CN115430397A - Biochar and preparation method thereof - Google Patents

Biochar and preparation method thereof Download PDF

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Publication number
CN115430397A
CN115430397A CN202210947478.XA CN202210947478A CN115430397A CN 115430397 A CN115430397 A CN 115430397A CN 202210947478 A CN202210947478 A CN 202210947478A CN 115430397 A CN115430397 A CN 115430397A
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biochar
carbide
powder
green
potassium hydroxide
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张志军
韩学超
谢智翔
成鹏
尹翔
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Huaide College of Changzhou University
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Huaide College of Changzhou 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
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28011Other properties, e.g. density, crush strength
    • 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
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054Solid 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 surface properties or porosity
    • B01J20/28057Surface area, e.g. B.E.T specific surface area
    • 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
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054Solid 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 surface properties or porosity
    • B01J20/28078Pore diameter
    • B01J20/2808Pore diameter being less than 2 nm, i.e. micropores or nanopores
    • 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
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • 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
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4887Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
    • 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
    • C02F2101/308Dyes; Colorants; Fluorescent agents

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Abstract

The invention provides biochar and a preparation method thereof, which relate to the technical field of biomass treatment methods, and the preparation method comprises the following steps: crushing green soybean pods to obtain green soybean pod powder; chemically activating the green soy pod powder by using a potassium hydroxide solution to obtain an activated solution; adding alumina and lauric acid to the activated solution to obtain a thick substance; drying the thick substance to obtain a solid; carbonizing the solid to obtain a carbide; and (3) washing the carbide, dehydrating in vacuum, and grinding into powder to obtain the biochar. The preparation method of the biochar provided by the invention is simple and convenient in process, and the biochar is prepared by taking agricultural wastes such as green soy pods which are low in price and rich in source as biological materials, so that a new way for treating the agricultural wastes in a green, energy-saving and environment-friendly manner is provided for the prior art while a biochar product with added economic benefit can be obtained and the production cost of the biochar is reduced.

Description

Biochar and preparation method thereof
Technical Field
The invention relates to the technical field of biomass treatment methods, and particularly relates to biochar and a preparation method thereof.
Background
Methylene blue is a phenothiazine cationic dye widely applied to printing and other industries; with the development of the printing and dyeing industry, the amount of wastewater containing methylene blue generated is increased sharply. The wastewater containing methylene blue can generate adverse effect on the growth of aquatic organisms after entering a natural water body.
At present, the commonly used wastewater treatment methods include a biological method, an electrochemical method and an adsorption method; the adsorption method is an effective method for treating wastewater because of simple treatment process, low operation cost and small occupied area.
The traditional adsorption method mostly uses biochar as an adsorbent, but the existing biochar has high preparation cost, so that the cost of wastewater treatment by the adsorption method is high.
Disclosure of Invention
The invention solves the technical problem that the existing biochar has higher preparation cost.
In order to solve the problems, the invention provides a preparation method of biochar, which comprises the following steps:
s1: crushing green soybean pods to obtain green soybean pod powder;
s2: chemically activating the green soy pod powder by using a potassium hydroxide solution to obtain an activated solution;
s3: adding alumina and lauric acid into the activated solution at the temperature of 40-50 ℃ to obtain a thick substance;
s4: drying the thick substance at 105 ℃ to obtain a solid;
s5: carbonizing the solid at 500-700 ℃ to obtain a carbide;
s6: and (3) after the carbide is washed, dehydrating in vacuum at 40-50 ℃, and grinding into powder to obtain the biochar.
Optionally, step S1 comprises: cleaning the green soybean pods, drying, and crushing into powder to obtain the green soybean pod powder.
Optionally, the green soybean pod powder has a particle size ranging from 40 mesh to 80 mesh.
Optionally, step S2 comprises: and placing the green soy pod powder and the potassium hydroxide solution in an ultrasonic cleaner, vibrating for 30min, and vibrating for 10-12 h at 40-50 ℃ in a constant-temperature oscillator.
