CN114836224B - Method for preparing biochar by increasing specific surface area of biochar - Google Patents
Method for preparing biochar by increasing specific surface area of biochar Download PDFInfo
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- CN114836224B CN114836224B CN202210475379.6A CN202210475379A CN114836224B CN 114836224 B CN114836224 B CN 114836224B CN 202210475379 A CN202210475379 A CN 202210475379A CN 114836224 B CN114836224 B CN 114836224B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
- C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid 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
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/08—Non-mechanical pretreatment of the charge, e.g. desulfurization
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Abstract
The invention discloses a method for preparing biochar with an increased specific surface area, and belongs to the field of biochar preparation. Modified soil powder is doped into crushed rice straw materials and is uniformly mixed to form a mixed material, the mixed material is pyrolyzed at the lower limit oxygen pyrolysis temperature of 550-650 ℃, a pyrolysis product is cooled and is screened to remove modified soil, and modified charcoal is obtained; wherein the modified soil is laterite or loess, and the doping amount of the modified soil is 1-10 wt% of the rice straw material. The specific surface area of the modified biochar prepared by the invention is obviously increased, and the average pore diameter is obviously reduced. The biochar with larger specific surface area and abundant pore structures is beneficial to efficiently adsorbing pollutants and breeding microorganisms, and has important economic and environmental values.
Description
Technical Field
The invention belongs to the technical field of agricultural solid waste treatment, and particularly relates to a method for adjusting physical and chemical properties of biomass charcoal.
Background
The agricultural wastes in China have huge output, especially the agricultural wastes such as straws have annual output as high as hundreds of millions of tons. The straws are prepared into the biochar by a high-temperature anaerobic thermal cracking technology, and the method is a good agricultural waste treatment mode. The biochar has larger specific surface area, perfect microporous structure, higher aromatizing degree and rich oxygen-containing functional groups, is widely used in the fields of agriculture and environmental remediation, and is a green and friendly environmental functional material.
The application function of the biochar is determined by the properties of the biochar, so that the key is how to regulate the physicochemical properties of the biochar. The specific surface area and pore structure of biochar are one of the basic physical properties of biochar. The large specific surface area and the abundant pore structure are beneficial to the adsorption of the biochar to pollutants and the propagation of microorganisms. The existing method for regulating and controlling the specific surface area and the pore structure of the biochar mainly focuses on two aspects of screening of raw materials and selection of preparation temperature.
At present, the demand of the market for the biochar is increasing day by day, and how to regulate the specific surface area and the pore structure of the biochar more economically and effectively, the problem that needs to be solved by biochar production enterprises at present is urgent. For the economic and effective regulation and control of the specific surface area and the pore structure of the biochar, a new method is not available at present, and further development is needed.
Disclosure of Invention
The invention aims to solve the problem that the specific surface area and the pore structure of the biochar are difficult to regulate in the prior art, and provides a method for preparing the biochar with the increased specific surface area.
The invention adopts the following specific technical scheme:
in a first aspect, the invention provides a method for preparing biochar with an increased specific surface area, which comprises the following steps: mixing the modified soil with the crushed rice straw material to form a mixed material, carrying out lower limit oxygen pyrolysis on the mixed material at a pyrolysis temperature of 550-650 ℃, cooling a pyrolysis product, and sieving to remove the modified soil to obtain modified charcoal; wherein the modified soil is laterite or loess, and the doping amount of the modified soil is 1-10 wt% of the rice straw material.
Preferably, as for the first aspect, the modified soil is laterite, and the incorporation amount of the modified soil is preferably 10wt.% of the rice straw material.
As a preference of the first aspect, the modified soil is loess, and the amount of the modified soil added is preferably 5wt.% of the rice straw material.
As a preference of the first aspect described above, the pyrolysis temperature is preferably 650 ℃.
In the first aspect, the rice straw is preferably washed, dried, and pulverized in advance, and then passed through a 60-mesh sieve.
Preferably, in the first aspect, the modified soil powder is obtained by naturally air-drying and grinding the modified soil, and then sieving the ground modified soil powder with a 100-mesh sieve.
