CN114773128B - Resource utilization method of waste tail vegetable leaves - Google Patents

Resource utilization method of waste tail vegetable leaves Download PDF

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CN114773128B
CN114773128B CN202210393902.0A CN202210393902A CN114773128B CN 114773128 B CN114773128 B CN 114773128B CN 202210393902 A CN202210393902 A CN 202210393902A CN 114773128 B CN114773128 B CN 114773128B
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waste
biochar
leaves
tail vegetable
mixture
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CN114773128A (en
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齐佳敏
李彬
周鹏翔
宁平
宿新泰
董鹏
王兴源
朱恒希
赵晨竹
仝朝
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Kunming University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D9/00—Other inorganic fertilisers
    • C—CHEMISTRY; METALLURGY
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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    • C01B32/318—Preparation characterised by the starting materials
    • C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
    • 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
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    • C01B32/312—Preparation
    • C01B32/342—Preparation characterised by non-gaseous activating agents
    • C01B32/348—Metallic compounds
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • C05G3/80—Soil conditioners

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Abstract

The invention discloses a recycling method of waste tail vegetable leaves, which comprises the steps of drying, breaking, grinding and sieving the waste tail vegetable leaves to obtain waste tail vegetable leaf powder, adding KOH solution after pre-carbonization, magnetically stirring at constant temperature, standing and centrifuging to obtain potassium humate solution and biochar, mixing the biochar with Fenton sludge and water, magnetically stirring and uniformly mixing the mixture at constant temperature, vacuum drying to constant weight, grinding, sieving and carbonizing, and activating carbonized materials after adding NaOH to obtain an iron-doped biochar electrode material; according to the invention, the complex waste cabbage leaves which are difficult to treat and are easy to generate diseases and insect pests are efficiently and quickly converted into the potassium humate organic fertilizer by a simple carbothermal method, so that the environment-friendly and green resource conversion of the waste cabbage leaves is realized, a new thought is provided for the treatment of Fenton sludge, meanwhile, the biochar generated in the extraction process is prepared into the iron-nitrogen doped biochar electrode material, the purposes of treating waste by waste, changing waste into valuable and comprehensively utilizing the waste are realized, and the method has remarkable economic and environmental values.

Description

Resource utilization method of waste tail vegetable leaves
Technical Field
The invention belongs to the technical field of organic solid waste recycling, and particularly relates to a recycling method of waste tail vegetable leaves.
Background
Organic solid waste is mainly a byproduct of living sources, agricultural sources and industrial sources, and is easy to generate stink and mosquitoes to pollute the land and air in the piling process. The means of landfill, incineration, ocean dumping, composting and the like adopted conventionally not only can cause secondary pollution, but also cause waste of valuable resources in the organic solid waste. The main components of the organic solid waste are organic matters and nutrient substances. The waste tail vegetable leaves are solid wastes with the largest proportion in the organic solid wastes.
Vegetables are one of the indispensable foods in people's daily diet, and can provide nutrients such as various vitamins and minerals necessary for human body. At present, china is the first major country of world vegetable production. According to statistics of the national statistical bureau, the vegetable yield of China reaches 7.4 million tons in 2020, and the trend of year-by-year growth is presented. The Yunnan is an important vegetable production main production area in China, the vegetable types are rich, the main vegetable types in China are basically covered, the production scale is large, the production scale reaches 2507.89 ten thousand tons in 2020, and the vegetable type is the third major agriculture leading industry in Yunnan province.
