CN112263989A - Method for preparing magnetic biochar by one-step method - Google Patents
Method for preparing magnetic biochar by one-step method Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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Abstract
The invention discloses a method for preparing magnetic biochar by a one-step method, which comprises the following steps of S1: straw pretreatment: drying and crushing plant straws, and screening particles with the particle size of 60-30 meshes for later use; s2: iron salt impregnation: adding an iron salt solution into the straw particles in the step S1 for dipping, adjusting the pH value to 10-11 by using an alkali liquor, and then preserving heat for dipping; s3: high-temperature pyrolysis: carrying out suction filtration and drying on the impregnated particles in the step S2, and transferring the particles to an atmosphere furnace for high-temperature pyrolysis to obtain a crude product of the magnetic biochar; s4: and (3) post-treatment: and (4) carrying out suction filtration, cleaning and drying on the crude product of the magnetic biochar obtained by pyrolysis in the S3 to obtain a finished product of the magnetic activated carbon. The method for preparing the magnetic biochar by the one-step method provided by the invention can be used for preparing the magnetic activated carbon by pyrolyzing and magnetizing plant straws serving as raw materials in one step, is simple and is easy to realize large-scale production.
Description
Technical Field
The invention belongs to the field of activated carbon preparation, and particularly relates to a method for preparing magnetic biochar by a one-step method.
Background
With the development of agriculture and the improvement of the living standard of people, the phenomena of crop straw waste, direct burning and the like become more common. According to related researches, the waste incineration of straws becomes a remarkable environmental and social problem in China, and farmers can incinerate the straws because the opportunity cost for harvesting and utilizing the straws is too high and the income is lower; the environment benefit of the novel straw resource utilization technologies such as straw power generation, straw gasification centralized gas supply and the like is obvious, but the economic benefit is influenced by the factors such as technology, raw materials, market and the like, and uncertainty exists; the high cost of straw collection, storage and transportation and the imperfect related systems become key factors restricting the large-scale utilization of straws. On the whole, the comprehensive benefits of the prior art are not obvious, which limits the improvement of the resource utilization level of the Chinese straws, and further promotes the technical innovation of the related fields. If the energy can be reasonably utilized, considerable economic benefit and environmental benefit can be brought.
Biochar is a porous carbon formed by pyrolysis of biomass raw materials such as livestock and poultry manure, animal bones, waste wood chips, sludge, crop straws and the like under the condition of low oxygen or no oxygen. The composite material has the characteristics of highly developed pore structure, large specific surface area, rich functional groups on the surface, stable performance, acid and alkali resistance, high temperature resistance and the like, has good adsorption capacity for heavy metals, organic pollutants and the like in the environments such as soil, water and the like, is low in preparation cost, and becomes a hotspot concerned in the fields of agriculture, ecological restoration, environmental protection and the like. It is commonly used for adsorption of pollutants in water and as a carrier of catalysts for chemical production. However, after the adsorption or catalytic process is completed, the spent adsorbent and the deactivated catalyst are generally recovered by high-speed centrifugation or filtration, resulting in energy waste and equipment loss. Based on the above, in recent years, researchers have effectively solved the problem that biochar is difficult to recover and separate by magnetizing the biochar to prepare magnetic biochar.
The magnetic biochar has certain adsorption performance and magnetism accompanied with the material. Its advantage is that the biochar can be used by external magnetic fieldThe separation of the biochar from other impurities is more conveniently realized. The existing process for preparing magnetic biochar and magnetic activated carbon utilizes FeCl on the basis of biochar and activated carbon prepared by carbonization and activation3The solution reacts with NaOH solution to form Fe on the surface of the carbon material3O4Thereby realizing the purpose of magnetization. The preparation process of the biochar is complex, the cost is high, and the obtained biochar has poor adsorption performance.
Therefore, the method for simply and efficiently preparing the magnetic biochar by using the crop straws has great significance for large-scale utilization of the straws and environmental protection.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for preparing magnetic biochar by a one-step method.