Preferably, the temperature rise speed of the oxygen-limited pyrolysis of the mixed material is 4-6 ℃/min, the temperature is raised to the pyrolysis temperature and then maintained for 1.5-2.5 h, and then the mixed material is naturally cooled; preferably, the heating rate of the limited-oxygen pyrolysis of the mixed material is 5 ℃/min, the temperature is maintained for 2h after the temperature is raised to the pyrolysis temperature, and then the mixed material is naturally cooled.
As a preference of the first aspect, the oxygen-limited pyrolysis of the mixed material is carried out in a tube furnace filled with an inert gas atmosphere; preferably, the inert gas is nitrogen.
As a preferable aspect of the first aspect, the pyrolysis product obtained by pyrolysis is cooled and then passed through a 100-mesh sieve to remove the modified powder, and the oversize product is collected to obtain the modified biochar.
In a second aspect, the invention provides a modified biochar prepared by the preparation method according to any one of the first aspect.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a method for simply and inexpensively regulating and controlling the specific surface area and the pore structure of biochar. In the preparation method provided by the invention, the modified biochar can be prepared by doping 1-10 wt.% of laterite or loess powder into rice straws and carrying out oxygen pyrolysis at the lower limit of pyrolysis temperature of 550-650 ℃, and the specific surface area and the average pore diameter of the modified biochar are obviously increased. The biochar with larger specific surface area and abundant pore structures is beneficial to efficiently adsorbing pollutants and breeding microorganisms, and has important economic and environmental values.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof will be described in detail with reference to the following examples. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, as those skilled in the art will recognize without departing from the spirit and scope of the present invention. The technical characteristics in the embodiments of the present invention can be combined correspondingly without mutual conflict.
The invention provides a method for preparing biochar with an increased specific surface area, which comprises the following steps: mixing the modified soil with the crushed rice straw material to form a mixed material, carrying out lower limit oxygen pyrolysis on the mixed material at a pyrolysis temperature of 550-650 ℃, cooling a pyrolysis product, and sieving to remove the modified soil to obtain modified charcoal; the modified soil is red soil or loess, and the doping amount of the modified soil is 1 wt% to 10 wt% of the rice straw material.
The modification of the biochar is mainly embodied in that the specific surface area and the pore structure of the biochar are changed, and after the biochar is mixed with the red soil or the loess for pyrolysis, compared with the pyrolysis of pure rice straw materials, the specific surface area of the modified biochar is obviously increased, and the average pore diameter is obviously reduced.
In the above-mentioned mixed materials, the corresponding doping percentages are all measured on the dry basis of the materials. Therefore, the rice straw is preferably washed, dried, crushed and sieved by a 60-mesh sieve, and the drying mode can adopt air drying or drying, and preferably the drying mode is that the rice straw is dried at the temperature of 70-80 ℃. Meanwhile, in the mixed material, the modified soil powder can be obtained by naturally drying and grinding the corresponding modified soil and sieving the ground modified soil with a 100-mesh sieve.
In addition, the oxygen-limited pyrolysis of the mixed material is carried out in a tubular furnace, the mixed material is placed in a pyrolysis boat, and the inert gas atmosphere is introduced into the tubular furnace to ensure that the material is in an oxygen-free or oxygen-deficient oxygen-limited environment during pyrolysis. In the pyrolysis process of the tubular furnace, the temperature can be raised from room temperature until reaching the pyrolysis temperature, the pyrolysis temperature is maintained for a certain time, and then the material is cooled to the room temperature after being carbonized. The inert gas melted in the furnace can adopt nitrogen. The specific heating rate or pyrolysis maintaining time can be adjusted according to actual needs. Preferably, the heating rate of the oxygen-limited pyrolysis of the mixed material is 4-6 ℃/min, the temperature is maintained for 1.5-2.5 h after being heated to the pyrolysis temperature, and then the mixed material is naturally cooled to the room temperature; further preferably, the heating rate of the oxygen-limited pyrolysis of the mixed material is 5 ℃/min, the temperature is maintained for 2h after being heated to the pyrolysis temperature, and then the mixed material is naturally cooled to the room temperature.
In addition, because the modified soil powder is added in the process of pyrolyzing the biochar, the modified soil powder needs to be removed as much as possible by screening after pyrolysis in order to avoid the influence of the modified soil powder on the properties of the final biochar finished product. Because the modified soil powder added with the mixed material is obtained by sieving with a 100-mesh sieve, the pyrolysis product obtained by pyrolysis can also be sieved with the 100-mesh sieve after being cooled to remove the modified soil powder, and the oversize product is collected to obtain the modified biochar.