Optionally, step S5 comprises: and (3) placing the solid in a tube furnace, vacuumizing, keeping the air pressure stable at-0.1-0 MPa, discharging carbonization gas to normal pressure when the air pressure reaches a critical point of 0MPa, increasing the temperature to 500-700 ℃ at a heating rate of 20 ℃/min, and pyrolyzing for 60-120 min to obtain the carbide.
Optionally, the step S6 of flushing the char comprises: cooling the carbide to room temperature, boiling the carbide with 0.1mol/L hydrochloric acid, soaking the carbide to remove ash, and washing the carbide with ultrapure water until the carbide is neutral.
Optionally, the mass ratio of the green soy pod powder to the potassium hydroxide solution in step S2 is 1.
Optionally, the amount of the aluminum oxide is 1% to 5% of the mass of the potassium hydroxide solution.
Optionally, the amount of the lauric acid is 5 to 10 percent of the mass of the potassium hydroxide solution.
Another object of the present invention is to provide a biochar prepared by the method for preparing biochar as described above.
Compared with the prior art, the preparation method of the biochar provided by the invention has the following advantages:
the preparation method of the biochar provided by the invention is simple and convenient in process, and the biochar is prepared by taking agricultural wastes such as green soy pods which are low in price and rich in source as biological materials, so that a new way for treating the agricultural wastes in a green, energy-saving and environment-friendly manner is provided for the prior art while a biochar product with added economic benefit can be obtained and the production cost of the biochar is reduced.
Detailed Description
The following describes in detail embodiments of the present invention. The embodiments described below are exemplary and are intended to be illustrative of the present invention and should not be construed as limiting the present invention, and all other embodiments that can be obtained by one of ordinary skill in the art based on the embodiments of the present invention without inventive step fall within the scope of the present invention.
In order to solve the problem of higher preparation cost of the existing biochar, the invention provides a preparation method of biochar, which comprises the following steps:
s1: crushing green soybean pods to obtain green soybean pod powder;
s2: chemically activating the green soy pod powder by using a potassium hydroxide solution to obtain an activated solution; the concentration of the potassium hydroxide solution is preferably 6mol/L;
s3: adding alumina and lauric acid into the activated solution at the temperature of 40-50 ℃ to obtain a thick substance;
s4: drying the thick substance at 105 ℃ to obtain a solid;
s5: carbonizing the solid at 500-700 ℃ to obtain a carbide;
s6: and (3) after the carbide is washed, dehydrating in vacuum at 40-50 ℃, and grinding into powder to obtain the biochar.
The green soybean pods are generally discarded as solid wastes in agriculture and life, but the cellulose content of the green soybean pods is high, and if the green soybean pods are recycled and used as biological materials to prepare biochar, the green soybean pods are an effective means for realizing waste recycling. The preparation of the adsorbent by using the green soy bean pods reflects the residual value of agricultural wastes, avoids resource waste and has important significance for developing circular economy and controlling waste pollution.
The preparation method of the biochar provided by the invention is simple and convenient in process, and the biochar is prepared by taking agricultural wastes such as green soy pods which are low in price and rich in source as biological materials, so that a new way for treating the agricultural wastes in a green, energy-saving and environment-friendly manner is provided for the prior art while a biochar product with added economic benefit can be obtained and the production cost of the biochar is reduced.
The green soybean pod biomass production technology takes the agricultural waste green soybean pods as the raw material, has short production period, low cost, wide sources, low energy consumption and no pollution, can improve the quality of cultivated land soil and reduce resource waste when being used as a biomass material in the environment, reasonably utilizes the agricultural waste resources, changes waste into valuables, and has great significance for relieving the energy pressure of China and protecting the ecological environment.
According to the preparation method provided by the invention, biomass is thermally cracked at high temperature under an anoxic condition to form a solid substance, non-carbon elements are decomposed and escaped to form a hole structure in a carbonization process, potassium is diffused into different carbon layers in a gaseous state to perform catalytic oxidation with carbon after carbonization, and the carbon is further etched to form abundant micropores.
