CN114042435A - Method for preparing biochar by pretreating biomass through steam explosion - Google Patents

Method for preparing biochar by pretreating biomass through steam explosion Download PDF

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CN114042435A
CN114042435A CN202111295279.7A CN202111295279A CN114042435A CN 114042435 A CN114042435 A CN 114042435A CN 202111295279 A CN202111295279 A CN 202111295279A CN 114042435 A CN114042435 A CN 114042435A
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biochar
steam explosion
biomass
pyrolysis
raw material
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陈燕
贾洪玉
李霞
王羽
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Shandong Agriculture and Engineering University
Shandong Academy of Agricultural Sciences
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Shandong Agriculture and Engineering University
Shandong Academy of Agricultural Sciences
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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
    • B01J20/28054Solid 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
    • 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
    • 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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  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The invention relates to a preparation method of biochar, in particular to a method for preparing biochar by pretreating biomass through steam explosion. The method comprises the following steps: pretreating a biomass raw material; performing steam explosion on the pretreated biomass raw material; pyrolyzing the biomass raw material subjected to steam explosion at the temperature of 100-300 ℃ for 3-5 h; grinding and sieving after pyrolysis to obtain the product. The invention takes the lianas as the raw material, and after the steam explosion of the lianas, the lianas is pyrolyzed at low temperature (100-; the removal rate of the prepared biochar to methylene blue is up to 98.67%.

