CN112093789A - Method for preparing biochar based on tea garden waste and biochar - Google Patents
Method for preparing biochar based on tea garden waste and biochar Download PDFInfo
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- C01—INORGANIC CHEMISTRY
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- C01B32/00—Carbon; Compounds thereof
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/40—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting fertiliser dosage or release rate; for affecting solubility
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- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/02—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
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- C—CHEMISTRY; METALLURGY
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- C09K2101/00—Agricultural use
Abstract
The invention discloses a method for preparing biochar from tea garden waste and biochar. The method utilizes the wastes of tea branches, tea leaves and the like obtained after pruning the tea garden as raw materials to prepare the biochar; the prepared biochar has the characteristics of high pH value, developed pore structure, large specific surface area, various element types and the like, so that the biochar has good adsorption performance, can adsorb and fix various pollutants in an environment medium of a producing area and reduce the biological effectiveness of the pollutants, and can be effectively applied to the fields of agriculture and environment to reduce potential environmental risks.
Description
Technical Field
The invention relates to the technical field of biomass resource utilization and environmental remediation. And more particularly, to a method for preparing bio-char based on tea garden waste and bio-char.
Background
The biochar is a material which is rich in carbon, fine in granularity and porous and is generated by pyrolyzing biomass at high temperature under the condition of oxygen limitation, has a surface adsorption effect, has certain effects of increasing the adsorption of soil on nutrients, reducing the emission to the atmosphere and water, reducing the pollution to the environment, improving the nutrient utilization rate and the like, and has the advantages of low price, environmental protection and the like. In addition, the biochar and the common organic fertilizer are organically combined, so that the method has the advantages of improving soil nutrients, improving the fertilizer utilization rate, stably increasing yield, reducing environmental pollution and the like, has higher research value, and has good development prospect. Therefore, the biochar material prepared from the agricultural wastes can be used as a novel, green and efficient solution technology for soil heavy metal remediation and soil fertility improvement.
At present, with the rapid development of agricultural product processing industry in China, the recycling links and modes of wastes in traditional agriculture are broken through, various problems of improper treatment of agricultural wastes, low utilization efficiency, resource waste and the like occur, excessive accumulation of a large amount of agricultural wastes also makes the agricultural wastes become important sources of ecological environment pollution, the quality of agricultural ecological environment is continuously deteriorated, the physical and mental health of people is harmed, a large amount of useful components with high added values and nutrient resources are lost, and the sustainable development capability of modern agriculture in China is greatly weakened. In the tea industry, tea waste is a general term for waste mainly containing tea biomass generated in the processes of planting, processing, deep processing, consumption and the like of tea. At present, it is estimated that pruning branches in the tea planting process can generate 5000 ten thousand tons of pruning source tea wastes per mu of China every year. However, these pruning source tea wastes are not paid attention and utilized effectively, or are piled up in tea gardens to become hotbeds for diseases and insect pests, or are discarded to cause waste of resources. The method effectively realizes the recycling, high-efficiency and comprehensive utilization and harmless treatment of the tea garden wastes, prolongs the ecological industrial chain of the tea industry, and promotes the gradient utilization of resources and energy, which is an urgent task to be solved urgently in the process of realizing the cyclic development of the tea industry.
Therefore, the application of the tea garden wastes to the preparation of the biochar material has important research values in the implementation of the circular economy concept and the improvement of the resource utilization rate and the benefit, but the difference of the internal structure of the obtained biochar material can be caused by the difference of the biomass raw materials and the preparation conditions, so that the improvement of the soil fertility and the reduction of the heavy metal pollution are obviously different. Patent CN201410120785.6 provides a method for preparing biochar based on agricultural and forestry waste, which is used for preparing biochar from rice straw, rice hull, wood dust, traditional Chinese medicine residue and peanut shell, but the method also needs to activate, wash and dry the lysate in the later period, has complicated steps, and is not suitable for preparing biochar from tea garden waste based on the microstructure specificity of tea garden waste. Therefore, the development of a method for preparing biochar which is specially suitable for tea garden waste and has simple preparation process, low cost and excellent adsorption and fixation performance is urgently needed.