The invention provides a method for preparing magnetic biochar by a one-step method, which comprises the following steps:
s1: straw pretreatment: drying and crushing plant straws, and screening particles with the particle size of 30-60 meshes for later use;
s2: iron salt impregnation: adding an iron salt solution into the straw particles in the step S1 for dipping, adjusting the pH value to 10-11 by using an alkali liquor, and then preserving heat for dipping;
s3: high-temperature pyrolysis: carrying out suction filtration and drying on the impregnated particles in the step S2, and transferring the particles to an atmosphere furnace for high-temperature pyrolysis to obtain a crude product of the magnetic biochar;
s4: and (3) post-treatment: and (4) carrying out suction filtration, cleaning and drying on the crude product of the magnetic biochar obtained by pyrolysis in the S3 to obtain a finished product of the magnetic activated carbon.
Preferably, in step S1, the plant straw is one or more of wheat straw, rice straw, corn straw and soybean straw; the drying mode is airing or drying; the water content of the dried straw is less than or equal to 10 percent.
Preferably, in step S2, the ferric salt solution is a mixed solution of one or more of ferric chloride, ferric nitrate, ferric sulfate or ferric oxalate; the alkali liquor used for adjusting the pH is one or more of potassium hydroxide or sodium hydroxide solution; the dipping temperature is 15-40 ℃, the dipping time is 0.5-12h, and the stirring is fully carried out in the dipping process.
Preferably, the concentration of iron ions in the iron salt solution is 0.01-0.05 mol/L; the concentration of the alkali liquor is 0.010-0.100 mol/L.
Preferably, in the step S3, the soaked straw particles are dried until the moisture content is less than or equal to 10%; in an anaerobic atmosphere of inert gas, the heating rate in the pyrolysis process is 10-30 ℃/min, the pyrolysis temperature is 500-1000 ℃, and the pyrolysis time is 2-6 h.
Preferably, the inert gas is one or more of nitrogen, helium, argon or carbon dioxide; the gas flow rate is 20-150 mL/min.
Preferably, in step S4, the solid-to-liquid ratio is first 1: 1-1: 3, washing the magnetic activated carbon once by using deionized water, and then using absolute ethyl alcohol according to a solid-to-liquid ratio of 1: 2-1: 5, washing once, and then drying for 1-6 h at 40-90 ℃ to obtain the magnetic biochar.
Compared with the prior art, the invention has the beneficial effects that:
(1) the crop straws are used as raw materials, a new way is provided for the resource treatment of the straws, the resource utilization level of the Chinese straws is improved, and the method has good economic value and practicability;
(2) the method can realize the preparation of the magnetic activated carbon by pyrolysis and magnetization in one step, is simple and is easy to realize large-scale production;
(3) the method can increase the porosity of the biochar by adjusting the pyrolysis temperature and improve the adsorption performance of the biochar;
(4) the magnetic activated carbon prepared by the method can be removed by a magnetic field, and the separation process is simple and efficient.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a method for preparing magnetic biochar by a one-step method sequentially comprises the following operation steps:
s1: straw pretreatment: drying the wheat straw in the sun until the water content is 9%, and screening particles with the particle size of 60-30 meshes for later use after crushing.
S2: iron salt impregnation: and (3) adding 0.03mol/L ferric chloride solution into the wheat straw particles in the step S1, adjusting the pH value to 10 by using 0.100mol/L sodium hydroxide aqueous solution, and preserving the temperature for 8 hours at 25 ℃.
S3: high-temperature pyrolysis: and (5) after the soaked wheat straw particles in the step S2 are subjected to suction filtration, drying at 80 ℃ until the moisture content is 9.5%, transferring to an atmosphere furnace, heating to 800 ℃ at a speed of 20 ℃/min under the protection of a nitrogen flow of 50mL/min, and pyrolyzing for 3 h.
S4: and (3) post-treatment: and (3) carrying out suction filtration on the crude product of the magnetic biochar obtained by pyrolysis in the S3, washing the crude product once by using 1:1 deionized water, washing the crude product once by using 1:2 absolute ethyl alcohol, and drying the crude product for 6 hours at the temperature of 60 ℃ to obtain the magnetic activated carbon.
Example 2:
a method for preparing magnetic biochar by a one-step method sequentially comprises the following operation steps:
s1: straw pretreatment: the corn straws are aired until the water content is 9.5%, and the crushed corn straws are screened to obtain particles with the particle size of 60-30 meshes for later use.
