, wherein the mass of the waste plastic-based porous activated carbon accounts for 70 percent of the total mass of the material, and MoO3The molar ratio of CuO is 1: 1.
comparative example 5
The preparation method of the waste plastic-based porous activated carbon composite material comprises the following steps:
s1, dissolving ammonium molybdate and bismuth nitrate in a dilute nitric acid solution with the concentration of 0.15mol/L, and then adding waste plastic-based porous activated carbon and uniformly stirring to obtain a mixed solution;
s2, adjusting the pH value of the mixed solution to 7-13, and uniformly stirring to obtain composite gel;
s3, performing microwave treatment on the composite gel for 30min under the condition of 1000W to obtain composite powder;
s4, drying the composite powder at 110 ℃ for 1h, and then calcining the dried composite powder at 400 ℃ for 3h in a nitrogen atmosphere to obtain the waste plastic-based porous activated carbon composite material, wherein the waste plastic-based porous activated carbon composite material comprises the waste plastic-based porous activated carbon and MoO loaded on the waste plastic-based porous activated carbon3And Bi2O3Wherein the mass of the waste plastic-based porous activated carbon accounts for 70 percent of the total mass of the material, and MoO3、 Bi2O3In a molar ratio of 1: 2.
comparative example 6
The preparation method of the waste plastic-based porous activated carbon composite material comprises the following steps:
s1, dissolving copper nitrate and bismuth nitrate in a dilute nitric acid solution with the concentration of 0.15mol/L, and then adding waste plastic-based porous activated carbon and uniformly stirring to obtain a mixed solution;
s2, adjusting the pH value of the mixed solution to 7-13, and uniformly stirring to obtain composite gel;
s3, performing microwave treatment on the composite gel for 30min under the condition of 1000W to obtain composite powder;
s4, drying the composite powder at 110 ℃ for 1h, and then calcining the dried composite powder at 400 ℃ for 3h in nitrogen atmosphere to obtain the waste plastic-based porous activated carbon composite materialThe composite material comprises the components of waste plastic-based porous activated carbon and CuO and Bi loaded on the waste plastic-based porous activated carbon2O3Wherein the mass of the waste plastic-based porous activated carbon accounts for 70 percent of the total mass of the material, and CuO and Bi2O3In a molar ratio of 1: 2.
test examples
(1) XRD test
XRD analysis of samples 1-7 prepared in example 2 of the present invention showed in FIG. 1, which shows that the XRD diffraction pattern has significant MoO3,CuO,Bi2O3And all the diffraction peaks are relatively sharp.
(2) SEM characterization
SEM analysis was performed on sample 2 obtained in example 2 of the present invention, and the result is shown in FIG. 2. It can be seen that the material has a mixed structure with a spherical shape and a sheet shape, and the microstructure is in multi-level and multi-scale, and the size range is between 100nm and 10 um.
(3) Adsorption test of phenol in organic wastewater
Samples 1-7 and common waste plastic-based porous activated carbon are respectively adopted as adsorbents, and the adsorbents are used for carrying out adsorption tests on phenol-containing chemical coke sewage solution under the condition of sunlight, so that the phenol removal rate is calculated. The adsorption test conditions were as follows: the dosage of the adsorbent is 50mg, the adsorption time is 60min, the volume of the chemical coke wastewater solution containing phenol is 100mL, the initial concentration is 100mg/L, and the calculation method of the phenol removal rate comprises the following steps: (C)0-Ci)/C0×100%,CiPhenol residual concentration of the adsorbed solution over time i, C0The initial concentration of phenol was the solution. The test results are shown in FIG. 3. As can be seen from figure 3, the waste plastic-based porous activated carbon composite material prepared by the method has a good adsorption removal effect on phenol in organic wastewater, and the removal rate of the phenol is far superior to 58.2% of that of common waste plastic-based porous activated carbon; wherein the removal rate of sample 2 reached 98%.
Respectively adopting samples 1-7 and common waste plastic-based porous activated carbon as adsorbents, and using the adsorbents to adsorb benzene under the condition of sunlightCarrying out an adsorption test on the phenol chemical coke sewage solution, and calculating the phenol adsorption quantity, wherein the calculation method of the phenol adsorption quantity comprises the following steps:the equilibrium adsorption capacity of the organic matters is mg/g; t adsorption time, min; total flow of phenol, mL/min; c0Initial concentration of phenol mg/m3;CiThe residual concentration of phenol after adsorption is mg/m3(ii) a W is the loading g of the adsorbent; t is teAdsorption equilibration time, min.
The dosage of the adsorbent is 60mg, the adsorption time is 60min, the volume of the chemical coke wastewater solution containing phenol is 500mL, and the initial concentration of phenol is 100 mg/L. The test results are shown in FIG. 4. As can be seen from FIG. 4, the adsorption amount of the waste plastic-based porous activated carbon composite material prepared by the invention on phenol in organic wastewater is far greater than that of common waste plastic-based porous activated carbon, and the adsorption speed is high; here, the adsorption amount of sample 2 reached 193 mg/g.
