CN111943200A - Preparation method of tobacco stem porous biochar - Google Patents
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- CN111943200A CN111943200A CN202010853784.8A CN202010853784A CN111943200A CN 111943200 A CN111943200 A CN 111943200A CN 202010853784 A CN202010853784 A CN 202010853784A CN 111943200 A CN111943200 A CN 111943200A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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- 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
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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Abstract
The preparation method of the bio-based tobacco stem porous carbon material has the advantages of simple preparation process, mild conditions and large-scale industrial production. The tobacco stem porous biochar prepared by the method has a large specific surface area and a rich pore structure, and the theoretical maximum adsorption capacity for rhodamine B can reach 580 mg/g. Meanwhile, the composite material has good recycling performance, the adsorption performance can be maintained to be about 90% or more for the first time after being recycled for 5 times.
Description
Technical Field
The invention relates to the technical field of carbon materials, in particular to a preparation method of tobacco stem porous biochar.
Technical Field
The tobacco planting area and the yield of China are the first in the world, and tens of thousands of tons of waste can be generated every year in the processes of harvesting and processing tobacco, so that the resource waste is caused, and the environmental pollution is also caused. But also because the planting area is wide and the yield is high, the produced tobacco waste resources such as tobacco stalks, tobacco roots, waste tobacco leaves and the like are more. Most of the tobacco waste is directly piled up in the field for composting or is disposed by burning. The method for directly piling tobacco wastes such as tobacco stalks, tobacco roots, waste tobacco leaves and the like in a tobacco field for composting has the disadvantages of bringing more harm to the tobacco field, and the tobacco wastes contain a large amount of germs and worm eggs and are easy to spread various diseases and insect pests when directly piled in the field for composting; in addition, the tobacco waste is treated by burning, so that the waste resources are not reasonably utilized, meanwhile, serious negative effects are brought to the living environment, the policy and strategy of sustainable development of the environment are not met, and even the health of human beings is threatened. Therefore, the problem of correctly processing the waste resources of the tobacco field is one of the problems to be solved in the tobacco industry and is also one of the key problems in the field of environmental protection and the field of resource recycling.
During the tobacco production and processing, a large amount of tobacco waste is generated every year. According to statistics, about 25% of leftovers such as tobacco leaves, tobacco stems, tobacco powder and the like can not be used for cigarette production and are discarded every year. If the wastes are recycled, not only can natural chemical raw materials or fuels meeting the green and sanitary standards be obtained, but also the purposes of cleaning agriculture and changing wastes into valuables can be achieved, and finally, the sustainable development of tobacco production and the dual benefits of ecological environment protection and economic benefit are realized.
The tobacco leaves contain a plurality of compounds, wherein solanesol, nicotine, protein, amino acid and the like have high utilization values. Research shows that at present, the resource utilization of waste tobacco at home and abroad is mainly to extract solanesol, nicotine, plant protein and other substances from tobacco leaves, and can also be used for preparing organic fertilizers, activated carbon, biomass fuels and the like.
The active carbon has stable chemical property and strong adsorbability, is a good adsorbent, can be used as a catalyst or a catalyst carrier, has sufficient mechanical strength and acid, heat and alkali resistance, has wide application in the aspects of chemistry, medical industry and the like, and has obvious effects in deodorization, color removal, sewage treatment and the like. At present, most of raw materials for producing activated carbon in China are wood raw materials, the carbon content of tobacco stems is more than 40%, the chemical composition is similar to that of wood, and the sources are wide. The activated carbon prepared by the tobacco stalk has good adsorption performance and can be used as commercial activated carbon. Therefore, the tobacco stalk is a high-quality raw material for manufacturing high-grade activated carbon. In addition, the residue after extracting useful components from the tobacco waste can be used for producing the activated carbon. Therefore, the comprehensive utilization efficiency is improved, the comprehensive utilization of wastes is realized, and the method has great significance in the aspects of economy and environmental protection.
The biological anatomical structure of the tobacco stems is different from that of the tobacco stems, and the research finds that the performance of the activated carbon prepared by the tobacco stems is better than that of the tobacco stems.
The invention relates to a method for comprehensively utilizing tobacco waste, which prepares biological carbon from tobacco stems by a two-step method, and can be widely applied to the environment-friendly industry of gas and liquid adsorption and other biological carbon application fields.
Disclosure of Invention
In order to utilize tobacco waste tobacco stems in a high-value mode, the invention provides a preparation method of tobacco stem porous biochar.