The quality and quality of the vegetables and the leaves, roots, stems, fruits and the like produced in the processing treatment and the market can be finally solid waste, so that the resource waste and the environmental pollution are caused. The waste tail vegetable leaves are generally short in storage period, not easy to transport and perishable, and the production peak period is generally in a high-temperature season. In China, due to the limitation of the current technical level, the waste tail vegetable leaves are discarded at will, so that huge resource waste is caused, and the environment is polluted. The traditional method for treating the waste tail vegetable leaves mainly comprises the steps of on-site incineration and random piling. Because the waste tail vegetable leaves have high water content, the waste tail vegetable leaves are piled up in a large amount in the field, are easy to rot and stink, and breed mosquitoes and flies, a good condition is provided for breeding and spreading disease microorganisms, and mineral elements contained in the waste tail vegetable leaves pollute surface water and underground water through surface runoff flushing, seepage and other ways. The on-site incineration can generate a large amount of dense smoke, so that the environment is polluted, the transportation of the channel is seriously influenced, and the haze weather and the like are caused.
Fenton technology is widely used, but this method produces a large amount of iron-containing sludge, which is called Fenton sludge, but which cannot be properly treated and is treated as hazardous waste. Fenton sludge mainly contains Fe 3+ Mainly contains some organic matters,An inorganic salt. Fenton sludge is a dangerous waste, wherein the content of iron and organic matters is too high, so that the water content is too high, scaling is easy to occur, pathogenic microorganisms, parasitic ova and refractory substances are also contained in the Fenton sludge, and the pollution to the environment is easy to cause when the Fenton sludge is discharged at will. A potential source of pollution for landfill sludge treatment is heavy metals in Fenton sludge. Organic matters obtained from Fenton sludge can also produce environmental problems such as decay, peculiar smell and the like in the landfill process. The Fenton sludge is characterized by the following: 1. the Fenton sludge has high heavy metal content, and the random discharge can bring a series of environmental problems; 2. ferric hydroxide flocs exist in Fenton sludge, so that organic matters and other inorganic ions can be removed; 3. the Fenton sludge has high iron content, and can provide an iron source for preparing the porous composite material; 4. easy scaling, strong water retention and failure to achieve the expected effect by common mechanical dehydration; 5. fenton sludge contains a large amount of organic pollutants.
Potassium humate is a high molecular organic matter widely existing in natural environment, is formed by animals and plants through long-time complex biology and chemistry, has complex structure and rich surface with various active functional groups, can interact with a plurality of organic matters and inorganic matters, has wide application, and is currently applied to the aspects of industry, agriculture, medicine, environmental protection and the like.
Disclosure of Invention
The invention reasonably utilizes the waste tail vegetable leaves in the organic solid waste to prepare the organic fertilizer potassium humate and iron doped biochar electrode material, can realize the resource utilization of the waste tail vegetable leaves, lighten the environmental pollution, simultaneously realize the efficient returning of the waste tail vegetable leaves to the field, obtain high added value products and realize the aim of increasing the income of farmers; the carbon residue and Fenton sludge generated in the process are utilized to prepare the iron-doped biochar electrode material while humic acid is extracted, and a new method is provided for the resource utilization of industrial solid waste Fenton sludge.
The technical scheme adopted by the invention is as follows:
a resource utilization method of waste tail vegetable leaves comprises the following specific steps:
(1) Drying the waste tail vegetable leaves in an oven at 100-110 ℃ to constant weight to obtain dried waste tail vegetable leaves, crushing the dried waste tail vegetable leaves, grinding the crushed waste tail vegetable leaves and sieving the crushed waste tail vegetable leaves with a 200-mesh sieve to obtain waste tail vegetable leaf powder, and putting the prepared waste tail vegetable leaf powder into a drying dish for standby;
(2) Placing waste tail vegetable leaf powder into a horizontal tube furnace for pre-carbonization, adjusting the ratio of hydrocarbon to oxygen, adding KOH solution with the concentration of 0.05mol/L into the pre-carbonized material to adjust the pH value to be about 9, stirring for 10-15min by a constant-temperature magnetic stirrer, standing, centrifuging to obtain potassium humate solution and biochar, and drying the potassium humate solution at 105 ℃ to obtain potassium humate (HA-K) particles;
(3) Mixing the biochar obtained in the step (2) with Fenton sludge and water, placing the mixture in a constant-temperature magnetic stirrer, stirring for 10min to uniformly mix, placing the mixture in a vacuum drying oven, drying to constant weight, grinding, sieving with a 100-mesh sieve, carbonizing in a tubular furnace, adding NaOH particles into carbonized materials, grinding and uniformly mixing, and activating the mixture in the tubular furnace to obtain the iron-doped biochar electrode material.