In order to ensure the adsorption performance of the biochar, the invention preferably comprises the following step S1: cleaning green soybean pods, drying, and crushing into powder to obtain green soybean pod powder; specifically, the method comprises the steps of cleaning the green soybean pods, drying the green soybean pods in an oven at 105 ℃ or in the sun to constant weight, crushing the green soybean pods into powder by a crusher, and sieving the powder by a sieve to remove impurities to obtain the green soybean pod powder.
The preferred particle size range of the green soy bean pod powder is 40-80 meshes.
In order to make the prepared biochar have a rich microporous structure, the invention preferably comprises the following step S2: placing the green soy pod powder and a potassium hydroxide solution in an ultrasonic cleaner for vibration for 30min, and then vibrating in a constant-temperature oscillator at 40-50 ℃ for 10-12 h.
The preferable step S3 of the invention specifically comprises the steps of adding alumina and lauric acid into the activated solution at the temperature of 40-50 ℃, and oscillating for 1h to obtain a thick substance.
And the step S4 specifically comprises the steps of pouring the thick substance into a quartz boat, placing the quartz boat in a drying box, and drying the quartz boat at 105 ℃ to obtain a solid.
The present invention preferably includes in step S5: and (3) putting the solid in a tube furnace, vacuumizing, keeping the air pressure to be stable at-0.1-0 MPa, discharging the carbonization gas to normal pressure when the air pressure reaches a critical point of 0MPa, increasing the temperature to 500-700 ℃ at a heating rate of 20 ℃/min, and pyrolyzing for 60-120 min to obtain the carbide.
The preferred step S6 of washing the carbide of the present invention comprises: cooling the carbide to room temperature, boiling with 0.1mol/L hydrochloric acid, soaking to remove ash, and washing with ultrapure water to neutrality.
In order to ensure the adsorption performance of the biochar, the invention preferably selects the mass ratio of the green soy pod powder to the potassium hydroxide solution in the step S2 as 1.5; preferably, the using amount of the alumina is 1 to 5 percent of the mass of the potassium hydroxide solution; the dosage of the lauric acid is 5 to 10 percent of the mass of the potassium hydroxide solution.
Another object of the present invention is to provide a biochar, which is prepared by the above-described method for preparing biochar.
According to the biochar provided by the invention, the agricultural waste which is low in price and rich in source and is green in the green energy-saving environment-friendly mode is used as a biological material to prepare the biochar, so that a biochar product with added economic benefits can be obtained, the production cost of the biochar is reduced, and a new way for treating the agricultural waste in a green energy-saving environment-friendly mode is provided for the prior art.
The biochar prepared from raw material of green soy bean pod has average pore diameter of 2.20nm and micropore volume of 0.2442cm 3 The specific surface area of Langumir is 954.6652m 2 /g。
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, specific embodiments thereof are described in detail below.
Example 1
The embodiment provides a preparation method of biochar, which specifically comprises the following steps:
s1: cleaning and drying 8g of green soybean pods, crushing the green soybean pods into powder by using a crusher, and sieving the powder by using a 40-mesh sieve to remove impurities to obtain green soybean pod powder;
s2: chemically activating green soybean pod powder by using a potassium hydroxide solution (the mass ratio of green soybean pods to potassium hydroxide is 1.5), placing the green soybean pod powder in an ultrasonic cleaner, vibrating for 30min, and then vibrating for 12h in a constant-temperature oscillator at 40 ℃ to obtain an activated solution;
s3: adding alumina and lauric acid into the activated solution, and oscillating for 1h at 45 ℃ to obtain a thick substance; wherein the dosage of the alumina is 3 percent of the mass of the potassium hydroxide solution, and the dosage of the lauric acid is 7 percent of the mass of the potassium hydroxide solution;
s4: pouring the thick substance into a quartz boat, and drying in a drying oven at 105 ℃ to obtain a solid;
s5: placing the solid in a tube furnace, vacuumizing, keeping the air pressure stable at-0.1-0 MPa, discharging carbonization gas to normal pressure when the air pressure reaches a critical point of 0MPa, increasing the temperature to 600 ℃ at a heating rate of 20 ℃/min, and pyrolyzing for 60min to carbonize to obtain a carbide;
s6: cooling the carbide to room temperature, boiling and soaking the carbide with 0.1mol/L hydrochloric acid to remove ash, repeatedly washing the carbide with ultrapure water to neutrality, performing vacuum dehydration at 50 ℃, and grinding the carbide into powder to obtain the biochar.