The purpose of the invention is realized by the following technical scheme:
a preparation method of tobacco stem porous biochar is characterized by comprising the following steps:
step (1): taking tobacco stems which are residues of tobacco processing as raw materials;
step (2): preparing the raw materials in the step (1), and crushing the raw materials into small sections of 2-5 mm;
and (3): pre-carbonizing the raw material treated in the step (2), namely putting the raw material into a tube furnace, heating to 400-700 ℃, firing for 30 minutes-3 hours at constant temperature under the protection of nitrogen, and then naturally cooling to room temperature;
and (4): adding potassium oxalate and calcium carbonate into the pre-carbonized sample obtained in the step (3), wherein the weight ratio of the pre-carbonized sample to the potassium oxalate to the calcium carbonate is 1: 0.5-2, and then mixing and grinding uniformly;
and (5): putting the mixture obtained in the step (4) into a tube furnace again, heating to 700-800 ℃ at a heating rate of 3-10 ℃/min, calcining at a constant temperature for 30 minutes-3 hours, and then naturally cooling;
and (6): and finally, soaking the sample fired in the step (5) for 2-8 hours by using 0.1-2 mol/L hydrochloric acid, filtering, washing with water, and drying to obtain the tobacco stem porous biochar product.
The invention has the following technical effects: the tobacco stem porous biochar prepared by the invention has large specific surface area and rich pore structure (shown in figure 1 and figure 2), and the theoretical maximum adsorption capacity to rhodamine B can reach 580 mg/g. Meanwhile, the adsorbent has good recycling performance, the adsorption performance can be maintained to be 90% for the first time after the adsorbent is recycled for 5 times (see figure 3).
Drawings
FIG. 1: tobacco stem biochar scanning electron microscope picture
FIG. 2 is a drawing: tobacco stem biochar nitrogen adsorption and desorption curve
Figure 3 shows the recycling capacity of tobacco stem biochar for adsorbing fuel rhodamine B
Detailed Description
Firstly, crushing tobacco stalk raw materials into small sections of 2-5 mm by using a crusher. Then weighing 10g (absolute dry basis) of tobacco stems, putting the tobacco stems into a quartz boat, putting the quartz boat into a tube furnace, and heating to 400-700 ℃ at a heating rate of 5-10 ℃. And (3) firing at constant temperature for 30 minutes to 3 hours under the protection of nitrogen for pre-carbonization, and then naturally cooling to room temperature. And then uniformly grinding the pre-carbonized samples of potassium oxalate and calcium carbonate, then putting the ground samples into a tubular furnace again, heating the ground samples to 700-800 ℃ at a heating rate of 3-10 ℃/min, calcining the ground samples at a constant temperature for 30 minutes-3 hours, and then naturally cooling the calcined samples. And finally, soaking the calcined sample in 0.1-2 mol/L hydrochloric acid for 2-8 hours, filtering, washing with water, and drying to obtain the tobacco stalk porous biochar product.
Example 1
Weighing absolutely dry 10g of tobacco stems, putting the tobacco stems into a quartz boat, placing the quartz boat in a tube furnace, and heating to 400 ℃ at a heating rate of 10 ℃. And (4) firing at constant temperature for 30 minutes under the protection of nitrogen gas for pre-carbonization, and then naturally cooling to room temperature. Then adding 3g of potassium oxalate and 4g of calcium carbonate into the pre-carbonized sample, uniformly grinding, then putting the sample into a tubular furnace again, heating to 700 ℃ at the heating rate of 10 ℃/min, calcining for 1 hour at constant temperature, and then naturally cooling. And finally, soaking the calcined sample in 0.1mol/L hydrochloric acid for 2 hours, filtering, washing with water, and drying to obtain the tobacco stalk porous biochar product. The product yield is 15.5%.
Example 2
Weighing absolutely dry 10g of tobacco stems, putting the tobacco stems into a quartz boat, placing the quartz boat in a tube furnace, and heating to 500 ℃ at a heating rate of 5 ℃. And (4) firing at constant temperature for 3 hours under the protection of nitrogen for pre-carbonization, and then naturally cooling to room temperature. Then adding 1g of potassium oxalate and 6g of calcium carbonate into the pre-carbonized sample, uniformly grinding, then putting the sample into a tubular furnace again, heating to 800 ℃ at the heating rate of 3 ℃/min, calcining at constant temperature for 30min, and then naturally cooling. And finally, soaking the calcined sample in 2mol/L hydrochloric acid for 5 hours, filtering, washing with water, and drying to obtain the tobacco stem porous biochar product. The product yield is 12.8%.
Example 3
Weighing absolutely dry 10g of tobacco stems, putting the tobacco stems into a quartz boat, placing the quartz boat in a tube furnace, and heating to 600 ℃ at a heating rate of 7 ℃. And (4) firing at constant temperature for 2 hours under the protection of nitrogen gas for pre-carbonization, and then naturally cooling to room temperature. Then 6g of potassium oxalate and 1g of calcium carbonate are added into the pre-carbonized sample, the mixture is uniformly ground and then put into a tubular furnace again to be heated to 750 ℃ at the heating rate of 5 ℃/min, and the mixture is calcined for 3 hours at constant temperature and then naturally cooled. And finally, soaking the calcined sample in 0.5mol/L hydrochloric acid for 8 hours, filtering, washing with water, and drying to obtain the tobacco stalk porous biochar product. The product yield is 13.9%.