Description

Method for preparing biochar by pretreating biomass through steam explosion
Technical Field
The invention relates to a preparation method of biochar, in particular to a method for preparing biochar by pretreating biomass through steam explosion.
Background
Agricultural waste refers to organic matter that is discarded throughout the agricultural process, including waste produced in agricultural production and livestock and poultry farming. The agricultural waste resources are fully utilized, the added value of the agricultural waste resources is improved, a new product is developed, the industrial chain is prolonged, and the method has important economic significance and social significance.
The preparation of the biochar by taking waste as a raw material is one of the main ways of resource utilization. Chinese patent application CN113145069A discloses a preparation method of porous biochar for multifunctional dye adsorption, which comprises the following steps: step (1): taking soybean cakes which are the remainders of soybean processing as raw materials; step (2): preparing and crushing the raw materials in the step (1); and (3): loading the raw materials treated in the step (2) into a steam explosion tank, introducing 3-8 MPa of steam into the explosion tank, releasing pressure through a pulp spraying port within 1-10 minutes, allowing tobacco waste to enter a separator under the pushing of the pressure, and then naturally cooling to room temperature; and (4): adding potassium oxalate and calcium carbonate (1: 1) into the pre-carbonized sample in the step (3) in equal mass, and then grinding uniformly; and (5): putting the mixture obtained in the step (4) into a tube furnace again for 3-10 ℃ min-1The temperature rising rate is increased to 700-800 ℃, the mixture is calcined for 0.5-3 h at a constant temperature, and then the mixture is naturally cooled: and (6): and finally, soaking the fired sample obtained in the step (5) for 2-8 h by using 0.1-2 mol L-1 hydrochloric acid, filtering, washing with water, and drying to obtain the porous biochar product for adsorbing the self-doped nitrogen multifunctional dye of the bean cake.
Chinese invention patent CN109603759B discloses a modified biochar adsorbed by dye and a preparation method thereof, which comprises the following steps: A. cleaning and airing crop straws; B. adding the aired crop straws into a pulverizer to perform twice pulverization and sieving; C. adding the sieved crushed material into a pyrolysis furnace for pyrolysis, introducing nitrogen in the pyrolysis process, wherein the pyrolysis temperature is 500-700 ℃, the flow rate of the introduced nitrogen is 3-5L/min, the introduction time is 10-15 min, and the pyrolysis time is 50-60 min, and then slowly cooling to the room temperature to obtain biochar; D. adding biochar into concentrated sulfuric acid for primary oxidation, and then adding into concentrated nitric acid for mixed oxidation to obtain oxidized biochar; E. adding the oxidized biochar into a calcining furnace, continuously introducing nitrogen, and cooling to room temperature after calcining to obtain modified biochar; in the step, the calcining temperature is 400-500 ℃, the time is 30-50 min, then the temperature is reduced to 200 ℃, the temperature is kept for 30min, and then the temperature is slowly cooled to the room temperature; F. and grinding the modified biochar to obtain the modified biochar adsorbed by the dye.
Chinese patent application CN109046247A discloses a modified biomass charcoal for reinforcing adsorption of organic dye and a preparation method thereof, wherein the method comprises the following steps: (1) peeling the straws to obtain straw cores, slicing, washing, drying, crushing and sieving to obtain powder straws; (2) soaking the powder stalk in FeCl3Soaking in the solution for 1-2 h, filtering and drying to obtain soaked straws; (3) placing the impregnated straws in a nitrogen atmosphere, heating to 600 ℃ at a heating rate of 10 ℃/min, keeping for 1h, turning off heating, cooling to room temperature, and taking out to obtain iron modified biochar; (4) grinding the iron modified biochar, washing until the pH value is neutral, drying and sieving to obtain the modified biochar for strengthening the adsorption of the organic dye.
At present, reagents such as acid, alkali, oxidant and the like are mostly adopted in a preparation method of the biochar to modify materials, however, the modifying reagents can cause harm to the environment, the process steps are complex, and the improvement of the adsorption performance of the obtained biochar is limited. Therefore, a method for preparing biochar which is more green and has lower production cost is needed.
In agricultural wastes, vine plants account for a relatively large proportion; at present, no effective treatment method for preparing the biochar with high-efficiency adsorption performance by using the lianas as a main raw material exists.
Disclosure of Invention
The invention mainly aims to provide a method for preparing biochar by pretreating biomass through steam explosion, the biochar prepared by the preparation method of the invention through main steps of steam explosion, low-temperature pyrolysis and the like does not need acid-base, oxidant and the like, the adsorption performance is good, and the removal rate of dyes such as methylene blue is high. The invention provides a method for preparing biochar, which has the advantages of simple steps, environmental friendliness and low production cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for preparing biochar by pretreating biomass through steam explosion, which comprises the following steps: pretreating a biomass raw material; performing steam explosion on the pretreated biomass raw material; pyrolyzing the biomass raw material subjected to steam explosion at the temperature of 100-300 ℃ for 3-5 h; grinding and sieving after pyrolysis to obtain the product.
Further, the biomass feedstock pretreatment comprises: drying, cutting and/or pulverizing the raw materials.
Further, the steam explosion conditions are as follows: maintaining for 3-10min under 1-8 MPa.
Further, after pyrolysis and grinding, sieving with a sieve of 80-100 meshes.
Further, the biomass raw material is a vine.
The invention also provides the biochar prepared by the method.
The invention also provides application of the biochar in dye adsorption.
Further, the biochar adsorbs the dye at 25-30 ℃ under the alkaline condition.
Compared with the prior art, the invention has the following advantages:
the preparation method of the biochar mainly adopts a steam explosion and pyrolysis method, does not need to add other medicines in the whole process, avoids secondary pollution, and is a green and low-cost method.
The invention takes the lianas as the raw material, the surface of the lianas contains a large amount of active functional groups such as hydroxyl, carboxyl, ester group and the like, and the lianas has the characteristics of large specific surface area, porous structure and the like; after the steam explosion of the biochar, the loss of carboxyl, hydroxyl and other groups can be effectively prevented by adopting low-temperature (100-.
The biochar prepared by the method has a good adsorption effect on dye substances, and the removal rate of methylene blue is up to 98.67%.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a graph showing the change in the influence of different pyrolysis temperatures on the adsorption performance of biochar.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, and/or combinations thereof, unless the context clearly indicates otherwise.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1
A method for preparing biochar by pretreating biomass through steam explosion comprises the following steps:
step 1, airing balsam pear vines, and cutting the balsam pear vines into small sections;