The biochar is tested, the pore diameter of the biochar is 0.8-42nm, and the volume of micropores is 0.244cm 3 The specific surface area of Langumir is 954.6652m 2 /g。
The application of the biochar comprises the following steps:
adsorbing 100ml of 100mg/L methylene blue solution, adjusting 8 different pH values of 3.5, 4.5, 5.5, 6.5, 7.5, 8.5, 9.5 and 10.5 by using 0.01mol/L HCl and NaOH solutions, adding 0.01g of biochar respectively, and putting the biochar into a shaking table at the temperature of 45 ℃ for mixing and contacting for 120min; the removal rate of the methylene blue solution by the biochar sample can reach 98%, and the adsorption quantity is 980mg/g.
Example 2
The embodiment provides a preparation method of biochar, which specifically comprises the following steps:
s1: cleaning 8g of green soybean pods, airing and drying, crushing the green soybean pods into powder by using a crusher, and sieving the powder by using a 40-mesh sieve to remove impurities to obtain green soybean pod powder;
s2: chemically activating green soybean pod powder by using a potassium hydroxide solution (the mass ratio of the green soybean pod to the potassium hydroxide is 1.5), placing the green soybean pod powder in an ultrasonic cleaner, vibrating the green soybean pod powder for 30min, and then vibrating the green soybean pod powder in a constant-temperature oscillator at 45 ℃ for 10h to obtain an activated solution;
s3: adding alumina and lauric acid into the activated solution, and oscillating for 1h at 45 ℃ to obtain a thick substance; wherein the dosage of the alumina is 1 percent of the mass of the potassium hydroxide solution, and the dosage of the lauric acid is 5 percent of the mass of the potassium hydroxide solution;
s4: pouring the thick substance into a quartz boat, and drying in a drying oven at 105 ℃ to obtain a solid;
s5: placing the solid in a tube furnace, vacuumizing, keeping the air pressure stable at-0.1-0 MPa, discharging carbonization gas to normal pressure when the air pressure reaches a critical point of 0MPa, increasing the temperature to 500 ℃ at a heating rate of 20 ℃/min, and pyrolyzing for 60min to carbonize to obtain a carbide;
s6: cooling the carbide to room temperature, boiling and soaking the carbide with 0.1mol/L hydrochloric acid to remove ash, repeatedly washing the carbide with ultrapure water to neutrality, performing vacuum dehydration at 50 ℃, and grinding the carbide into powder to obtain the biochar.
The application of the biochar comprises the following steps:
when adsorbing 100ml of 50mg/L methylene blue solution, adjusting 8 different pH values of 3.5, 4.5, 5.5, 6.5, 7.5, 8.5, 9.5 and 10.5 by using 0.01mol/L HCl and NaOH solutions, respectively adding 0.01g of biochar, and putting the biochar into a shaking table at the temperature of 55 ℃ for mixing and contacting for 60min; the removal rate of the methylene blue solution by the biochar sample can reach 99%, and the adsorption quantity is 497mg/g.
Example 3
The embodiment provides a preparation method of biochar, which specifically comprises the following steps:
s1: cleaning 8g of green soybean pods, airing and drying, crushing the green soybean pods into powder by using a crusher, and sieving the powder by using a 40-mesh sieve to remove impurities to obtain green soybean pod powder;
s2: chemically activating green soybean pod powder by using a potassium hydroxide solution (the mass ratio of green soybean pods to potassium hydroxide is 1.5), placing the green soybean pod powder in an ultrasonic cleaner, vibrating for 30min, and then vibrating for 12h in a constant-temperature oscillator at 45 ℃ to obtain an activated solution;
s3: adding alumina and lauric acid into the activated solution, and oscillating for 1h at 45 ℃ to obtain a thick substance; wherein the dosage of the alumina is 5 percent of the mass of the potassium hydroxide solution, and the dosage of the lauric acid is 10 percent of the mass of the potassium hydroxide solution;
s4: pouring the thick substance into a quartz boat, and drying in a drying oven at 105 ℃ to obtain a solid;
s5: placing the solid in a tube furnace, vacuumizing, keeping the air pressure stable at-0.1-0 MPa, discharging carbonization gas to normal pressure when the air pressure reaches a critical point of 0MPa, increasing the temperature to 700 ℃ at a heating rate of 20 ℃/min, and pyrolyzing for 80min to carbonize to obtain a carbide;
s6: cooling the carbide to room temperature, boiling and soaking the carbide with 0.1mol/L hydrochloric acid to remove ash, repeatedly washing the carbide with ultrapure water to neutrality, performing vacuum dehydration at 50 ℃, and grinding the carbide into powder to obtain the biochar.