Disclosure of Invention
The invention aims to provide a method for preparing biochar based on tea garden waste and biochar prepared based on the method.
The invention aims to provide the biochar prepared by the method.
The invention also aims to provide the application of the biochar in preparing a soil conditioner and/or a fertilizer slow-release product and/or a heavy metal adsorption product and/or a carbon fixation product.
In order to achieve the purpose, the invention is realized by the following scheme:
the invention provides a method for preparing biochar from tea garden wastes, which comprises the following steps:
s1, drying the tea garden waste;
s2, crushing and sieving the dried tea garden waste to obtain a powdery biomass raw material;
s3, placing the biomass raw material in a sealed pyrolysis furnace, introducing protective gas, and then performing two-stage heating treatment:
the first stage is as follows: heating from room temperature to 200-300 ℃, wherein the heating rate is 5-10 ℃/min, and the heat preservation time is 30-60 min;
and a second stage: continuously heating to 300-700 ℃ from the final temperature of the first stage, wherein the heating rate is 2-5 ℃/min, and the pyrolysis time is 1-3 h;
and S4, cooling the biomass raw material pyrolyzed in the step S3 to room temperature, and then sequentially grinding and sieving to obtain the tea garden waste biochar.
The inventor obtains the optimal preparation method of the tea garden waste biochar through a great deal of research and exploration, in the method, aiming at the specific structural characteristics of tea branches and tea leaves, the operation conditions in the cracking process are controlled, including the heating rate, the highest temperature, the pyrolysis time, the flow of protective gas, the type of a reaction furnace and the pretreatment and post-treatment methods, the obtained biochar is high in yield, high in pH value, developed in pore structure, large in specific surface area, various in element types and rich in surface functional groups, and the optimized structural characteristics can enable the biochar to have excellent adsorption performance, and can adsorb and fix various pollutants in an environmental medium and reduce the biological effectiveness. The preparation process is simple, wastes such as tea branches, tea leaves and the like obtained after pruning the tea garden are used as raw materials, the raw materials are sufficient and easily obtained, and the environment protection of the tea garden is facilitated.
Preferably, the waste of the tea garden is tea branches or tea leaves.
Further preferably, when the garden waste is tea branches, the temperature rise treatment in the second stage is 500-700 ℃ in the two-stage temperature rise treatment in the step S3; when the garden waste is tea leaves, the temperature rise in the second stage is 300-500 ℃ in the two-stage temperature rise treatment in the step S3.
Preferably, the step S2 is to sieve the crushed materials into 2-5 meshes.
Preferably, the pyrolysis furnace in step S3 is a pyrolysis carbonization furnace, a carbonization furnace or a high-temperature electric heating furnace.
Preferably, the drying treatment in step S1 is natural air drying, and then drying at 70-80 ℃ for 12-24 hours.
Most preferably, the protective gas in step S3 is nitrogen.
Preferably, the flow rate of the introduced protective gas is 2-4L/min, and the introduction time is 15-30 min.
Most preferably, the flow rate of the protective gas is 2L/min, and the flow time is 20 min.
Preferably, the step S4 is to sieve the mixture through a 50-100 mesh sieve after grinding.
The invention also claims the biochar prepared by the method. The pot experiment result shows that the biochar material prepared by the invention can obviously increase the content of organic matters in soil, improve the pH value of the soil, improve acid soil and reduce the activity of heavy metal cadmium in the soil.
