CN113617337A - Preparation method and application of adsorbent based on garden waste - Google Patents

Preparation method and application of adsorbent based on garden waste Download PDF

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Publication number
CN113617337A
CN113617337A CN202110981715.XA CN202110981715A CN113617337A CN 113617337 A CN113617337 A CN 113617337A CN 202110981715 A CN202110981715 A CN 202110981715A CN 113617337 A CN113617337 A CN 113617337A
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garden waste
composite material
garden
based adsorbent
adsorbent
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朱琨
周璐
李诗佳
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Qiqihar University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/06Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Hydrology & Water Resources (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Water Treatment By Sorption (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

A preparation method and application of an adsorbent based on garden waste aims to solve the problem that the existing charcoal-based adsorbent is poor in removing effect of organic pollutants and heavy metals in water. The preparation method comprises the following steps: firstly, carrying out ultrasonic cleaning and drying on garden waste; secondly, immersing garden wastes into zinc acetate seed liquid for soaking treatment, and introducing nitrogen to keep anaerobic condition for firing; thirdly, immersing the zinc seed layer/biochar composite material into a growth solution for reaction to obtain a ZnO/biochar composite material; and fourthly, adding the graphene oxide and ZnO/biochar composite material into the chitosan solution, adding a coagulant, standing, and then carrying out vacuum freeze drying. The garden waste-based adsorbent can treat various organic pollutants and heavy metal pollutants, the degradation rate of organic pollutants bisphenol A or nitrophenol can reach 60-75%, and the removal rate of lead or cadmium is 60-72%.