The pre-carbonization in the step (2) is to bake for 1-2h in nitrogen atmosphere at the temperature rising rate of 5 ℃/min to 300-350 ℃.
And (3) ensuring the constant temperature magnetic stirring in the step (2) to be in a room temperature state, wherein the rotating speed of the magnetic stirrer is 450-550rpm.
In the step (3), the mass ratio of the biochar to the Fenton sludge to the water is 0.5-1:0.5-2:30; urea is also added into the mixture in the step (3), and the mass ratio of the urea to the water is 0.5-1:30.
And (3) ensuring the constant temperature magnetic stirring process to be in a room temperature state, wherein the rotating speed of the magnetic stirrer is 450-550rpm.
And (3) ensuring the constant temperature of 60-65 ℃ in the drying process of the vacuum drying oven.
The carbonization process of the step (3) is as follows: firstly introducing nitrogen for 20min, then starting heating, continuously heating to 500-550 ℃ under the protection of nitrogen, preserving heat for 2h, and then heating to 750-800 ℃ and preserving heat for 2h, wherein the flow rate of the nitrogen is 30mL/min, and the heating rate is 3-5 ℃/min.
In the step (3), the mass ratio of the carbonized material to the NaOH particles is 1:1-5, and the NaOH particles are added for mixed grinding.
In the step (3), the activation is carried out in nitrogen atmosphere at the temperature rising rate of 3-5 ℃/min for 2h at 600-650 ℃.
The invention has the beneficial effects that:
(1) The invention extracts the potassium humate organic fertilizer with high added value from the waste cabbage leaves in the organic solid waste.
(2) The invention prepares the iron-nitrogen doped biochar electrode material by using the biochar generated in the extraction process, and solid waste is not generated.
(3) The invention provides a new method for recycling industrial solid waste Fenton sludge.
(4) The invention can achieve the purposes of treating waste with waste, changing waste into valuable and comprehensively utilizing under the condition of not producing secondary pollution; not only can reduce the pollution of waste tail vegetable leaves to the environment, but also can prepare high-value solid fertilizer and iron-doped biochar electrode material, and can achieve the aim of recycling waste.
(5) The invention not only provides a new thought for the treatment of organic solid wastes, but also provides possibility for the full recycling and high-value utilization of the organic solid wastes.
Drawings
FIG. 1 is a thermogravimetric diagram of a waste celery cabbage leaf sample;
FIG. 2 is a process flow diagram of example 2;
FIG. 3 is a process flow diagram of example 5;
fig. 4 is an SEM image of the iron-nitrogen doped biochar electrode material prepared in example 7;
FIG. 5 is a CV diagram of the Fe-N doped biochar electrode material and unmodified CC material prepared in example 7;
fig. 6 is an EIS diagram of the iron-nitrogen doped biochar electrode material and the unmodified CC material prepared in example 7.
Detailed Description
The above-described matters of the present invention will be described in further detail by way of examples, but it should not be construed that the scope of the above-described subject matter of the present invention is limited to the following examples, and all techniques realized based on the above-described matters of the present invention are within the scope of the present invention.
Fenton sludge used in the embodiment of the invention is from a Guangzhou Datansha sewage treatment plant.