Example 4
Weighing absolutely dry 10g of tobacco stems, putting the tobacco stems into a quartz boat, placing the quartz boat in a tube furnace, and heating to 700 ℃ at a heating rate of 7 ℃. And (4) firing at constant temperature for 1 hour under the protection of nitrogen for pre-carbonization, and then naturally cooling to room temperature. Then adding 4g of potassium oxalate and 3g of calcium carbonate into the pre-carbonized sample, uniformly grinding, then placing the sample into a tubular furnace again, heating to 800 ℃ at the heating rate of 8 ℃/min, calcining for 2 hours at constant temperature, and then naturally cooling. And finally, soaking the calcined sample in 1mol/L hydrochloric acid for 8 hours, filtering, washing with water, and drying to obtain the tobacco stem porous biochar product. The product yield is 12.5%.
Example 5
Weighing absolutely dry 10g of tobacco stems, putting the tobacco stems into a quartz boat, placing the quartz boat in a tube furnace, and heating to 600 ℃ at the heating rate of 6 ℃. And (4) firing at constant temperature for 2 hours under the protection of nitrogen gas for pre-carbonization, and then naturally cooling to room temperature. Then 6g of potassium oxalate and 5g of calcium carbonate are added into the pre-carbonized sample, the mixture is uniformly ground and then put into a tubular furnace again to be heated to 800 ℃ at the heating rate of 3 ℃/min, and the mixture is calcined for 1 hour at constant temperature and then naturally cooled. And finally, soaking the calcined sample in 2mol/L hydrochloric acid for 8 hours, filtering, washing with water, and drying to obtain the tobacco stem porous biochar product. The product yield is 14.3%.
Technical effects
The invention uses tobacco stems to prepare the activated carbon. Finally, the specific surface area, the pore structure and the adsorption of dye rhodamine B are used for evaluating the performance of the material.
The specific surface area and pore structure were determined as follows: the whole pore (specific surface area plus pore size distribution, containing mesopores and micropores) is carried out under the test mode of N2, the degassing temperature is 200 ℃, and the degassing time is 4h.
The adsorption experiment for rhodamine B is as follows: the tobacco stem biochar prepared by the method is added into 100mg/L rhodamine B solution according to the amount of 0.5g of 1L solution, the adsorption process is carried out in a gas bath constant-temperature shaking table, the temperature in the shaking table is 25 ℃, and the speed is 150 r/min. After adsorbing for a certain time, sampling, and measuring the absorbance by using an ultraviolet spectrophotometer after passing the sample solution through a 0.22 micron water system filter core.
Biochar yield, BET specific surface area 1842m in example 12Per g, average pore volume of 0.930cm3In terms of/g, the mean pore diameter is 2.31 nm. The rhodamine B adsorption speed is high, and the removal rate of 92 percent can be achieved within 30 min. The theoretical maximum adsorption capacity for rhodamine B can reach 580 mg/g. Meanwhile, the composite material has good recycling performance, the adsorption performance can be maintained to be 90% for the first time after being recycled for 5 times.
Biochar yield, BET specific surface area 1723m in example 22Per g, average pore volume of 0.850cm3In terms of a/g, the mean pore diameter is 2.15 nm. The rhodamine B adsorption speed is high, and the removal rate of 82% can be achieved within 30 min. The theoretical maximum adsorption capacity for rhodamine B can reach 526 mg/g. Meanwhile, the composite material has good recycling performance, the adsorption performance can be maintained to be 92% for the first time after being recycled for 5 times. .
Biochar yield, BET specific surface area 1780m in example 32Per g, average pore volume 0.910cm3In terms of/g, the mean pore diameter is 2.21 nm. The adsorption speed of rhodamine B is high, and the removal rate of 88 percent can be reached within 30 min. The theoretical maximum adsorption capacity for rhodamine B can reach 551 mg/g. At the same time haveGood recycling performance, 5 times of recycling, and the adsorption performance of the material can maintain 95 percent of that of the material used for the first time.
Biochar yield, BET specific surface area 1659m for example 42Per g, average pore volume 0.810cm3In terms of a/g, the mean pore diameter is 1.98 nm. The rhodamine B adsorption speed is high, and the removal rate of 92 percent can be achieved within 30 min. The theoretical maximum adsorption capacity of the rhodamine B can reach 491 mg/g. Meanwhile, the composite material has good recycling performance, the adsorption performance can be maintained to be 85% of that of the first use after being recycled for 5 times.
