CN110975805A - Preparation method and application of biochar for reducing enrichment effect of vegetables on Pb (II) in soil - Google Patents

Preparation method and application of biochar for reducing enrichment effect of vegetables on Pb (II) in soil Download PDF

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CN110975805A
CN110975805A CN201911173834.1A CN201911173834A CN110975805A CN 110975805 A CN110975805 A CN 110975805A CN 201911173834 A CN201911173834 A CN 201911173834A CN 110975805 A CN110975805 A CN 110975805A
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biochar
soil
lead
vegetables
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刘淼
温泉
原帅
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Liaoning Petrochemical Vocational and Technical College
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09C—RECLAMATION OF CONTAMINATED SOIL
    • B09C1/00—Reclamation of contaminated soil
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Abstract

The invention discloses a preparation method and application of biochar for reducing enrichment effect of vegetables on Pb (II) in soil, which comprises the steps of cleaning corn straws, drying, cutting into sections, soaking in potassium hydroxide solution, carbonizing for 180min at 500-700 ℃ in an oxygen-free mode, grinding, sieving with a 100-mesh sieve, washing with deionized water to be neutral, drying, and sieving with the 100-mesh sieve to obtain modified biochar. The modified biochar applied to Pb (II) -polluted soil can obviously reduce exchangeable-state lead in the soil and increase residual-state lead so as to reduce the migration and bioavailability of Pb (II). The invention effectively utilizes the corn straws, has sufficient and easily obtained raw materials, simple modification process and strong operability; can be widely applied to micro-polluted soil, reduces the enrichment effect of vegetables on Pb (II), improves the food safety and has multiple environmental protection meanings.

Description

Preparation method and application of biochar for reducing enrichment effect of vegetables on Pb (II) in soil
Technical Field
The invention relates to a preparation method and application of biochar for reducing the enrichment effect of vegetables on Pb (II) in soil.
Background
Lead is the most well-documented toxic substance among all known toxic substances. Lead can damage the nervous system, causing peripheral neuritis, and presenting motor and sensory disturbances. In addition, lead flows into brain tissue along with blood, damages cerebellum and cerebral cortex cells, interferes with metabolic activity, causes insufficient supply of nutrients and oxygen, causes swelling of small capillary endothelial cells in brain, and further develops into diffuse brain injury. People who often contact with low-concentration lead can have headache, dizziness, fatigue, hypomnesis and insomnia when the blood lead reaches 60-80 micrograms per 100 milliliters, and the symptoms of digestive systems such as inappetence, constipation, abdominal pain and the like are often accompanied. Therefore, the control of lead pollution has attracted much attention from the whole society.
At present, the treatment of Pb (II) in water by using activated carbon has been reported, and Vanming Xia and the like disclose that the 'adsorption of Pb (II) by ammonia modified mesoporous activated carbon' disclosed in the environmental engineering bulletin (2014, 12, 8, 12 th volume) adopts NH3As a modifier, surface modification treatment is carried out on the activated carbon by NH3After reduction modification, the specific surface area and the total pore volume of the activated carbon are both slightly increased, the content of N element in the activated carbon is increased, the number of oxygen-containing functional groups is reduced, and the zero charge point is increased, so that the adsorption effect of the modified activated carbon on Pb (II) is obviously improved. The method mainly aims at the treatment of Pb (II) in the water body, and achieves the treatment purpose through adsorption. Lead can exist in different forms in polluted soil, each existing form has different influences on the ecological environment, lead existing in a residue form in the soil can stably exist, is not easy to migrate, has the minimum harm to the ecological environment, exchangeable form lead is easy to migrate, has high biotoxicity and has the maximum harm to the ecological environment, and therefore, the method is suitable for treating the water body Pb (II) and is not suitable for treating the soil for planting crops and vegetables.
Disclosure of Invention
The invention aims to provide a preparation method and application of biochar for reducing the Pb (II) enrichment effect of vegetables on soil, which reduces the bioavailability of Pb (II), is low in price and free of secondary pollution.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of biochar for reducing the Pb (II) enrichment effect of vegetables on soil comprises the following steps:
(1) cleaning and drying corn straws, cutting the corn straws into straw sections of 8cm-12cm, soaking the corn straw sections in a potassium hydroxide solution with the mass concentration of 10% for 24 hours, and drying the corn straw sections at the temperature of 60 ℃ to constant weight;
(2) carrying out anaerobic carbonization on the soaked straw sections in the step (1) for 180min at 500-700 ℃ under the protection of nitrogen, and cooling to room temperature in a furnace;
(3) and (3) grinding the biochar obtained in the step (2), sieving the biochar by a 100-mesh sieve, washing the biochar by deionized water until the biochar is neutral, drying the biochar, and sieving the biochar by the 100-mesh sieve to obtain the biochar for reducing the enrichment effect of the vegetables on Pb (II) in the soil.