Example 1
The method comprises the steps of collecting waste cabbage leaves (waste cabbage leaves) from a certain vegetable market in Kunming, yunnan province on the same day, placing the waste cabbage leaves in an oven, drying the waste cabbage leaves to constant weight at 100-110 ℃ to obtain dry waste cabbage leaves, breaking the dry waste cabbage leaves by a mortar small hammer, placing the dry waste cabbage leaves in a mortar for grinding, sieving the crushed waste cabbage leaves with a 200-mesh sieve to obtain brown cabbage powder, and placing the prepared dry waste cabbage leaf powder in a drying dish for later use;
taking 5g of dry waste Chinese cabbage leaf powder for thermogravimetric determination, analyzing the weightlessness process, wherein the thermogravimetric result is shown in figure 1, and the thermogravimetric result shows that: decomposing at 200-400 deg.c.
Taking 5g of dry waste Chinese cabbage leaf powder for XRF measurement, primarily determining elements in the powder, judging whether the powder is a good precursor for extracting potassium humate, and obtaining XRF results shown in table 1, wherein the result shows that the potassium content in the dry waste Chinese cabbage leaf powder is high, so that a good basis can be provided for preparing the potassium humate.
TABLE 1 XRF determination of waste Chinese cabbage leaves
Element(s) Percentage content% Element(s) Percentage content% Element(s) Percentage content%
Na 0.1088 S 1.0900 Cu 0.0135
Mg 0.4783 Cl 0.6888 Zn 0.0305
Mg 1.0116 K 12.4285 Rb 0.0098
Al 0.0182 Ca 4.6191 Sr 0.0061
Si 0.0329 Mn 0.0151 Fe 0.0829
P 1.1678
The XRF measurement is carried out by taking 5g of Fenton sludge powder, the XRF result is shown in table 2, and the result shows that the waste Fenton sludge has higher iron content, thereby providing a good basis for preparing the iron-nitrogen doped biochar electrode material.
TABLE 2 Fenton sludge XRF assay
Element(s) Percentage content% Element(s) Percentage content% Element(s) Percentage content%
Al 0.3419 K 0.8639 Cr 0.0148
Na 0.9975 Ti 0.8043 Cl 0.6102
Mg 1.0116 Fe 54.7715 Ca 5.5474
Si 0.9387 O 27.0222<balance> S 1.5229
P 0.4229 Zn 0.0898 Sr 0.0282
Mn 0.2280
Example 2
A resource utilization method of waste tail vegetable leaves is shown in fig. 2, and comprises the following specific steps:
(1) Placing the dried waste Chinese cabbage leaf powder prepared in the example 1 into a horizontal tube furnace, roasting for 2 hours at the temperature rising rate of 5 ℃/min to 300 ℃ in a nitrogen atmosphere, pre-carbonizing, adjusting the ratio of hydrocarbon to oxygen, adding KOH solution with the concentration of 0.05mol/L into the pre-carbonized material to adjust the pH value to be about 9, stirring for 10 minutes by using a constant-temperature magnetic stirrer, ensuring the constant-temperature magnetic stirring process to be in a room temperature state, keeping the magnetic stirrer at the rotating speed of 500rpm, standing and centrifuging to obtain potassium humate solution and biochar, and drying the potassium humate solution at 105 ℃ to obtain potassium humate (HA-K) particles;
(2) Mixing the biochar obtained in the step (1) with Fenton sludge and water according to the mass ratio of 0.5:1.5:30, placing the mixture in a constant-temperature magnetic stirrer, stirring for 10min to uniformly mix, ensuring that the mixture is in a room temperature state in the constant-temperature magnetic stirring process, drying the mixture in a 62 ℃ vacuum drying oven until the weight is constant, grinding the mixture, sieving the mixture with a 100-mesh sieve, and carbonizing the mixture in a tubular furnace, wherein the carbonization process comprises the following steps: firstly introducing nitrogen for 20min, then starting heating, continuously introducing nitrogen, heating to 500 ℃ at a heating rate of 3 ℃/min, preserving heat for 2h, heating to 750 ℃ at a heating rate of 3 ℃/min, preserving heat for 2h, adding NaOH particles into the carbonized material according to the mass ratio of the carbonized material to the NaOH particles of 1:3, grinding and uniformly mixing, and activating the mixture in a tube furnace at 600 ℃ at a heating rate of 3 ℃/min in a nitrogen atmosphere to obtain the iron-doped biochar electrode material.