The biochar can be used as a soil conditioner for practical application, can effectively relieve the acidification of cultivated soil, improves the soil fertility, improves the crop yield and quality, and reduces the heavy metal pollution risk of soil. Therefore, the invention also claims the application of the biochar in the preparation of a soil conditioner and/or a fertilizer slow-release product and/or a heavy metal adsorption product and/or a carbon fixation product.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation process of the biochar is simple, waste tea branches and tea trees are used as raw materials, and carbonization conditions are reasonably controlled based on specific structural characteristics of the tea branches and the tea leaves, so that the microstructure of the final biochar is effectively regulated and controlled, the strong adsorption effect of the biochar on organic pollutants is realized, and the fixation of the biochar on heavy metals such as cadmium, lead and the like in soil is promoted.
(2) The surface of the biochar prepared by the method has the characteristics of higher pH value, developed pore structure, larger specific surface area, various element types and the like, and the structural characteristics can ensure that the biochar has good adsorption performance, can adsorb and fix various pollutants in an environment medium of a producing area and reduce the biological effectiveness, and can be effectively applied to the agricultural and environmental fields to reduce potential environmental risks;
(3) the biochar prepared by the method can be used as a soil conditioner, effectively relieves the acidification of cultivated soil, improves the soil fertility, improves the crop yield and quality, and reduces the risk of heavy metal pollution of soil.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
EXAMPLE 1 biochar obtained by different preparation methods
1. Preparation method
S1, naturally drying the tea garden waste, and drying the tea branches at 80 ℃ for 24 hours; drying tea leaves at 70 deg.C for 12 hr;
s2, crushing the dried tea garden waste, and sieving the crushed dried tea garden waste with a 4-mesh sieve to obtain a powdery biomass raw material;
s3, placing the biomass raw material in a sealed pyrolysis carbonization furnace, introducing nitrogen at the flow rate of 2L/min for 20min, and then performing two-stage heating treatment:
the first stage is as follows: heating to T1 from room temperature at a heating rate of V1 and at a heat preservation time of K;
and a second stage: continuously heating from the final temperature of the first stage to T2 at a heating rate of V2 for a pyrolysis time of H;
s4, cooling the biomass raw material pyrolyzed in the step S3 to room temperature, and then sequentially grinding and sieving, wherein the tea branches are sieved by a 50-mesh sieve, and the tea leaves are sieved by a 100-mesh sieve, so that the tea garden waste biochar is obtained.
The temperature-raising conditions in the above embodiments are shown in tables 1 (tea branches) and 2 (tea leaves):
TABLE 1 tea Branch biochar pyrolysis conditions
TABLE 2 pyrolysis conditions of tea leaves biochar
2. Characterization analysis
The biochar materials prepared in the above examples were characterized according to the following methods.
(1) And (3) calculating the yield: after the biochar is naturally cooled, the obtained biochar mass is accurately weighed, the yield of the biochar at different pyrolysis temperatures is calculated through the following formula, and each biochar sample is subjected to parallel determination for 3 times.
Y＝M2/M1×100％
Wherein: y is charcoal yield (%); m1 is biomass raw material mass (g); m2 is the prepared biochar mass (g).
(2) And (3) determination of ash content: accurately weighing 1.0g (accurate to 0.01g) of the processed biochar, paving the biochar at the bottom of a porcelain crucible, placing the biochar in a muffle furnace in an open manner, ashing for 4 hours at 800 ℃, cooling to room temperature, taking out, weighing the mass of residues, and calculating the ash content of the biochar by using the following formula. Each charcoal sample was assayed in parallel 3 times.
A＝(M2-M1)/M×100％
In the formula: a represents the percentage content (%) of ash in the biochar; m represents the mass (g) of the biochar before burning; m1 represents the mass (g) of an empty crucible; m2 represents the mass (g) of the residue and crucible after firing.
(3) And (3) pH measurement: accurately weighing 0.5g of a biochar sample into a 15mL round-bottom centrifuge tube, adding 10mL of deionized water, placing the centrifuge tube into a constant-temperature oscillation box at 25 ℃ and continuously oscillating for 24h at 150r/min, and measuring by using a pH meter, wherein each biochar sample is measured in parallel for 3 times.