Further, when the anaerobic carbonization is carried out, the carbonization temperature is 700 ℃.
Further, when the temperature in the tubular atmosphere furnace is increased, the temperature is increased at a constant speed of 10 ℃/min.
Application of biochar for reducing Pb (II) enrichment effect of vegetables on soil in reduction of Pb (II) adsorption of vegetables on soil.
The invention has the beneficial effects that:
(1) the modified corn straw biochar can obviously reduce exchangeable-state lead in soil, increase residue-state lead, and convert Pb (II) pollution to a stabilized state so as to reduce the mobility and bioavailability of Pb (II) pollution and further achieve the purpose of in-situ remediation of the polluted soil; can be widely applied to micro-polluted soil, reduces the enrichment effect of vegetables on Pb (II), and improves the food safety.
(2) The surplus corn straws in northeast regions are used for preparing the biochar, the raw materials are cheap, the modification process is simple, the operability is strong, the pollution caused by burning the straws is reduced, the straw resources can be recycled, the call of 'five actions of green development of agriculture' of Ministry of agriculture is responded, and the biochar has multiple environmental protection meanings.
Drawings
FIG. 1 is a graph showing the effect of activated carbon of examples 1 to 3 of the present invention and comparative examples 1 and 2 on lead morphology in soil;
FIG. 2 is a graph comparing the Pb (II) content of the soil-improved soil-planted crowndaisy chrysanthemum according to examples 1 to 3 of the present invention and comparative examples 1 and 2;
FIG. 3 is a graph showing the comparison of Pb (II) content in soil after potting test in activated carbon-improved soil according to examples 1 to 3 of the present invention and comparative examples 1 and 2;
FIG. 4 is a graph comparing the removal rates of activated carbon of example 1, comparative example 3 and comparative example 4 of the present invention for Pb (II).
Detailed Description
Example 1
(1) Cleaning and drying corn straws, cutting the corn straws into straw sections of 8cm-12cm, soaking the corn straw sections in a potassium hydroxide solution with the mass concentration of 10% for 24 hours, and drying the corn straw sections at the temperature of 60 ℃ to constant weight;
(2) putting the soaked straw sections in the step (1) into a tubular atmosphere furnace, filling nitrogen into the tubular atmosphere furnace, raising the temperature at a constant speed of 10 ℃/min by adopting a program, carrying out anaerobic carbonization for 180min at 700 ℃, and cooling to room temperature in the furnace;
(3) and (3) grinding the biochar obtained in the step (2), sieving the biochar by using a 100-mesh sieve, washing the biochar by using deionized water until the biochar is neutral, drying the biochar, and sieving the biochar by using a 100-mesh sieve to obtain modified corn straw biochar which is marked as KBC 700.
Comparative example 1
(1) Cleaning and drying corn straws, cutting the corn straws into straw sections of 8cm-12cm, soaking the corn straw sections in deionized water for 24 hours, and drying the corn straw sections at 60 ℃ to constant weight;
(2) putting the soaked straw sections in the step (1) into a tubular atmosphere furnace, filling nitrogen into the tubular atmosphere furnace, raising the temperature at a constant speed of 10 ℃/min by adopting a program, carrying out anaerobic carbonization for 180min at 700 ℃, and cooling to room temperature in the furnace;
(3) and (3) grinding the biochar obtained in the step (2), sieving the biochar by a 100-mesh sieve, washing the biochar by deionized water until the biochar is neutral, drying the biochar, sieving the biochar by the 100-mesh sieve to obtain modified corn straw biochar, marking as BC700, and storing the biochar in a dryer to be used as a control.
Influence of alkali modified corn stalk biochar on Pb (II) form in soil (continuous leaching experiment)
Lead exists in contaminated soil in different forms, and each form has different influences on the ecological environment. Therefore, the damage degree of lead to the ecological environment cannot be simply evaluated by the total amount of lead in the soil, and the proportion of each form of lead in the soil needs to be comprehensively considered. The influence on the lead-polluted soil can be evaluated more objectively only through the various existing morphological contents of lead in the soil. Lead existing in the soil in a residue state can exist stably, is not easy to migrate, has the minimum harm to the ecological environment, can migrate easily in an exchangeable state, has high biotoxicity and the maximum harm to the ecological environment, can be in a reduced state, is relatively stable in an oxidizable state, and can be released to cause harm to the ecological environment in the presence of certain acidity or oxidizing agents.