Description

Preparation method and application of adsorbent based on garden waste
Technical Field
The invention relates to a preparation method of a composite adsorbent and application of the composite adsorbent in water treatment.
Background
About 300-400 million tons of heavy metals and organic pollutants are released into global water bodies every year in industrial activities, so that the environment of the water bodies is seriously damaged, and meanwhile, the serious threat to human beings is also caused through a food chain. The discharge of industrial three wastes causes the excessive accumulation of heavy metals in soil and water around a mining area, and heavy metals in the soil can finally enter surface water or underground water after being leached and washed by rainwater, so that the water body is polluted by the heavy metals.
There are many treatment methods for water bodies polluted by heavy metals and/or organic pollutants, such as adsorption, biological, electrochemical, advanced oxidation, and photocatalytic methods. The adsorption method is characterized in that a porous solid adsorbent is used for adsorbing pollutants in water, and the adsorption method has the characteristics of diversity, high efficiency, easiness in treatment, reusability and the like. Biochar mainly refers to a product obtained by pyrolyzing biomass such as wood, crop waste, plant tissues and the like under an anoxic condition. Biochar has become one of the most important substances for purifying water sources, improving soil and adsorbing heavy metals at present.
The photocatalytic method means that pollutants are decomposed by a catalyst under the irradiation of light. The photocatalysis reaction has the outstanding advantages of mild condition, low energy consumption, capability of mineralizing most organic matters, reduction of secondary pollution, utilization of sunlight as a light source and the like, so that the photocatalysis reaction has incomparable advantages in organic pollutant treatment compared with other traditional technologies.
Because different organic pollutant treatment methods have respective advantages and disadvantages, in the practical application process, a single treatment method is often difficult to meet the practical requirements. Therefore, two or more methods and technologies are selected to be combined for use, respective advantages are exerted, even synergistic effect is generated among different methods, certain adverse factors can be avoided, and the efficiency and the effect of organic pollutant treatment are greatly improved. The existing solid adsorbent is difficult to simultaneously achieve a good removal effect on organic pollutants and heavy metals in a water body.
Disclosure of Invention
The invention provides a preparation method and application of an adsorbent based on garden waste, aiming at solving the problem that the existing charcoal-based adsorbent has poor removal effect on organic pollutants and heavy metals in water.
The preparation method of the adsorbent based on garden waste is realized according to the following steps:
firstly, carrying out ultrasonic cleaning and drying on garden waste to obtain dried garden waste;
adding zinc acetate into absolute ethyl alcohol to obtain zinc acetate seed liquid, soaking garden waste in the zinc acetate seed liquid, taking out and drying the garden waste, putting the garden waste into a vacuum tube furnace, and introducing nitrogen to keep oxygen-free (limited) condition for firing to obtain a zinc seed layer/biochar composite material;
thirdly, soaking the zinc seed layer/biochar composite material into growth liquid at the temperature of 70-85 ℃ for reaction for 3-4 hours, and drying to obtain the ZnO/biochar composite material;
adding a graphene oxide and ZnO/biochar composite material into the chitosan solution, adding a coagulant, standing at room temperature, washing with distilled water, and then performing vacuum freeze drying to obtain the garden waste-based adsorbent;
wherein the growth liquid in the third step is an aqueous solution containing zinc salt and HMT (hexamethylenetetramine).
The invention applies the adsorbent based on garden waste as the adsorbent in water treatment under the photocatalysis condition.
The chitosan/biochar composite material is obtained by the garden waste-based adsorbent preparation method, and meanwhile, ZnO photocatalysis materials are loaded on the surface of the biochar. Firstly, preparing a zinc seed layer on the surface of garden waste, firing to obtain a biochar material, then soaking biochar in a growth solution for reaction to grow ZnO on the surface of the biochar, and finally compounding the biochar with chitosan to form an adsorbent.
Under the irradiation of ultraviolet light, electrons in a ZnO valence band are excited to jump to a conduction band, correspondingly, holes are formed on the valence band, and the formed electron-hole pairs and dissolved oxygen and H existing in the environment2O reacts to generate hydroxyl radicals with high chemical activity. The generated hydroxyl free radicals and organic pollutants or inorganic pollutants are subjected to oxidation-reduction reaction, so that the pollutants are degraded. According to the invention, the ZnO and charcoal composite interface and the chitosan aerogel doped with graphene oxide are beneficial to conducting electrons, can reduce the recombination of photo-generated electron hole pairs, and improve the photocatalytic water treatment performance. Meanwhile, the chitosan is compounded with the biochar, the chitosan has good biodegradability, the surface of the chitosan contains a large number of active groups such as amino, hydroxyl and the like, the surface of the biochar contains rich oxygen-containing functional groups such as hydroxyl, carboxyl, phenolic hydroxyl and the like, and the active groups on the surfaces of the chitosan and the biochar can be complexed with heavy metal ions to generate adsorption. And the active groups on the surfaces of the chitosan and the biochar can also improve the stability (half-life) of high chemical active free radicals generated by photocatalysis.
The invention can treat various organic pollutants and heavy metal pollutants based on the characteristics of an adsorbent synergistic adsorption method and a photocatalysis method of garden wastes, the degradation rate of bisphenol A or nitrophenol of the organic pollutants can reach 60-75%, and the removal rate of lead or cadmium is 60-72%.
Drawings
FIG. 1 is an XRD pattern of a zinc oxide/biochar composite obtained in an example;
fig. 2 is a graph illustrating the degradation rate of organic pollutants by the garden waste based adsorbent obtained in the first example, wherein a represents bisphenol a and b represents nitrophenol;
fig. 3 is a graph illustrating the degradation rate of heavy metal pollutants by the garden waste-based adsorbent according to example two, in which a represents cadmium and b represents lead.
Detailed Description
The first embodiment is as follows: the preparation method of the adsorbent based on garden waste is implemented according to the following steps:
firstly, carrying out ultrasonic cleaning and drying on garden waste to obtain dried garden waste;