Example 3
A resource utilization method of waste tail vegetable leaves comprises the following specific steps:
(1) Placing the dried waste Chinese cabbage leaf powder prepared in the example 1 into a horizontal tube furnace, roasting for 1h at the temperature rising rate of 5 ℃/min to 350 ℃ in nitrogen atmosphere, pre-carbonizing, adjusting the ratio of hydrocarbon to oxygen, adding KOH solution with the concentration of 0.05mol/L into the pre-carbonized material to adjust the pH value to be about 9, stirring for 15min by a constant-temperature magnetic stirrer, ensuring the room temperature state in the constant-temperature magnetic stirring process, keeping the rotating speed of the magnetic stirrer at 550rpm, standing and centrifuging to obtain potassium humate solution and biochar, and drying the potassium humate solution at 105 ℃ to obtain potassium humate (HA-K) particles;
(2) Mixing the biochar obtained in the step (1) with Fenton sludge and water according to the mass ratio of 1:2:30, placing the mixture in a constant-temperature magnetic stirrer, stirring for 10min to uniformly mix, ensuring that the mixture is in a room temperature state in the constant-temperature magnetic stirring process, placing the magnetic stirrer in a vacuum drying oven at 65 ℃ for drying until the weight is constant, grinding, sieving with a 100-mesh sieve, and carbonizing in a tubular furnace, wherein the carbonizing process comprises the following steps: firstly introducing nitrogen for 20min, then starting heating, continuously introducing nitrogen, heating to 550 ℃ at a heating rate of 5 ℃/min, preserving heat for 2h, heating to 800 ℃ at a heating rate of 5 ℃/min, preserving heat for 2h, wherein the nitrogen flow rate is 30mL/min, adding NaOH particles into the carbonized material according to the mass ratio of the carbonized material to the NaOH particles being 1:5, grinding and uniformly mixing, and activating the mixture in a tube furnace at 650 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere to obtain the iron-doped biochar electrode material.
Example 4
A resource utilization method of waste tail vegetable leaves comprises the following specific steps:
(1) Placing the dried waste Chinese cabbage leaf powder prepared in the example 1 into a horizontal tube furnace, roasting for 1.5 hours at a temperature rising rate of 5 ℃/min to 320 ℃ in a nitrogen atmosphere, pre-carbonizing, adjusting the ratio of hydrocarbon to oxygen, adding KOH solution with the concentration of 0.05mol/L into the pre-carbonized material to adjust the pH value to be about 9, stirring for 12 minutes by a constant-temperature magnetic stirrer, ensuring the constant-temperature magnetic stirring process to be in a room temperature state, standing and centrifuging at the rotating speed of 450rpm of the magnetic stirrer to obtain potassium humate solution and biochar, and drying the potassium humate solution at 105 ℃ to obtain potassium humate (HA-K) particles;
(2) Mixing the biochar obtained in the step (1) with Fenton sludge and water according to the mass ratio of 0.75:0.5:30, placing the mixture in a constant-temperature magnetic stirrer, stirring for 10min to uniformly mix, ensuring that the mixture is in a room temperature state in the constant-temperature magnetic stirring process, drying the mixture in a vacuum drying oven at 60 ℃ until the weight is constant, grinding the mixture, sieving the mixture with a 100-mesh sieve, and carbonizing the mixture in a tubular furnace, wherein the carbonization process comprises the following steps: firstly introducing nitrogen for 20min, then starting heating, continuously introducing nitrogen, heating to 520 ℃ at a heating rate of 4 ℃/min, preserving heat for 2h, heating to 780 ℃ at a heating rate of 4 ℃/min, preserving heat for 2h, wherein the nitrogen flow rate is 30mL/min, adding NaOH particles into the carbonized material according to the mass ratio of the carbonized material to the NaOH particles being 1:1, grinding and uniformly mixing, and activating the mixture in a tube furnace at 640 ℃ at a heating rate of 4 ℃/min in a nitrogen atmosphere, thereby obtaining the iron-doped biochar electrode material.