The BCR continuous extraction method is proposed by European Union in 1992, and has wide application in the aspect of heavy metal morphological analysis. By PbNO3Preparing a solution for a lead source, preparing lead-containing Soil of 2000mg/kg, adding water for culturing for 5-7 days/time periodically, and aging for 2 months to obtain the lead-containing Soil (Pb-Soil). And then adding BC700 and KBC respectively, and mixing uniformly, wherein the mass ratio of the biochar to the soil is 1: and 40, aging for 30 days, and determining the existence form of lead in the soil by adopting a BCR method. 2g of soil was taken for leaching analysis as shown in the following procedure.
Exchangeable state: 30mL of 0.11mol/L HAC, 25 ℃, continuously shaking for 16h, centrifuging, washing the residue with water, using the residue for the next step, and determining the Pb (II) content of the supernatant.
Reducible state: 30mL 0.1mol/L NH at pH 22OH & HCI, shaking continuously for 16h at 25 ℃, centrifuging, washing the residue with water, and then using the residue in the next step to determine the Pb (II) content of the supernatant.
Oxidizable state: 10mL of H with pH 22O2(volume fraction of 30%), heating in a thermostatic water bath at 25 deg.C for 1H, evaporating to dryness at 85 deg.C to about 2mL, and adding 10mL H2O2(8.8mol/L), heated to dryness at 85 ℃, and finally added with 30mL of 1.0mol/L ammonium acetate solution with pH 2, continuously shaken for 16h at 25 ℃, centrifuged, and the Pb (II) content of the supernatant is determined.
Residue state: total amount of lead in the soil-exchangeable-reducible-oxidizable.
Total amount of lead in soil: taking 0.2g of soil, adding 10mL of concentrated hydrochloric acid, heating and boiling to 3mL, cooling, sequentially adding 10mL of concentrated nitric acid, 5mL of hydrofluoric acid and 10mL of perchloric acid, and heating and digesting the soil at 170 ℃. And (4) after digestion is finished, adding 1mL of dilute nitric acid into the soil digestion solution, then fixing the volume to 50mL, and determining the lead concentration. And calculating the residue content by adopting a subtraction method.
Secondly, adding different kinds of active carbon into the crowndaisy chrysanthemum planted in the soil, wherein the content of Pb (II) is PbNO3As a lead source, a solution was prepared, 400mg/kg of lead-containing soil was prepared, and after culturing for 2 months with periodic addition of water, the actual lead content in the aged soil was found to be 417.65 mg/kg. Then 3kg of mixed soil is respectively added into porcelain flowerpots with the diameter of 20cm and the height of 21 cm. The soil is divided into four treatments: background Soil (Soil), lead-containing Soil (Pb-Soil), corn straw biochar lead-contaminated Soil (BC700-Pbsoil) added with 700 ℃ pyrolysis, and alkali-modified biochar lead-contaminated Soil (KBC-Pbsoil) added with alkali, wherein the mass ratio of biochar to Soil is 1: 40, aging for 30 days, and setting 5-pot parallel samples in each group. The method comprises the steps of adopting crowndaisy chrysanthemum which has proper growth cycle, does not have harsh requirements on planting environment, is common in daily market and has strong Pb (II) enrichment function as an experimental plant, carrying out pot experiment, planting for 60 days, watering for 3 times per week, and keeping the field water holding capacity at 70%. The plants were harvested 60 days after planting, washed with water and dried at 105 ℃ to constant weight. Crushing the dried crowndaisy chrysanthemum, digesting the ground crowndaisy chrysanthemum by using nitric acid and perchloric acid, and determining the content of lead.
In the lead-containing soil without the corn straw biochar, the garland chrysanthemum germinates late, the early growth is normal, but the later growth is not as good as the group added with BC700 and KBC. The adverse effect of lead on the growth of the crowndaisy chrysanthemum can be inhibited by adding the corn straw biochar into the lead-containing soil. As shown in the figure 2, in each group of crowndaisy chrysanthemum collected in the pot experiment, the lead content in the normal soil group is very low, the crowndaisy chrysanthemum is a plant which can greatly enrich Pb (II) in the lead-added soil, and the crowndaisy chrysanthemum planted in the lead-containing soil has higher lead content. After BC700 and KBC are added into the lead-containing soil, Pb (II) in the harvested crowndaisy chrysanthemum is reduced, wherein the reduction is more remarkable after the KBC is added. The corn stalk biochar is added into the lead-containing soil to inhibit the absorption of Pb (II) in the soil by the garland chrysanthemum.
Thirdly, the Pb (II) content in the soil after the pot experiment
Adding different types of activated carbon into the soil after the potted plant test of the Pb (II) content in the crowndaisy chrysanthemum planted in the soil, and detecting the total lead content in the soil by adopting a digestion method.