step 2, filling the balsam pear vines processed in the step 1 into a steam explosion tank, introducing steam, discharging cold air in the tank, closing a charging valve, boosting the pressure to 1.5MPa, maintaining for 5min, opening a discharging valve, and instantly decompressing and releasing to obtain the steam exploded balsam pear vines;
step 3, subjecting the melon vine subjected to steam explosion treatment in the step 2 to pyrolysis at the temperature of 200 ℃ for 3 hours, and taking out after the pyrolysis is finished; grinding and sieving with a 100-mesh sieve to obtain the biochar.
The method for adsorbing the dye by using the biochar comprises the following steps:
adjusting the temperature of the sewage containing the dye to 25 ℃, adding the prepared biochar, adjusting the pH value of the solution to 12, and adsorbing to obtain the dye.
Example 2
A method for preparing biochar by pretreating biomass through steam explosion comprises the following steps:
step 1, airing balsam pear vines, and cutting the balsam pear vines into small sections;
step 2, filling the balsam pear vines processed in the step 1 into a steam explosion tank, introducing steam, discharging cold air in the tank, closing a charging valve, boosting the pressure to 1-2MPa, maintaining for 10min, opening a discharging valve, and instantly decompressing and releasing to obtain the steam exploded balsam pear vines;
step 3, subjecting the melon vine subjected to steam explosion treatment in the step 2 to pyrolysis at the temperature of 100 ℃ for 5 hours, and taking out after the pyrolysis is finished; grinding and sieving with a 100-mesh sieve to obtain the biochar.
The method for adsorbing the dye by using the biochar comprises the following steps:
adjusting the temperature of the sewage containing the dye to 30 ℃, adding the prepared biochar, adjusting the pH value of the solution to 11, and adsorbing to obtain the dye.
Example 3
A method for preparing biochar by pretreating biomass through steam explosion comprises the following steps:
step 1, airing balsam pear vines, and cutting the balsam pear vines into small sections;
step 2, filling the balsam pear vines processed in the step 1 into a steam explosion tank, introducing steam, discharging cold air in the tank, closing a charging valve, boosting the pressure to 8MPa, maintaining for 3min, opening a discharging valve, and instantly decompressing and releasing to obtain the balsam pear vines subjected to steam explosion;
step 3, subjecting the melon vine subjected to steam explosion treatment in the step 2 to pyrolysis at the temperature of 300 ℃ for 3 hours, and taking out after the pyrolysis is finished; grinding and sieving with a 80-mesh sieve to obtain the biochar.
The method for adsorbing the dye by using the biochar comprises the following steps:
adjusting the temperature of the sewage containing the dye to 28 ℃, adding the prepared biochar, adjusting the pH value of the solution to 8, and adsorbing to obtain the dye.
Example 4
A method for preparing biochar by pretreating biomass through steam explosion comprises the following steps:
step 1, airing the muskmelon vines, and cutting the muskmelon vines into small sections;
step 2, filling the melon vines processed in the step 1 into a steam explosion tank, introducing steam, discharging cold air in the tank, closing a material filling valve, boosting the pressure to 2MPa, maintaining for 3min, opening a material discharging valve, and instantly decompressing and releasing to obtain the melon vines subjected to steam explosion;
step 3, subjecting the melon vine subjected to steam explosion treatment in the step 2 to pyrolysis at the temperature of 250 ℃ for 3 hours, and taking out after the pyrolysis is finished; grinding and sieving with a 100-mesh sieve to obtain the biochar.
Example 5
A method for preparing biochar by pretreating biomass through steam explosion comprises the following steps:
step 1, airing luffa stems, and cutting the luffa stems into small sections;
step 2, filling the luffa stem processed in the step 1 into a steam explosion tank, introducing steam, discharging cold air in the tank, closing a charging valve, boosting the pressure to 2.5MPa, maintaining for 5min, opening a discharging valve, and instantly decompressing and releasing to obtain the luffa stem subjected to steam explosion;
step 3, subjecting the melon vine subjected to steam explosion treatment in the step 2 to pyrolysis at the temperature of 150 ℃ for 3 hours, and taking out after the pyrolysis is finished; grinding and sieving with a 100-mesh sieve to obtain the biochar.
Test examples
1. Influence of pyrolysis temperature on adsorption properties of biochar
Preparing a plurality of groups of water solutions with the methylene blue concentration of 150mg/L, and adjusting the pH value of the solution to 7. Biochar prepared at different pyrolysis temperatures (except for different pyrolysis temperatures, other steps for preparing the biochar are the same as those in example 1) is added respectively, and adsorption is carried out for 12 hours. The adsorption amounts of biochar in each group are shown in table 1 and fig. 1.
A control group is arranged in the test process, and the preparation method of the biochar of the control group comprises the following specific steps:
air drying melon vine, cutting into small sections, placing in a muffle furnace, adopting high temperature oxygen-limited pyrolysis method, carbonizing at 200 deg.C, 300 deg.C, 400 deg.C, 500 deg.C, 600 deg.C for 3h, cooling, grinding, and sieving with 100 mesh sieve.
TABLE 1
Figure BDA0003336356610000071
2. Influence of different adsorption temperatures on adsorption performance of biochar
The biochar described in example 1 was placed in aqueous solutions containing methylene blue at different concentrations at different temperatures, and the adsorption amount of the biochar is specifically shown in table 2 below.
TABLE 2
Figure BDA0003336356610000072
3. Influence of sewage with different pH values on adsorption amount of biochar
The biochar described in example 1 was placed in sewage of different pH, and the influence of the sewage of different pH on the adsorption amount of the biochar was studied. The concentration of methylene blue in the wastewater was 50mg/L, the adsorption time was 12 hours, and the results are shown in Table 3 below.
TABLE 3
Figure BDA0003336356610000081
4. The influence of different adsorption times on the adsorption performance of the biochar.
The biochar described in example 1 was placed at a methylene blue concentration of 50mg/L and a pH of 7.0 (the adsorption amounts of the biochar at different adsorption times are shown in Table 4 below).
TABLE 4
Figure BDA0003336356610000082
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (8)

1. A method for preparing biochar by pretreating biomass through steam explosion is characterized by comprising the following steps: pretreating a biomass raw material; performing steam explosion on the pretreated biomass raw material; pyrolyzing the biomass raw material subjected to steam explosion at the temperature of 100-300 ℃ for 3-5 h; grinding and sieving after pyrolysis to obtain the product.
2. The method of claim 1, wherein the biomass feedstock pretreatment comprises: drying, cutting and/or pulverizing the raw materials.
3. The method of claim 1, wherein the steam explosion conditions are: maintaining for 3-10min under 1-8 MPa.
4. The method of claim 1, wherein the pyrolysis and grinding are followed by passing through a 80-100 mesh screen.
5. The method of claim 1 or 2, wherein the biomass feedstock is a vine.
6. Biochar produced by the method of any one of claims 1 to 5.
7. Use of biochar according to claim 6 in dye adsorption.
8. The use according to claim 7, wherein the biochar adsorbs the dye under alkaline conditions at 25-30 ℃.
CN202111295279.7A 2021-11-03 2021-11-03 Method for preparing biochar by pretreating biomass through steam explosion Pending CN114042435A (en)

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