It should be noted that, since the modified soil in the present invention has two types of red soil and yellow soil, it is found from the related experiments that there is a difference in the optimum blending amount for different soil types. The doping amount of the modified soil is defined as the percentage of the mass of the doped modified soil relative to the mass of the rice straw material. If the modified soil is red soil, the doping amount of the modified soil is preferably 10 wt% of that of the rice straw material, so that the optimal modification effect can be achieved, namely the maximum biochar specific surface area is achieved; if loess is selected as the modified soil, the doping amount of the modified soil is preferably 5 wt% of the rice straw material, which can achieve the best modification effect, i.e. the maximum specific surface area of the biochar.
The pyrolysis temperature of the oxygen-limited pyrolysis of the mixed material can be adjusted within the range of 550-650 ℃, the overall modification effect is good, and according to tests, the optimal modification effect can be achieved when the pyrolysis temperature is 650 ℃, namely the maximum specific surface area of the biochar is achieved.
The preparation method of the modified biochar and the corresponding technical effects are shown by a plurality of examples.
Example 1
In the embodiment, laterite is used as modified soil to adjust the specific surface area and the pore structure of the straw biochar, and the influence of different laterite incorporation amounts and different pyrolysis temperatures on the specific surface area and the pore structure of the final biochar is shown. The method comprises the following steps:
1) Washing rice straws with water to remove dust on the surface, then drying in an oven at 80 ℃, crushing the dried rice straws in a crusher, and sieving with a 60-mesh sieve to obtain the rice straw material.
2) Naturally drying the laterite, grinding, and sieving with a 100-mesh sieve to obtain laterite powder.
3) According to different material ratios, a plurality of groups of single materials or mixed materials required by different tests are formed, and the specific material ratios are as follows:
control group 1: rice straw material 2.5g (corresponding to incorporation of 0wt.% red soil)
Experimental group 1: mixing materials (0.025 g laterite powder +2.5g rice straw material, corresponding to 1wt.% laterite incorporation)
Experimental group 2: mixing materials (0.125 g laterite powder +2.5g rice straw material, corresponding to 5wt.% laterite incorporation)
Experimental group 3: mixing materials (0.25 g laterite powder +2.5g rice straw material, corresponding to 10wt.% laterite incorporation)
Experimental group 4: mixing materials (0.375 g laterite powder +2.5g rice straw material, corresponding to 15wt.% laterite incorporation)
And (3) placing the materials of the 5 groups of tests in a pyrolysis boat, then placing the materials in a tubular furnace filled with inert gas atmosphere, and carrying out calcination pyrolysis in an oxygen-free environment, wherein two groups of tests are arranged in parallel. And setting three different pyrolysis temperatures for each group of materials according to the mixture ratio, wherein the three different pyrolysis temperatures are 550 ℃, 600 ℃ and 650 ℃, the temperatures are increased from the room temperature to the corresponding pyrolysis temperatures at the heating rate of 5 ℃/min when pyrolysis starts, the pyrolysis temperatures are kept for 2 hours, and the pyrolysis products are obtained after the materials are naturally cooled to the room temperature. Pyrolysis products obtained by the 5 groups of tests at different pyrolysis temperatures respectively need to be sieved by a 100-mesh sieve to remove laterite powder, and then the biochar remained on the sieve is preserved, namely the finished laterite modified biochar.
Example 2
In this example, the difference from example 1 is that the modified soil in example 1 was replaced with loess instead of laterite, and the rest of the procedure was exactly the same as example 1. The method comprises the following steps:
in the embodiment, loess is used as modified soil to adjust the specific surface area and the pore structure of the straw biochar, and the influence of different loess doping amounts and different pyrolysis temperatures on the final specific surface area and the pore structure of the biochar is shown. The method comprises the following steps:
1) Washing rice straws with water to remove dust on the surface, then drying in an oven at 80 ℃, crushing the dried rice straws in a crusher, and sieving with a 60-mesh sieve to obtain the rice straw material.