(4) Specific surface area: the determination is carried out by a full-automatic physical chemical adsorption instrument: the biochar is degassed for 24h at 105 ℃, and then the specific surface area and pore structure of the biochar are measured in a liquid nitrogen environment at 77K by using high-purity nitrogen. The specific surface area of the biochar is calculated by using multipoint Brunauer-Emmett-Teller (BET) model software carried by the instrument.
(5) Elemental analysis: and (4) determining the percentage content of each element in the sample by using an element analyzer.
The characterization results are shown in table 3:
TABLE 3 biochar characterization results
As can be seen from the results in Table 3, the pH values of the biochar prepared by the invention are alkaline; the content of C in the biochar is high; the biochar has a larger specific surface area, and can provide more adsorption sites for removing heavy metals in soil.
Example 2 biochar on Cd2+Adsorption experiment of
(1) The experimental method comprises the following steps:
testing of biochar pair Cd prepared in example 12+Adsorption kinetics of (a):
accurately weighing 0.01g of biochar to different Cd contents2+Performing oscillatory adsorption test at pH 7 and rotation speed of 150r/min in 10mL solution with concentration (20, 50, 100mg/L), sampling at different time points of 1, 3, 5, 7, 24h, etc., and determining Cd in supernatant by AAS2+And (4) concentration. Calculating the biochar pair Cd at different reaction times through an equation2+The amount of adsorption of (3).
Qt＝(C0-Ct)/M
In the formula: qt is Cd in unit mass of biochar adsorption solution at t moment2+Amount of (g/g); c0 is Cd in the initial solution2 +Concentration (mg/L); ct is Cd in solution at t moment2+Concentration (mg/L); v is the volume of the reaction solution (mL); m is the mass (g) of added biochar.
Using quasi first order kineticsMethod for adsorbing Cd by biochar at different times by quasi-second-stage kinetic model2+ fitting the data and analyzing different biochar Cd2+Adsorption kinetics of (a).
(2) Results of the experiment
The fitting parameters of the tea branch biochar adsorption kinetic model are shown in table 4:
TABLE 4 determination of charcoal adsorption kinetics of tea branches
The fitting parameters of the tea tree leaf charcoal adsorption kinetic model are shown in table 5:
TABLE 5 determination of charcoal adsorption kinetics of tea leaves
From the table 4 and the table 5, the adsorption kinetic processes of the tea tree leaves and the tea tree branches biochar on cadmium are in accordance with the quasi-first-order kinetic model, and the tea garden waste biochar material prepared by the method has excellent adsorption effect on heavy metals.
Example 3 potting experiment
(1) Experimental methods
The charcoal prepared in example 1 was subjected to potting test: the method is characterized in that standard annual tea seedlings are used as test objects, different biochar is adopted for cadmium-polluted soil to carry out improvement tests, the influences of the biochar on the cadmium element content of the soil, the soil nutrient and the pH value of the soil in the tea tree planting process are evaluated, and the influences of the biochar material on the physicochemical properties of the soil are analyzed.
(2) Results of the experiment
TABLE 6 physicochemical properties of the soil after 12 months of testing
As can be seen from the data in Table 6, the biochar prepared by the method can obviously increase the content of organic matters in soil, improve the pH value of the soil, improve acid soil and reduce the activity of heavy metal cadmium in the soil.