adding zinc acetate into absolute ethyl alcohol to obtain zinc acetate seed liquid, soaking garden waste in the zinc acetate seed liquid, taking out and drying the garden waste, putting the garden waste into a vacuum tube furnace, and introducing nitrogen to keep oxygen-free (limited) condition for firing to obtain a zinc seed layer/biochar composite material;
thirdly, soaking the zinc seed layer/biochar composite material into growth liquid at the temperature of 70-85 ℃ for reaction for 3-4 hours, and drying to obtain the ZnO/biochar composite material;
adding a graphene oxide and ZnO/biochar composite material into the chitosan solution, adding a coagulant, standing at room temperature, washing with distilled water, and then performing vacuum freeze drying to obtain the garden waste-based adsorbent;
wherein the growth liquid in the third step is an aqueous solution containing zinc salt and HMT (hexamethylenetetramine).
The second embodiment is as follows: the difference between the first embodiment and the second embodiment is that the garden waste in the first step is garden fallen leaves or branches.
The third concrete implementation mode: the difference between the first embodiment and the second embodiment is that the concentration of the zinc acetate seed liquid in the second step is 0.1-0.3 mol/L.
The fourth concrete implementation mode: the second embodiment is different from the first to the third embodiments in that the second step is fired at 500 to 700 ℃ for 1 to 2.5 hours under oxygen-free conditions.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is that the drying is performed at a temperature of 100 ℃ to 150 ℃ in the third step.
The sixth specific implementation mode: the difference between the embodiment and one of the first to fifth embodiments is that the concentration of the zinc salt in the growth liquid in the third step is 0.01 mol/L-0.015 mol/L, and the concentration of the HMT is 0.01 mol/L-0.015 mol/L.
In the embodiment, the ZnO crystal grows along the <0001> crystal face by controlling the component proportion of the zinc salt and the HMT in the growth liquid.
The seventh embodiment: the difference between the embodiment and one of the first to sixth embodiments is that the mass ratio of the graphene oxide to the ZnO/biochar composite in the fourth step is 1: (1-3).
The specific implementation mode is eight: this embodiment differs from the first to seventh embodiments in that the coagulant in step four is a 2mol/L NaOH solution.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is that the standing treatment time in the fourth step is 20 to 30 hours.
The detailed implementation mode is ten: the difference between this embodiment and one of the first to ninth embodiments is that the freeze-drying in the fourth step is carried out at-40 to-60 ℃ for 24 to 36 hours.
The first embodiment is as follows: the preparation method of the adsorbent based on the garden waste is implemented according to the following steps:
firstly, carrying out ultrasonic cleaning and drying on garden waste, and crushing to obtain cleaned garden waste (fiber);
adding zinc acetate into absolute ethyl alcohol to obtain 0.2mol/L zinc acetate seed liquid, soaking garden waste into the zinc acetate seed liquid, taking out and drying the garden waste, putting the garden waste into a vacuum tube furnace, introducing nitrogen to maintain an anaerobic condition, and firing the garden waste for 1.5 hours at 500 ℃ to obtain a zinc seed layer/biochar composite material;
thirdly, soaking the zinc seed layer/biochar composite material into growth solution at the temperature of 80 ℃ for reaction for 4 hours, and drying to obtain the ZnO/biochar composite material;
adding 2.5g of graphene oxide and 4.0g of ZnO/charcoal composite material into a chitosan solution (containing 3.0g of chitosan), adding 2mol/L of NaOH solution, standing at room temperature for 24 hours, washing with distilled water, and then carrying out vacuum freeze drying for 28 hours to obtain the garden waste-based adsorbent;
wherein the growth solution in the third step is an aqueous solution containing 0.012mol/L zinc salt and 0.012mol/L HMT.
The garden waste-based adsorbent prepared in the embodiment is a chitosan/biochar composite material, and the specific surface area of the chitosan/biochar composite material is 53.216m2/g。
Photocatalytic degradation experiment:
the formula for calculating the degradation rate is: percent degradation rate (%) ═ C/C 0100 of formula C0Represents the initial concentration of the organic contaminant; c represents the concentration of organic contaminants during the irradiation reaction phase.
Preparing 100mL of bisphenol A solution with the concentration of 2mg/L, adding 20mg of the chitosan/charcoal composite adsorbent prepared in the first embodiment, turning on an ultraviolet light source, and irradiating for 100min until the maximum removal rate of bisphenol A reaches 64.2%.
Preparing 100mL of nitrophenol solution with the concentration of 2mg/L, adding 20mg of the chitosan/charcoal composite adsorbent prepared in the first embodiment, turning on an ultraviolet light source, and irradiating for 100min to ensure that the maximum removal rate of the nitrophenol reaches 75.6 percent.
Example two: the preparation method of the adsorbent based on the garden waste is implemented according to the following steps:
firstly, carrying out ultrasonic cleaning and drying on garden waste to obtain cleaned garden waste (fiber);
adding zinc acetate into absolute ethyl alcohol to obtain 0.2mol/L zinc acetate seed liquid, soaking garden waste into the zinc acetate seed liquid, taking out and drying the garden waste, putting the garden waste into a vacuum tube furnace, introducing nitrogen, keeping an anaerobic condition, and firing the garden waste for 2 hours at 600 ℃ to obtain a zinc seed layer/biochar composite material;
thirdly, soaking the zinc seed layer/biochar composite material into growth solution at the temperature of 85 ℃ for reaction for 4 hours, and drying to obtain the ZnO/biochar composite material;
adding 1.5g of graphene oxide and 4.0g of ZnO/charcoal composite material into a chitosan solution (containing 4.0g of chitosan), adding 2mol/L of NaOH solution, standing at room temperature for 24 hours, washing with distilled water, and then carrying out vacuum freeze drying for 28 hours to obtain the garden waste-based adsorbent;
wherein the growth solution in the third step is an aqueous solution containing 0.01mol/L zinc salt and 0.01mol/L HMT.
Photocatalytic degradation experiment:
the initial concentration of lead in 100mL of water to be treated was measured to be 10mg/L, and the pH of the water to be treated was measured to be 5, and 80mg of the chitosan/biochar composite adsorbent prepared in example two was added to the water to be treated. And (3) turning on an ultraviolet light source, and when the irradiation is carried out for 100min, the maximum removal rate of the divalent lead reaches 72.5%.
The initial concentration of cadmium in 100mL of water to be treated was measured to be 10mg/L, and the pH of the water to be treated was measured to be 4, and 80mg of the chitosan/biochar composite adsorbent prepared in example two was added to the water to be treated. And (3) turning on an ultraviolet light source, and when the ultraviolet light source is irradiated for 100min, the maximum removal rate of cadmium reaches 60.1%.