The application of the biochar comprises the following steps:
transferring 100mL of methylene blue solutions of 50mg/L, 100mg/L and 150mg/L into a conical flask of 150mL respectively, adding 0.01g of biochar respectively, placing in a shaking table at 35, 45 and 55 ℃ for shaking, and sampling after the adsorption balance is achieved. The adsorption amount of the biochar to the methylene blue is increased along with the increase of the temperature, which indicates that the adsorption is an endothermic reaction, and the temperature rise is favorable for adsorption. And as the concentration increases, the adsorption amount of methylene blue also increases, and the removal rate decreases.
Example 4
The embodiment provides a preparation method of biochar, which specifically comprises the following steps:
s1: cleaning and drying 8g of green soybean pods, crushing the green soybean pods into powder by using a crusher, and sieving the powder by using a 40-mesh sieve to remove impurities to obtain green soybean pod powder;
s2: chemically activating green soybean pod powder by using a potassium hydroxide solution (the mass ratio of green soybean pods to potassium hydroxide is 1.5), placing the green soybean pod powder in an ultrasonic cleaner, vibrating for 30min, and then vibrating for 12h in a constant-temperature oscillator at 45 ℃ to obtain an activated solution;
s3: adding alumina and lauric acid into the activated solution, and oscillating for 1h at 45 ℃ to obtain a thick substance; wherein the dosage of the alumina is 5 percent of the mass of the potassium hydroxide solution, and the dosage of the lauric acid is 10 percent of the mass of the potassium hydroxide solution;
s4: pouring the thick substance into a quartz boat, and drying in a drying oven at 105 ℃ to obtain a solid;
s5: putting the solid in a tube furnace, vacuumizing, keeping the air pressure stable at-0.1-0 MPa, discharging carbonization gas to normal pressure when the air pressure reaches a critical point of 0MPa, increasing the temperature to 600 ℃ at a heating rate of 20 ℃/min, and pyrolyzing for 80min to carbonize to obtain a carbide;
s6: cooling the carbide to room temperature, boiling and soaking the carbide with 0.1mol/L hydrochloric acid to remove ash, repeatedly washing the carbide with ultrapure water to neutrality, performing vacuum dehydration at 50 ℃, and grinding the carbide into powder to obtain the biochar.
The application of the biochar comprises the following steps:
transferring 100mL of methylene blue solutions of 40mg/L and 800mg/L into a conical flask of 150mL respectively, adding 0.01g of biochar respectively, placing the bottles in shaking tables of 35, 45 and 55 ℃ for oscillation, and sampling after adsorption balance is achieved; the adsorption amount of the biochar to the methylene blue is increased along with the increase of the temperature, which indicates that the adsorption is an endothermic reaction, and the temperature rise is favorable for adsorption. And as the concentration increases, the adsorption amount of methylene blue also increases, and the removal rate decreases.