Biochar yield, BET specific surface area 1793m for example 52Per g, average pore volume of 0.90cm3In terms of/g, the mean pore diameter is 2.23 nm. The rhodamine B adsorption speed is high, and the removal rate of 90 percent can be reached within 30 min. The theoretical maximum adsorption capacity for rhodamine B can reach 561 mg/g. Meanwhile, the composite material has good recycling performance, the adsorption performance can be maintained to be 88% for the first time after being recycled for 5 times.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been disclosed in the above-mentioned preferred embodiments, it should be understood that the present invention is not limited thereto, and those skilled in the art can make various changes and modifications to the above-mentioned embodiments without departing from the scope of the present invention.
Claims (1)
1. A preparation method of tobacco stem porous biochar is characterized by comprising the following steps:
step (1): taking tobacco stems which are residues of tobacco processing as raw materials;
step (2): preparing the raw materials in the step (1), and crushing the raw materials into small sections of 2-5 mm;
and (3): pre-carbonizing the raw material treated in the step (2), namely putting the raw material into a tube furnace, heating to 400-700 ℃, firing for 30 minutes-3 hours at constant temperature under the protection of nitrogen, and then naturally cooling to room temperature;
and (4): and (4): adding potassium oxalate and calcium carbonate into the pre-carbonized sample obtained in the step (3), wherein the weight ratio of the pre-carbonized sample to the potassium oxalate to the calcium carbonate is 1: 0.5-2, and then mixing and grinding uniformly;
and (5): putting the mixture obtained in the step (4) into a tube furnace again, heating to 700-800 ℃ at a heating rate of 3-10 ℃/min, calcining at a constant temperature for 30 minutes-3 hours, and then naturally cooling;
and (6): and (3) finally, soaking the fired sample obtained in the step (5) for 8 hours by using 0.1mol/L hydrochloric acid, filtering, and drying to obtain the tobacco stalk porous biochar product.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112551524A (en) * | 2020-12-18 | 2021-03-26 | 广东中烟工业有限责任公司 | Tobacco stem-based graded porous carbon material and preparation method and application thereof |
| CN113145069A (en) * | 2021-03-12 | 2021-07-23 | 南京林业大学 | Preparation method of multifunctional porous biochar for dye adsorption |
| CN113318732A (en) * | 2021-07-05 | 2021-08-31 | 南京林业大学 | Palladium nanoparticle-three-dimensional activated carbon composite catalyst and preparation method and application thereof |
| CN113562728A (en) * | 2021-03-12 | 2021-10-29 | 南京林业大学 | Method for preparing activated carbon by sucrose one-pot method |
| CN113578269A (en) * | 2021-08-30 | 2021-11-02 | 南通大学 | Waste paperboard biochar for treating rhodamine B dye wastewater and preparation method and application thereof |
| CN113731374A (en) * | 2021-08-18 | 2021-12-03 | 暨南大学 | Modified tobacco straw biochar material and preparation method and application thereof |
| CN113731358A (en) * | 2021-08-18 | 2021-12-03 | 暨南大学 | Tobacco straw core biochar material and preparation method and application thereof |
| CN114146701A (en) * | 2021-12-24 | 2022-03-08 | 中国海洋大学 | Preparation method and application of nitrogen/oxygen self-doped porous biochar |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112551524A (en) * | 2020-12-18 | 2021-03-26 | 广东中烟工业有限责任公司 | Tobacco stem-based graded porous carbon material and preparation method and application thereof |
| CN113145069A (en) * | 2021-03-12 | 2021-07-23 | 南京林业大学 | Preparation method of multifunctional porous biochar for dye adsorption |
| CN113562728A (en) * | 2021-03-12 | 2021-10-29 | 南京林业大学 | Method for preparing activated carbon by sucrose one-pot method |
| CN113318732A (en) * | 2021-07-05 | 2021-08-31 | 南京林业大学 | Palladium nanoparticle-three-dimensional activated carbon composite catalyst and preparation method and application thereof |
| CN113731374A (en) * | 2021-08-18 | 2021-12-03 | 暨南大学 | Modified tobacco straw biochar material and preparation method and application thereof |
| CN113731358A (en) * | 2021-08-18 | 2021-12-03 | 暨南大学 | Tobacco straw core biochar material and preparation method and application thereof |
| CN113578269A (en) * | 2021-08-30 | 2021-11-02 | 南通大学 | Waste paperboard biochar for treating rhodamine B dye wastewater and preparation method and application thereof |
| CN114146701A (en) * | 2021-12-24 | 2022-03-08 | 中国海洋大学 | Preparation method and application of nitrogen/oxygen self-doped porous biochar |
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