Example 5
A resource utilization method of waste tail vegetable leaves is shown in fig. 3, and comprises the following specific steps:
(1) Placing the dried waste Chinese cabbage leaf powder prepared in the example 1 into a horizontal tube furnace, roasting for 2 hours at the temperature rising rate of 5 ℃/min to 300 ℃ in a nitrogen atmosphere, pre-carbonizing, adjusting the ratio of hydrocarbon to oxygen, adding KOH solution with the concentration of 0.05mol/L into the pre-carbonized material to adjust the pH value to be about 9, stirring for 10 minutes by using a constant-temperature magnetic stirrer, ensuring the constant-temperature magnetic stirring process to be in a room temperature state, keeping the rotating speed of the magnetic stirrer at 550rpm, standing and centrifuging to obtain potassium humate solution and biochar, and drying the potassium humate solution at 105 ℃ to obtain potassium humate (HA-K) particles;
(2) Mixing the biochar obtained in the step (1) with Fenton sludge, urea and water according to the mass ratio of 0.6:1.5:0.75:30, placing the mixture in a constant-temperature magnetic stirrer, stirring for 10min to uniformly mix, ensuring that the mixture is in a room temperature state in the constant-temperature magnetic stirring process, drying the mixture in a vacuum drying oven at 60 ℃ until the weight is constant, grinding the mixture, sieving the ground mixture with a 100-mesh sieve, and carbonizing the ground mixture in a tubular furnace, wherein the carbonization process comprises the following steps: firstly introducing nitrogen for 20min, then starting heating, continuously introducing nitrogen, heating to 530 ℃ at a heating rate of 4 ℃/min, preserving heat for 2h, heating to 780 ℃ at a heating rate of 4 ℃/min, preserving heat for 2h, wherein the nitrogen flow rate is 30mL/min, adding NaOH particles into the carbonized material according to the mass ratio of the carbonized material to the NaOH particles being 1:1, grinding and uniformly mixing, and activating the mixture in a tube furnace at 620 ℃ at a heating rate of 4 ℃/min in a nitrogen atmosphere, thereby obtaining the iron-nitrogen doped biochar electrode material.
Example 6
A resource utilization method of waste tail vegetable leaves comprises the following specific steps:
(1) Placing the dried waste Chinese cabbage leaf powder prepared in the example 1 into a horizontal tube furnace, roasting for 1h at the temperature rising rate of 5 ℃/min to 350 ℃ in nitrogen atmosphere, pre-carbonizing, adjusting the ratio of hydrocarbon to oxygen, adding KOH solution with the concentration of 0.05mol/L into the pre-carbonized material to adjust the pH value to be about 9, stirring for 15min by a constant-temperature magnetic stirrer, ensuring the room temperature state in the constant-temperature magnetic stirring process, keeping the rotating speed of the magnetic stirrer at 500rpm, standing and centrifuging to obtain potassium humate solution and biochar, and drying the potassium humate solution at 105 ℃ to obtain potassium humate (HA-K) particles;
(2) Mixing the biochar obtained in the step (1) with Fenton sludge, urea and water according to the mass ratio of 0.5:0.5:0.5:30, placing the mixture in a constant-temperature magnetic stirrer, stirring for 10min to uniformly mix, ensuring that the mixture is in a room temperature state in the constant-temperature magnetic stirring process, drying the mixture in a 62 ℃ vacuum drying oven until the rotating speed of the magnetic stirrer is 500rpm, grinding the mixture, sieving the mixture with a 100-mesh sieve, and carbonizing the mixture in a tubular furnace, wherein the carbonization process comprises the following steps: firstly introducing nitrogen for 20min, then starting heating, continuously introducing nitrogen, heating to 500 ℃ at a heating rate of 3 ℃/min, preserving heat for 2h, heating to 750 ℃ at a heating rate of 3 ℃/min, preserving heat for 2h, wherein the nitrogen flow rate is 30mL/min, adding NaOH particles into the carbonized material according to the mass ratio of the carbonized material to the NaOH particles being 1:5, grinding and uniformly mixing, and activating the mixture in a tube furnace at 600 ℃ at a heating rate of 3 ℃/min in a nitrogen atmosphere, thereby obtaining the iron-nitrogen doped biochar electrode material.