Comparative example 1
The comparative example provides a preparation method of biochar, which specifically comprises the following steps:
s1: cleaning and drying 8g of green soybean pods, crushing the green soybean pods into powder by using a crusher, and sieving the powder by using a 40-mesh sieve to remove impurities to obtain green soybean pod powder;
s2: adding green soy pod powder into deionized water to obtain a solution;
s3: adding alumina and lauric acid into the solution, and oscillating at 45 ℃ for 1h to obtain a thick substance; wherein the dosage of the alumina is 3 percent of the mass of the potassium hydroxide solution, and the dosage of the lauric acid is 7 percent of the mass of the potassium hydroxide solution;
s4: pouring the thick substance into a quartz boat, and drying in a drying oven at 105 ℃ to obtain a solid;
s5: putting the solid in a tube furnace, vacuumizing, keeping the air pressure stable at-0.1-0 MPa, discharging carbonization gas to normal pressure when the air pressure reaches a critical point of 0MPa, increasing the temperature to 600 ℃ at a heating rate of 20 ℃/min, and pyrolyzing for 60min to carbonize to obtain a carbide;
s6: cooling the carbide to room temperature, boiling and soaking the carbide with 0.1mol/L hydrochloric acid to remove ash, repeatedly washing the carbide with ultrapure water to neutrality, performing vacuum dehydration at 50 ℃, and grinding the carbide into powder to obtain the biochar.
The biochar is tested, the aperture of the biochar is 6.2-28nm, and the volume of the micropore is 0.078cm 3 G, langmuir specific surface area 217.43m 2 /g。
The application of the biochar comprises the following steps:
adsorbing 100ml of 100mg/L methylene blue solution, adjusting 8 different pH values of 3.5, 4.5, 5.5, 6.5, 7.5, 8.5, 9.5 and 10.5 by using 0.01mol/L HCl and NaOH solutions, adding 0.01g of biochar respectively, and putting the biochar into a shaking table at the temperature of 45 ℃ for mixing and contacting for 120min; the removal rate of the methylene blue solution by the biochar sample is 47%, and the adsorption capacity is 139mg/g.
The difference between the comparative example 1 and the example 1 is that the prepared charcoal has obviously reduced adsorption performance on methylene blue without being activated by potassium hydroxide in the preparation process.
Comparative example 2
The embodiment provides a preparation method of biochar, which specifically comprises the following steps:
s1: cleaning and drying 8g of green soybean pods, crushing the green soybean pods into powder by using a crusher, and sieving the powder by using a 40-mesh sieve to remove impurities to obtain green soybean pod powder;
s2: chemically activating green soybean pod powder by using a potassium hydroxide solution (the mass ratio of the green soybean pod to the potassium hydroxide is 1.5), placing the green soybean pod powder in an ultrasonic cleaner, vibrating the green soybean pod powder for 30min, and then vibrating the green soybean pod powder in a constant-temperature oscillator at 45 ℃ for 10h to obtain an activated solution;
s3: pouring the activated solution into a quartz boat, and drying the quartz boat in a drying oven at 105 ℃ to obtain a solid;
s4: putting the solid in a tube furnace, vacuumizing, keeping the air pressure stable at-0.1-0 MPa, discharging carbonization gas to normal pressure when the air pressure reaches a critical point of 0MPa, increasing the temperature to 500 ℃ at a heating rate of 20 ℃/min, and pyrolyzing for 60min to carbonize to obtain a carbide;
s5: cooling the carbide to room temperature, boiling and soaking the carbide with 0.1mol/L hydrochloric acid to remove ash, repeatedly washing the carbide with ultrapure water to neutrality, performing vacuum dehydration at 50 ℃, and grinding the carbide into powder to obtain the biochar.
The biochar is tested, the pore diameter of the biochar is 3.3-39nm, and the volume of micropores is 0.109cm 3 G, langmuir specific surface area 277.09m 2 /g。
The application of the biochar comprises the following steps:
adsorbing 50mg/L methylene blue solution 100ml, adjusting pH values of 8 different pH values of 3.5, 4.5, 5.5, 6.5, 7.5, 8.5, 9.5 and 10.5 with 0.01mol/L HCl and NaOH solutions, adding 0.01g of biochar respectively, and placing in a shaking table at 55 ℃ for mixing and contacting for 60min; the removal rate of the methylene blue solution by the biochar sample is 59 percent, and the adsorption quantity is 236mg/g.
The difference between the comparative example 2 and the example 1 is that alumina is not introduced in the preparation process, and the adsorption performance of the prepared biochar to methylene blue is obviously reduced.