S2: iron salt impregnation: and (3) adding 0.04mol/L ferric chloride solution into the wheat straw particles in the step S1, adjusting the pH value to 10 by using 0.100mol/L sodium hydroxide aqueous solution, and preserving the temperature for 8 hours at 25 ℃.
S3: high-temperature pyrolysis: and (5) after the soaked wheat straw particles in the step S2 are subjected to suction filtration, drying at 80 ℃ until the moisture content is 9.5%, transferring to an atmosphere furnace, heating to 850 ℃ at a speed of 20 ℃/min under the protection of a nitrogen flow of 50mL/min, and pyrolyzing for 4 h.
S4: and (3) post-treatment: and (3) carrying out suction filtration on the crude product of the magnetic biochar obtained by pyrolysis in the S3, washing the crude product once by using 1:1 deionized water, washing the crude product once by using 1:2 absolute ethyl alcohol, and drying the crude product for 6 hours at the temperature of 60 ℃ to obtain the magnetic activated carbon.
Example 3:
a method for preparing magnetic biochar by a one-step method sequentially comprises the following operation steps:
s1: straw pretreatment: drying the wheat straw in the sun until the water content is 9.5%, and screening particles with the particle size of 60-30 meshes for later use after crushing.
S2: iron salt impregnation: and (3) adding 0.05mol/L ferric chloride solution into the wheat straw particles in the step S1, adjusting the pH value to 10 by using 0.100mol/L sodium hydroxide aqueous solution, and preserving the temperature for 8 hours at 25 ℃.
S3: high-temperature pyrolysis: and (5) after the soaked wheat straw particles in the step S2 are subjected to suction filtration, drying at 80 ℃ until the moisture content is 9.5%, transferring to an atmosphere furnace, heating to 850 ℃ at a speed of 20 ℃/min under the protection of a nitrogen flow of 50mL/min, and pyrolyzing for 4 h.
S4: and (3) post-treatment: and (3) carrying out suction filtration on the crude product of the magnetic biochar obtained by pyrolysis in the S3, washing the crude product once by using 1:1 deionized water, washing the crude product once by using 1:2 absolute ethyl alcohol, and drying the crude product for 6 hours at the temperature of 60 ℃ to obtain the magnetic activated carbon.
Example 4:
a method for preparing magnetic biochar by a one-step method sequentially comprises the following operation steps:
s1: straw pretreatment: drying wheat straw in the sun until the water content is 9.0%, pulverizing, and sieving to obtain particles with particle size of 60-30 meshes.
S2: iron salt impregnation: and (3) adding 0.05mol/L ferric chloride solution into the wheat straw particles in the step S1, adjusting the pH value to 10 by using 0.100mol/L sodium hydroxide aqueous solution, and preserving the temperature for 8 hours at 25 ℃.
S3: high-temperature pyrolysis: and (5) after the soaked wheat straw particles in the step S2 are subjected to suction filtration, drying at 80 ℃ until the moisture content is 9.5%, transferring to an atmosphere furnace, heating to 900 ℃ at a speed of 20 ℃/min under the protection of a nitrogen flow of 50mL/min, and pyrolyzing for 5 hours.
S4: and (3) post-treatment: and (3) carrying out suction filtration on the crude product of the magnetic biochar obtained by pyrolysis in the S3, washing the crude product once by using 1:1 deionized water, washing the crude product once by using 1:2 absolute ethyl alcohol, and drying the crude product for 6 hours at the temperature of 60 ℃ to obtain the magnetic activated carbon.
The performance of the magnetic biochar obtained by the invention is detected, a certain amount of methylene blue standard substance is taken to prepare a standard solution with the concentration of 100mg/L, 1g of the magnetic biochar prepared in the embodiment 1-4 is respectively added into 25mL of the solution, the solution is vibrated and balanced for 12 hours under the conditions of the mass at 25 ℃ and the rpm/min, a conical flask is placed above a magnet, the turbidity of the supernatant is taken after 60 seconds, the methylene blue residual concentration in the supernatant is measured by using a liquid chromatography, and after calculation, the methylene blue removal rates are respectively 85.2%, 88.1%, 88.9% and 92.4%, so that the activated carbon prepared in the embodiment 4 has the best adsorption performance.