Example 7
A resource utilization method of waste tail vegetable leaves comprises the following specific steps:
(1) Placing the dried waste Chinese cabbage leaf powder prepared in the example 1 into a horizontal tube furnace, roasting for 2 hours at the temperature rising rate of 5 ℃/min to 300 ℃ in a nitrogen atmosphere, pre-carbonizing, adjusting the ratio of hydrocarbon to oxygen, adding KOH solution with the concentration of 0.05mol/L into the pre-carbonized material to adjust the pH value to be about 9, stirring for 12 minutes by using a constant-temperature magnetic stirrer, ensuring the constant-temperature magnetic stirring process to be in a room temperature state, keeping the rotating speed of the magnetic stirrer at 450rpm, standing and centrifuging to obtain potassium humate solution and biochar, and drying the potassium humate solution at 105 ℃ to obtain potassium humate (HA-K) particles;
(2) Mixing the biochar obtained in the step (1) with Fenton sludge, urea and water according to the mass ratio of 1:2:1:30, placing the mixture in a constant-temperature magnetic stirrer, stirring for 15min to uniformly mix, ensuring that the mixture is in a room temperature state in the constant-temperature magnetic stirring process, drying the mixture in a vacuum drying oven at 65 ℃ until the weight is constant, grinding the mixture, sieving the mixture with a 100-mesh sieve, and carbonizing the mixture in a tubular furnace, wherein the carbonization process comprises the following steps: firstly introducing nitrogen for 20min, then starting heating, continuously introducing nitrogen, heating to 550 ℃ at a heating rate of 5 ℃/min, preserving heat for 2h, heating to 800 ℃ at a heating rate of 5 ℃/min, preserving heat for 2h, wherein the nitrogen flow rate is 30mL/min, adding NaOH particles into the carbonized material according to the mass ratio of the carbonized material to the NaOH particles being 1:3, grinding and uniformly mixing, and activating the mixture in a tube furnace at 650 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere, thereby obtaining the iron-nitrogen doped biochar electrode material.
SEM characterization of the Fe-N doped biochar electrode material obtained in example 7 shows the results in FIG. 4, in which nano-scale FeOOH and Fe are clearly seen 2 O 3 And Fe (Fe) 3 O 4 In-situ growth on biochar surface, wherein FeOOH particles and Fe 2 O 3 The size of (2) is about 500nm, fe 3 O 4 The size of the particles is 100-200nm, and the doping of iron and nitrogen has been found to improve the biocompatibility of the anode surface to promote the growth of electrogenic microorganisms on the anode surface, increasing the probability of electrons being transferred to the anode.
The cyclic voltammetry test (CV, shown in fig. 5) and the electrochemical impedance spectroscopy test (EIS, shown in fig. 6) were performed on the iron-nitrogen doped biochar electrode material prepared in example 7 in a PBS solution, and it can be clearly seen from the figure that the integrated area of the CV curve of the prepared iron-nitrogen doped biochar electrode material is larger than that of the unmodified CC material (i.e., the biochar material obtained in step (1)), and the maximum current density achieved is also higher than that of the unmodified CC material, which indicates that the conductivity of the electrode material can be improved and the specific capacitance can be increased by performing the present example.