2) Naturally air drying loess, grinding, and sieving with 100 mesh sieve to obtain loess powder.
3) According to different material ratios, a plurality of groups of single materials or mixed materials required by different tests are formed, and the specific material ratios are as follows:
control group 1: rice straw Material 2.5g (corresponding to 0wt.% loess incorporation)
Experimental group 1: mixing materials (0.025 g loess powder +2.5g rice straw material, corresponding to 1wt.% loess mixed)
Experimental group 2: mixing materials (0.125 g loess powder +2.5g rice straw material, corresponding to 5wt.% loess being doped)
Experimental group 3: mixing materials (0.25 g loess powder +2.5g rice straw material, corresponding to 10wt.% loess mixed)
Experimental group 4: mixing materials (0.375 g loess powder +2.5g rice straw material, corresponding to 15wt.% loess mixed)
And (3) placing the materials of the 5 groups of tests in a pyrolysis boat, then placing the materials in a tubular furnace with inert gas atmosphere, and carrying out calcination pyrolysis in an oxygen-free environment, wherein two groups of tests are arranged in parallel. And setting three different pyrolysis temperatures for each group of materials according to the mixture ratio, wherein the three different pyrolysis temperatures are 550 ℃, 600 ℃ and 650 ℃, the temperatures are increased from the room temperature to the corresponding pyrolysis temperatures at the heating rate of 5 ℃/min when pyrolysis starts, the pyrolysis temperatures are kept for 2 hours, and the pyrolysis products are obtained after the materials are naturally cooled to the room temperature. The pyrolysis products obtained in the above 5 tests at different pyrolysis temperatures respectively need to be sieved by a 100-mesh sieve to remove loess powder, and the biochar remained on the sieve is preserved, namely the finished loess modified biochar.
The properties of each of the laterite-modified biochar and the loess-modified biochar prepared in the above examples 1 and 2 were analyzed, the specific surface area and the pore structure of the biochar were measured using a specific surface area analyzer, and the specific surface area and the pore average pore diameter of each group of modified biochar were recorded. Wherein the specific surface area and pore size change of each of the laterite-modified biochar prepared in example 1 are shown in table 1, and the specific surface area (BET-SA) and pore size change of each of the loess-modified biochar prepared in example 2 are shown in table 2:
TABLE 1 variation of specific surface area and pore size of biochar at pyrolysis temperature and different laterite incorporation levels
TABLE 2 incorporation of loess and variation of specific surface area and pore size of biochar at pyrolysis temperature
As shown in Table 1, the addition of laterite in the range of 1 to 10wt.% has a significant effect of increasing the specific surface area of biochar and a significant effect of decreasing the average pore diameter. Therefore, the amount of laterite incorporation has a significant effect on the specific surface area of the biochar. Taking the pyrolysis temperature of 600 ℃ as an example, under the condition of adding 1%,5% and 10% of laterite, the specific surface area of the biochar is increased by 37%,28% and 89% respectively. Under the condition of adding 1 percent, 5 percent and 10 percent of laterite, the average pore diameter of the biochar is reduced by 5.1,2.7 and 4.8 nanometers respectively. But the greater the incorporation, the better, the 15wt.% laterite incorporation will cause the specific surface area of the biochar to decrease by 1% instead, increasing the average pore size by 1.1 nm. Meanwhile, the pyrolysis temperature also has influence on the specific surface area and the pore size change of the biochar, and within the range of 550-650 ℃, the higher the pyrolysis temperature is, the better the modification effect is. Therefore, for laterite as modified soil, the mixing amount is preferably 10wt.% of the rice straw material, the pyrolysis temperature is preferably 650 ℃, and the specific surface area of the biochar is increased by 116%.