Claims (7)
1. A method for preparing magnetic biochar by a one-step method is characterized by comprising the following steps: the operation steps are as follows in sequence:
s1: straw pretreatment: drying and crushing plant straws, and screening particles with the particle size of 30-60 meshes for later use;
s2: iron salt impregnation: adding an iron salt solution into the straw particles in the step S1 for dipping, adjusting the pH value to 10-11 by using an alkali liquor, and then preserving heat for dipping;
s3: high-temperature pyrolysis: carrying out suction filtration and drying on the impregnated particles in the step S2, and transferring the particles to an atmosphere furnace for high-temperature pyrolysis to obtain a crude product of the magnetic biochar;
s4: and (3) post-treatment: and (4) carrying out suction filtration, cleaning and drying on the crude product of the magnetic biochar obtained by pyrolysis in the S3 to obtain a finished product of the magnetic activated carbon.
2. The one-step method for preparing magnetic biochar according to claim 1, which is characterized in that: in the step S1, the plant straws are one or more of wheat straws, rice straws, corn straws and soybean straws; the drying mode is airing or drying; the water content of the dried straw is less than or equal to 10 percent.
3. The one-step method for preparing magnetic biochar according to claim 1, which is characterized in that: in the step S2, the ferric salt solution is a mixed solution of one or more of ferric chloride, ferric nitrate, ferric sulfate, or ferric oxalate; the alkali liquor used for adjusting the pH is one or more of potassium hydroxide or sodium hydroxide solution; the dipping temperature is 15-40 ℃, the dipping time is 0.5-12h, and the stirring is fully carried out in the dipping process.
4. The one-step method for preparing magnetic biochar according to claim 3, wherein the one-step method comprises the following steps: in the ferric salt solution, the concentration of ferric ions is 0.01-0.05 mol/L; the concentration of the alkali liquor is 0.010-0.100 mol/L.
5. The one-step method for preparing magnetic biochar according to claim 1, which is characterized in that: in the step S3, drying the soaked straw particles until the moisture content is less than or equal to 10%; in an anaerobic atmosphere of inert gas, the heating rate in the pyrolysis process is 10-30 ℃/min, the pyrolysis temperature is 500-1000 ℃, and the pyrolysis time is 2-6 h.
6. The one-step method for preparing magnetic biochar according to claim 5, wherein the one-step method comprises the following steps: the inert gas is one or more of nitrogen, helium, argon or carbon dioxide; the gas flow rate is 20-150 mL/min.
7. The one-step method for preparing magnetic biochar according to claim 1, which is characterized in that: in the step S4, the solid-to-liquid ratio is first 1: 1-1: 3, washing the magnetic activated carbon once by using deionized water, and then using absolute ethyl alcohol according to a solid-to-liquid ratio of 1: 2-1: 5, washing once, and then drying for 1-6 h at 40-90 ℃ to obtain the magnetic biochar.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113332973A (en) * | 2021-05-20 | 2021-09-03 | 济南大学 | Preparation method of hydrogenation catalyst |
| CN114505054A (en) * | 2022-02-17 | 2022-05-17 | 江西省水利科学院 | Preparation method and application of high-content zero-valent ferromagnetic loaded biochar |
| CN115055161A (en) * | 2022-06-20 | 2022-09-16 | 南京林业大学 | Preparation method of magnetic activated carbon, magnetic activated carbon and application thereof |
| CN115337905A (en) * | 2022-08-19 | 2022-11-15 | 重庆大学 | Nano-iron modified biochar composite material and preparation method and application thereof |
| CN115634676A (en) * | 2022-12-17 | 2023-01-24 | 王翀 | Composite environment-friendly water purifying material |
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| CN114505054A (en) * | 2022-02-17 | 2022-05-17 | 江西省水利科学院 | Preparation method and application of high-content zero-valent ferromagnetic loaded biochar |
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| CN115337905B (en) * | 2022-08-19 | 2023-09-19 | 重庆大学 | Nano-iron modified biochar composite material and preparation method and application thereof |
| CN115634676A (en) * | 2022-12-17 | 2023-01-24 | 王翀 | Composite environment-friendly water purifying material |
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