Claims (7)

1. A resource utilization method of waste tail vegetable leaves is characterized by comprising the following specific steps:
(1) Drying the waste tail vegetable leaves at 100-110 ℃ to constant weight, breaking and grinding the waste tail vegetable leaves and sieving the waste tail vegetable leaves with a 200-mesh sieve to obtain waste tail vegetable leaf powder;
(2) Pre-carbonizing waste cabbage leaf powder, adding KOH solution with the concentration of 0.05mol/L into the pre-carbonized material to adjust the pH value to 9, magnetically stirring at constant temperature for 10-15min, standing, centrifuging to obtain potassium humate solution and biochar, and drying the potassium humate solution to obtain potassium humate particles;
(3) Mixing the biochar obtained in the step (2) with Fenton sludge and water, adding urea into the mixture, wherein the mass ratio of urea to water is 0.5-1:30, magnetically stirring the mixture at constant temperature for 10min, vacuum drying to constant weight, grinding, sieving with a 100-mesh sieve, carbonizing, adding NaOH particles into carbonized materials, grinding, uniformly mixing, activating, and preserving the temperature for 2h at 600-650 ℃ at a heating rate of 3-5 ℃/min in a nitrogen atmosphere to obtain the iron-doped biochar electrode material.
2. The method for recycling waste cabbage leaves according to claim 1, wherein the pre-carbonization in the step (2) is performed in a nitrogen atmosphere at a temperature rising rate of 5 ℃/min to 300-350 ℃ for roasting for 1-2 hours.
3. The recycling method of waste cabbage leaves according to claim 1, wherein the constant temperature magnetic stirring process of the step (2) and the step (3) is in a room temperature state, and the rotating speed is 450-550rpm.
4. The method for recycling waste cabbage leaves according to claim 1, wherein the mass ratio of the biochar, fenton sludge and water in the step (3) is 0.5-1:0.5-2:30.
5. The method for recycling waste cabbage leaves according to claim 1, wherein the vacuum drying temperature in the step (3) is 60-65 ℃.
6. The method for recycling waste cabbage leaves according to claim 1, wherein the carbonization process of step (3) is: introducing nitrogen for 20min, heating to 500-550 ℃, preserving heat for 2h, and heating to 750-800 ℃ for 2h, wherein the flow rate of the nitrogen is 30mL/min, and the heating rate is 3-5 ℃/min.
7. The method for recycling waste cabbage leaves according to claim 1, wherein the mass ratio of the carbonized material to the NaOH particles in the step (3) is 1:1-5.
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* Cited by examiner, † Cited by third party
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CN110330024A (en) * 2019-04-03 2019-10-15 沈阳化工大学 A method of ultramarine green pigment is prepared with discarded molecular sieve and charcoal
CN113786804A (en) * 2021-09-18 2021-12-14 昆明理工大学 Preparation method and application of magnetic porous composite material for adsorbing heavy metals

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CN103779111A (en) * 2014-01-27 2014-05-07 华南理工大学 Method for manufacturing electrode materials of super-capacitors by using surplus sludge
CN110482656A (en) * 2019-09-05 2019-11-22 中国科学院过程工程研究所 A kind of resource utilization method of coagulation sludge and products thereof and purposes
CN112194133A (en) * 2020-10-12 2021-01-08 管小丹 Activated carbon material applied to electrode material of supercapacitor
CN112938963B (en) * 2021-02-09 2023-02-10 同济大学 Method for preparing magnetic carbon by using straws and Fenton sludge and application

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110330024A (en) * 2019-04-03 2019-10-15 沈阳化工大学 A method of ultramarine green pigment is prepared with discarded molecular sieve and charcoal
CN113786804A (en) * 2021-09-18 2021-12-14 昆明理工大学 Preparation method and application of magnetic porous composite material for adsorbing heavy metals

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