Respectively adopting the waste plastic-based porous activated carbon composite materials prepared in comparative examples 1-6 as adsorbents, carrying out adsorption tests on phenol-containing chemical coke sewage solution by using the adsorbents under the condition of sunlight, and calculating the phenol adsorption capacity, wherein the calculation method of the phenol adsorption capacity comprises the following steps:the equilibrium adsorption capacity of the organic matters is mg/g; t adsorption time, min; total flow of phenol, mL/min; c0Initial concentration of phenol mg/m3;CiThe residual concentration of phenol after adsorption is mg/m3(ii) a W is the loading g of the adsorbent; t is teAdsorption equilibration time, min. The dosage of the adsorbent is 60mg, the adsorption time is 60min, the volume of the chemical coke wastewater solution containing phenol is 500mL, and the initial concentration of phenol is 100 mg/L. The amount of phenol adsorbed was calculated and compared to sample 2 and the results are shown in table 1:
TABLE 1 adsorption of phenol by waste plastic-based porous activated carbon composite
As can be seen from Table 1, the adsorption capacity of the waste plastic-based porous activated carbon composite material prepared by the method is far greater than that of the waste plastic-based porous activated carbon composite materials prepared by comparative examples 1-6.
(4) Adsorption test of VOCs
Adsorption tests were carried out on acetone, styrene, toluene, ethyl acetate with samples 2, 3, 5, 7 and comparative examples 1 to 6 as adsorbents. The VOCs adsorption device uses nitrogen as carrier gas, and is divided into three paths of gas through two three-way pipes, wherein one path of gas is used for dilution; one path is introduced into a VOCs bubbling bottle to carry out VOCs gas with certain concentration; the last path is introduced into a water vapor generation bottle to carry out water vapor with a certain concentration; and finally merging the three paths of gas into one path of gas, uniformly mixing the gas and the one path of gas, and introducing the gas into an adsorption tube for an adsorption experiment. The flow of the three-way gas is adjusted by a mass flow meter, and the simulated gas in the experiment is introduced into a Gas Chromatograph (GC) for analysis. All samples in the experiment need to be pretreated before adsorption. The absorption of VOCs waste gas is closed first way gas, gets into the VOCs generator with second way gas, and last way is as the diluent gas with the air, through adjusting the flowmeter flow, joins in marriage the VOCs waste gas of certain concentration and airspeed, lets in the adsorption tube after waste gas concentration is stable and adsorbs, observes the change of VOCs content in the tail gas, when VOCs concentration no longer changes, considers from this that the absorption has reached the balance. When the adsorption of high-humidity VOCs gas is measured, a third path of water vapor generator is added to prepare gas with certain VOCs concentration, airspeed and relative humidity. The test apparatus is shown in FIG. 9.
The test results are shown in table 2:
TABLE 2 adsorption of VOCs by waste plastic-based porous activated carbon composite
Therefore, the waste plastic-based porous active carbon composite material has larger adsorption capacity to VOCs.
Fig. 5-8 are graphs of penetration data for samples 2, 3, 5, 7, respectively, in example 2 of the present invention. Assuming an outlet concentration of C and an inlet concentration of C0, the adsorbent adsorbs VOCs to reach the breakthrough point when C/C0 is 0.1; when the C/C0 is 0.95, the adsorbent adsorbs VOCs to saturation. Under the assumption condition, the waste plastic-based porous activated carbon composite material disclosed by the invention is used as an adsorbent to adsorb VOCs quickly.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The waste plastic-based porous activated carbon composite material is characterized by comprising the following components of waste plastic-based porous activated carbon and MoO loaded on the waste plastic-based porous activated carbon3CuO and Bi2O3。
2. The waste plastic-based porous activated carbon composite material as described in claim 1, wherein the mass of the waste plastic-based porous activated carbon is 60 to 80% of the total mass of the material; preferably, the mass of the waste plastic-based porous activated carbon accounts for 70% of the total mass of the material.
3. The waste plastic-based porous activated carbon composite as claimed in claim 1, wherein the MoO is3、CuO、Bi2O3In a molar ratio of (1-2): (1-2): (1-2); preferably, the MoO3、CuO、Bi2O3In a molar ratio of 1:1: 2.
4. The waste plastic-based porous activated carbon composite material as claimed in claim 1, wherein the mesh number of the waste plastic-based porous activated carbon is 48 to 800 mesh and the specific surface area is 10 to 1000m2Per g, an average pore diameter of 20-300 μm, and a density of 0.35-0.56g/cm3The purity is more than or equal to 98 percent.
5. A method for preparing a waste plastic-based porous activated carbon composite as described in any one of claims 1 to 4, comprising the steps of:
s1, dissolving molybdenum salt, copper salt and bismuth salt in a dilute nitric acid solution, and then adding waste plastic-based porous activated carbon and uniformly stirring to obtain a mixed solution;
s2, adjusting the pH value of the mixed solution to 7-13, and uniformly stirring to obtain composite gel;
s3, performing microwave treatment on the composite gel to obtain composite powder;
and S4, drying the composite powder, and calcining in an inert atmosphere to obtain the waste plastic-based porous activated carbon composite material.
6. The method for preparing a waste plastic-based porous activated carbon composite material as defined in claim 5, wherein in the step S3, the microwave treatment is performed under the conditions of 800-1500W for 20-60 min; preferably, the microwave treatment is performed under 1000W for 30 min.
7. The method for preparing a waste plastic-based porous activated carbon composite material as claimed in claim 5 or 6, wherein in the step S4, the drying condition is 100-120 ℃ for 0.5-1.5h, and the calcining condition is 350-450 ℃ for 1-6 h; preferably, the drying conditions are 110 ℃ for 1h, and the calcining conditions are 400 ℃ for 3 h.
8. A process for preparing a waste plastic-based porous activated carbon composite as described in any one of claims 5 to 7, wherein said dilute nitric acid solution has a concentration of 0.1 to 0.2mol/L in said step S1.
9. Use of a waste plastic-based porous activated carbon composite as claimed in any one of claims 1 to 4 in the treatment of organic waste water.
10. Use of a waste plastic based porous activated carbon composite as claimed in any one of claims 1 to 4 for the purification of VOCs.
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