Comparative example 1
1. Preparation method
S1, naturally drying the tea garden waste, and drying the tea branches at 80 ℃ for 24 hours; drying tea leaves at 70 deg.C for 12 hr;
s2, crushing the dried tea garden waste, and sieving the crushed dried tea garden waste with a 4-mesh sieve to obtain a powdery biomass raw material;
s3, placing the biomass raw material in a sealed pyrolysis carbonization furnace, introducing protective gas nitrogen at the flow rate of 5L/min for 10min, and then performing two-stage heating treatment:
the first stage is as follows: heating to T1 from room temperature at a heating rate of V1 and at a heat preservation time of K;
and a second stage: continuously heating from the final temperature of the first stage to T2 at a heating rate of V2 for a pyrolysis time of H;
s4, cooling the biomass raw material pyrolyzed in the step S3 to room temperature, grinding, and sieving with a 40-mesh sieve to obtain the tea garden waste biochar.
The temperature raising conditions in each treatment group are shown in table 7.
TABLE 7
2. The biochar material prepared according to the 6-group scheme is characterized by the method of example 1, and the results are shown in table 8:
TABLE 8 biochar characterization results
From the above experiments, it can be obtained that when the pyrolysis temperature is too high, the obtained biochar has partially collapsed pore structure, reduced specific surface area, reduced pore volume, increased average pore diameter, significantly reduced yield, large loss to machine equipment, high energy consumption, and is not beneficial to production; when the pyrolysis temperature is too low, the pH value is relatively low, the specific surface area is small, the obtained tea leaf and tea branch biochar has a poor heavy metal adsorption effect, and the prepared biochar has poor effects of increasing the content of organic matters in soil, increasing the pH value of the soil and improving acid soil.
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 (10)
1. The method for preparing the biochar from the tea garden waste is characterized by comprising the following steps:
s1, drying the tea garden waste;
s2, crushing and sieving the dried tea garden waste to obtain a powdery biomass raw material;
s3, placing the biomass raw material in a sealed pyrolysis furnace, introducing protective gas, and then performing two-stage heating treatment:
the first stage is as follows: heating from room temperature to 200-300 ℃, wherein the heating rate is 5-10 ℃/min, and the heat preservation time is 30-60 min;
and a second stage: continuously heating to 300-700 ℃ from the final temperature of the first stage, wherein the heating rate is 2-5 ℃/min, and the pyrolysis time is 1-3 h;
and S4, cooling the biomass raw material pyrolyzed in the step S3 to room temperature, and then sequentially grinding and sieving to obtain the tea garden waste biochar.
2. The method of claim 1, wherein the tea garden waste is tea tree branches or leaves.
3. The method according to claim 2, wherein when the garden waste is tea tree branches, the temperature rise in the second stage is 500 to 700 ℃ in the two-stage temperature rise treatment in step S3.
4. The method according to claim 2, wherein, when the garden waste is tea leaves, the temperature raising process of step S3 is performed in two stages, and the temperature raising temperature of the second stage is 300 to 500 ℃.
5. The method according to claim 1, wherein the step S2 is carried out by sieving the crushed material with a 2-5 mesh sieve.
6. The method according to claim 1, wherein the drying treatment in step S1 is natural air drying, and then drying at 70-80 ℃ for 12-24 h.
7. The method of claim 1, wherein the protective gas in step S3 is nitrogen; the flow rate of the introduced protective gas is 2-4L/min, and the introduction time is 15-30 min.
8. The method according to claim 1, wherein the step S4 is carried out by sieving the ground material with a 50-100 mesh sieve.
9. Biochar prepared by the method of any one of claims 1 to 8.
10. Use of the biochar of claim 9 in the preparation of soil amendments and/or fertilizer slow release products and/or heavy metal adsorption products and/or carbon fixation products.
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| CN113559822A (en) * | 2021-07-28 | 2021-10-29 | 中国冶金地质总局中南地质调查院 | Preparation method and application of tea seed shell biochar |
| CN113634227A (en) * | 2021-08-17 | 2021-11-12 | 江西农业大学 | Method for preparing biochar from Nanfeng tangerine branches and application of biochar |
| CN113745509A (en) * | 2021-08-09 | 2021-12-03 | 华侨大学 | Phosphorus-nitrogen doped biomass hard carbon material and preparation method and application thereof |
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