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present disclosure, and such changes and modifications will fall within the scope of the present invention.

Claims (10)

1. The preparation method of the biochar is characterized by comprising the following steps:
s1: crushing green soybean pods to obtain green soybean pod powder;
s2: chemically activating the green soy pod powder by using a potassium hydroxide solution to obtain an activated solution;
s3: adding alumina and lauric acid into the activated solution at the temperature of 40-50 ℃ to obtain a thick substance;
s4: drying the thick substance at 105 ℃ to obtain a solid;
s5: carbonizing the solid at 500-700 ℃ to obtain a carbide;
s6: and (3) after the carbide is washed, dehydrating in vacuum at 40-50 ℃, and grinding into powder to obtain the biochar.
2. The method of preparing biochar according to claim 1, wherein step S1 comprises: and cleaning the green soybean pods, drying, and crushing into powder to obtain the green soybean pod powder.
3. The method of producing biochar according to claim 2, wherein the green soybean pod powder has a particle size ranging from 40 mesh to 80 mesh.
4. The method for preparing bio-char according to claim 1, wherein the step S2 comprises: and placing the green soy pod powder and the potassium hydroxide solution in an ultrasonic cleaner, vibrating for 30min, and vibrating for 10-12 h at 40-50 ℃ in a constant-temperature oscillator.
5. The method of preparing biochar of claim 1, wherein step S5 comprises: and (3) placing the solid in a tube furnace, vacuumizing, keeping the air pressure stable at-0.1-0 MPa, discharging carbonization gas to normal pressure when the air pressure reaches a critical point of 0MPa, increasing the temperature to 500-700 ℃ at a heating rate of 20 ℃/min, and pyrolyzing for 60-120 min to obtain the carbide.
6. The method for producing biochar according to claim 1, wherein the washing of the char in step S6 includes: cooling the carbide to room temperature, boiling the carbide with 0.1mol/L hydrochloric acid, soaking the carbide to remove ash, and then washing the carbide with ultrapure water to be neutral.
7. The method for producing biochar according to any one of claims 1 to 6, wherein the mass ratio of the green soy pod powder to the potassium hydroxide solution in step S2 is 1.
8. The method for preparing biochar according to claim 7, wherein the amount of the alumina is 1 to 5% by mass of the potassium hydroxide solution.
9. The method for preparing biochar according to claim 7, wherein the amount of the lauric acid is 5-10% of the mass of the potassium hydroxide solution.
10. Biochar characterized by being produced by the method for producing biochar as claimed in any one of claims 1 to 9.
CN202210947478.XA 2022-08-09 2022-08-09 Biochar and preparation method thereof Pending CN115430397A (en)

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CN111686686A (en) * 2020-05-27 2020-09-22 北京林丰源生态环境规划设计院有限公司 Preparation method of reed biochar and method for treating methylene blue in water body by using reed biochar
CN113145076A (en) * 2021-05-13 2021-07-23 沈阳农业大学 Preparation method of modified biochar and modified biochar
CN113457624A (en) * 2021-06-18 2021-10-01 广西大学 Modified mushroom dreg biochar and preparation method thereof
CN113952928A (en) * 2021-11-16 2022-01-21 东北农业大学 Carbon-based adsorbent and preparation method thereof
CN114405473A (en) * 2022-02-17 2022-04-29 广东石油化工学院 Preparation method and application of calcium hydroxide modified straw stalk biochar
CN114797766A (en) * 2022-03-14 2022-07-29 南京工业大学 Porous biochar and preparation method and application thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105056882A (en) * 2015-07-20 2015-11-18 昆明理工大学 Preparation method of modified charcoal-based adsorbent for removing hydrogen sulfide
CN111686686A (en) * 2020-05-27 2020-09-22 北京林丰源生态环境规划设计院有限公司 Preparation method of reed biochar and method for treating methylene blue in water body by using reed biochar
CN113145076A (en) * 2021-05-13 2021-07-23 沈阳农业大学 Preparation method of modified biochar and modified biochar
CN113457624A (en) * 2021-06-18 2021-10-01 广西大学 Modified mushroom dreg biochar and preparation method thereof
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