Claims (10)

1. The preparation method of the adsorbent based on the garden waste is characterized by comprising the following steps:
firstly, carrying out ultrasonic cleaning and drying on garden waste to obtain dried garden waste;
adding zinc acetate into absolute ethyl alcohol to obtain zinc acetate seed liquid, soaking garden waste in the zinc acetate seed liquid, taking out and drying the garden waste, putting the garden waste into a vacuum tube furnace, introducing nitrogen to keep anaerobic conditions, and firing to obtain a zinc seed layer/biochar composite material;
thirdly, soaking the zinc seed layer/biochar composite material into growth liquid at the temperature of 70-85 ℃ for reaction for 3-4 hours, and drying to obtain the ZnO/biochar composite material;
adding a graphene oxide and ZnO/biochar composite material into the chitosan solution, adding a coagulant, standing at room temperature, washing with distilled water, and then performing vacuum freeze drying to obtain the garden waste-based adsorbent;
wherein the growth solution in the third step is an aqueous solution containing zinc salt and HMT.
2. The method for preparing the garden waste-based adsorbent according to claim 1, wherein the garden waste in the first step is garden fallen leaves or branches.
3. The preparation method of the garden waste-based adsorbent according to claim 1, wherein the concentration of the zinc acetate seed liquid in the second step is 0.1-0.3 mol/L.
4. The method for preparing the garden waste-based adsorbent according to claim 1, wherein the second step is firing at 500-700 ℃ for 1-2.5 h in the absence of oxygen.
5. The method for preparing the garden waste-based adsorbent according to claim 1, wherein the concentration of the zinc salt in the growth solution in the third step is 0.01-0.015 mol/L, and the concentration of the HMT is 0.01-0.015 mol/L.
6. The preparation method of the garden waste-based adsorbent according to claim 1, wherein the mass ratio of the graphene oxide to the ZnO/biochar composite in the fourth step is 1: (1-3).
7. The method for preparing an adsorbent based on garden waste according to claim 1, wherein the coagulant in the fourth step is 2mol/L NaOH solution.
8. The method for preparing the garden waste-based adsorbent according to claim 1, wherein the standing treatment time in the fourth step is 20 to 30 hours.
9. The method for preparing the garden waste-based adsorbent according to claim 1, wherein the freeze-drying in the fourth step is performed at-40 to-60 ℃ for 24 to 36 hours.
10. The application of the garden waste-based adsorbent is characterized in that the garden waste-based adsorbent is applied to water treatment as an adsorbent under a photocatalytic condition.
CN202110981715.XA 2021-08-25 2021-08-25 Preparation method and application of adsorbent based on garden waste Withdrawn CN113617337A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
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Application publication date: 20211109