Also, as shown in table 2, the addition of loess in the range of 1 to 10wt.% has a significant effect of increasing the specific surface area of the biochar and a significant effect of decreasing the average pore diameter. Therefore, the amount of loess added has a significant effect on the specific surface area of the biochar. Taking the pyrolysis temperature of 600 ℃ as an example, the specific surface area of the biochar is increased by 92%,205% and 34% respectively under the condition of adding 1%,5% and 10% of loess. The average pore diameters of biochar were reduced by 8.1, 17.6 and 0.6 nm with the addition of 1%,5% and 10% loess, respectively. However, the larger the amount of the loess is, the better, the 15wt.% of the loess will cause the specific surface area of the bio-char to be decreased by 1% conversely, and the average pore diameter to be increased by 1.1 nm. Meanwhile, the pyrolysis temperature also has influence on the specific surface area and the pore size change of the biochar, and within the range of 550-650 ℃, the higher the pyrolysis temperature is, the better the modification effect is. Therefore, for loess as modified soil, the mixing amount is preferably 5wt.% of the rice straw material, the pyrolysis temperature is preferably 650 ℃, and the specific surface area of the biochar is increased by 221%.
The above-described embodiments are merely preferred embodiments of the present invention, which should not be construed as limiting the invention. Various changes and modifications may be made by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present invention. Therefore, the technical scheme obtained by adopting the mode of equivalent replacement or equivalent transformation is within the protection scope of the invention.
Claims (12)
1. A preparation method of biochar for increasing the specific surface area of the biochar is characterized in that modified soil powder is doped into crushed rice straw materials and mixed uniformly to form a mixed material, the mixed material is subjected to lower limit oxygen pyrolysis at the pyrolysis temperature of 550-650 ℃, a pyrolysis product is cooled and then screened to remove the modified soil, and the modified biochar is obtained; wherein the modified soil is laterite or loess, and the doping amount of the modified soil is 1-10 wt% of the rice straw material.
2. The method for preparing biochar with the increased specific surface area according to claim 1, wherein the modified soil is laterite, and the doped amount of the modified soil is 10wt.% of the rice straw material.
3. The method for preparing biochar with an increased specific surface area according to claim 1, wherein the modified soil is loess, and the modified soil is incorporated in an amount of 5wt.% of the rice straw material.
4. The method for preparing biochar with an increased specific surface area of biochar as claimed in claim 2 or 3, wherein the pyrolysis temperature is 650 ℃.
5. The method for preparing biochar with an increased specific surface area according to claim 1, wherein rice straw in the mixed material is washed, dried and crushed in advance, and then is sieved through a 60-mesh sieve.
6. The method for preparing biochar with the increased specific surface area according to claim 1, wherein the modified soil powder in the mixed material is obtained by naturally air-drying and grinding modified soil, and then sieving the ground modified soil powder with a 100-mesh sieve.
7. The method for preparing biochar with an increased specific surface area according to claim 1, wherein the heating speed of limited-oxygen pyrolysis of the mixed material is 4 to 6 ℃/min, the temperature is maintained for 1.5 to 2.5 hours after the temperature is raised to the pyrolysis temperature, and then the mixed material is naturally cooled.
8. The method for preparing biochar with the increased specific surface area of the biochar as claimed in claim 7, wherein the temperature rise speed of the oxygen-limited pyrolysis of the mixed material is 5 ℃/min, the temperature is maintained for 2h after the temperature is raised to the pyrolysis temperature, and then the mixed material is naturally cooled.
9. The method for preparing biochar with an increased specific surface area according to claim 1, wherein the oxygen-limited pyrolysis of the mixed materials is carried out in a tube furnace filled with an inert gas atmosphere.
10. The method for preparing biochar with an increased specific surface area according to claim 9, wherein the inert gas is nitrogen.
11. The method for preparing biochar with an increased specific surface area according to claim 6, wherein the pyrolysis product obtained by pyrolysis is cooled and then passed through a 100-mesh sieve to remove modified soil powder, and the oversize product is collected to obtain modified biochar.
12. Modified biochar prepared by the preparation method according to any one of claims 1 to 11.
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| CN109847693A (en) * | 2018-12-17 | 2019-06-07 | 石河子大学 | A kind of bentonite modified charcoal and its preparation method and application |
| CN111018293A (en) * | 2019-12-30 | 2020-04-17 | 华南理工大学 | Device for preparing composite biochar by co-pyrolysis of sludge and biomass and use method thereof |
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| CN109847693A (en) * | 2018-12-17 | 2019-06-07 | 石河子大学 | A kind of bentonite modified charcoal and its preparation method and application |
| CN111018293A (en) * | 2019-12-30 | 2020-04-17 | 华南理工大学 | Device for preparing composite biochar by co-pyrolysis of sludge and biomass and use method thereof |
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