As can be seen from FIG. 3, after the potting experiment, the content of Pb (II) in the leaded soil without biochar is significantly lower than that of the leaded soil with biochar, because during the potting experiment, the lead in the soil is removed by the enrichment and transpiration of the garland chrysanthemum, and the lead content in the soil with biochar from corn stalks is less reduced than that before the potting experiment (417.65mg/kg), which indicates that the BC700 and KBC can improve the stability of Pb in the leaded soil and reduce the migration of Pb in the natural world. Therefore, the modified corn straw biochar can be applied to slightly polluted agricultural land, and the safety of vegetables is improved on the premise of not stopping planting.
As mentioned above, the preparation method of the biochar and the method for removing Pb (II) in soil by the biochar can obviously reduce exchangeable-state lead in soil, increase residual-state lead and play an important role in promoting the fixation and stabilization of lead. The corn straw biochar is added into the lead-containing soil, so that the adverse effect of lead on the growth of the crowndaisy chrysanthemum can be inhibited, and the intake of the crowndaisy chrysanthemum on the lead in the soil is inhibited; the biochar has the advantages of low-cost raw materials and simple preparation process, can be widely applied to micro-polluted soil, can carry out in-situ remediation on Pb (II) pollution in the soil, and improves the safety of crops.
Example 2
(1) Cleaning and drying corn straws, cutting the corn straws into straw sections of 8cm-12cm, soaking the corn straw sections in a potassium hydroxide solution with the mass concentration of 10% for 24 hours, and drying the corn straw sections at the temperature of 60 ℃ to constant weight;
(2) putting the soaked straw sections in the step (1) into a tubular atmosphere furnace, filling nitrogen into the tubular atmosphere furnace, raising the temperature at a constant speed of 10 ℃/min by adopting a program, carrying out anaerobic carbonization for 180min at the temperature of 600 ℃, and cooling to room temperature in the furnace;
(3) and (3) grinding the biochar obtained in the step (2), sieving the biochar by using a 100-mesh sieve, washing the biochar by using deionized water until the biochar is neutral, drying the biochar, and sieving the biochar by using a 100-mesh sieve to obtain modified corn straw biochar which is marked as KBC 600.
Example 3
(1) Cleaning and drying corn straws, cutting the corn straws into straw sections of 8cm-12cm, soaking the corn straw sections in a potassium hydroxide solution with the mass concentration of 10% for 24 hours, and drying the corn straw sections at the temperature of 60 ℃ to constant weight;
(2) putting the soaked straw sections in the step (1) into a tubular atmosphere furnace, filling nitrogen into the tubular atmosphere furnace, raising the temperature at a constant speed of 10 ℃/min by adopting a program, carrying out anaerobic carbonization for 180min at the temperature of 500 ℃, and cooling to room temperature in the furnace;
(3) and (3) grinding the biochar obtained in the step (2), sieving the biochar by using a 100-mesh sieve, washing the biochar by using deionized water until the biochar is neutral, drying the biochar, and sieving the biochar by using a 100-mesh sieve to obtain modified corn straw biochar which is marked as KBC 500.
Comparative example 2
(1) Cleaning and drying corn straws, cutting the corn straws into straw sections of 8cm-12cm, soaking the corn straw sections in a potassium hydroxide solution with the mass concentration of 10% for 24 hours, and drying the corn straw sections at the temperature of 60 ℃ to constant weight;
(2) putting the soaked straw sections in the step (1) into a tubular atmosphere furnace, filling nitrogen into the tubular atmosphere furnace, raising the temperature at a constant speed of 10 ℃/min by adopting a program, carrying out anaerobic carbonization for 180min at the temperature of 400 ℃, and cooling to room temperature in the furnace;
(3) and (3) grinding the biochar obtained in the step (2), sieving the biochar by using a 100-mesh sieve, washing the biochar by using deionized water until the biochar is neutral, drying the biochar, and sieving the biochar by using a 100-mesh sieve to obtain modified corn straw biochar which is marked as KBC 400.
The results of the BCR continuous leaching are shown in fig. 1, and the prepared aged soil has lead mainly existing in exchangeable state and then in residue state, and the exchangeable state, the reduced state, the oxidizable state and the residue state respectively account for 68.27%, 9.80%, 6.19% and 15.74% of the total lead in turn. After the corn stalk biochar BC700 is added, the exchangeable state quantity of lead is reduced to 40.65 percent of the total quantity of lead, and the residue state content is increased to 35.77 percent. After the KBC 400-700 series biochar is added, the exchangeable state quantity of lead in the lead-containing soil is reduced from 65.27% to 53.11%, 37.85%, 25.85% and 15.33% in sequence, and the residue state quantity is increased from 15.74% to 22.42%, 36.51%, 48.55% and 56.32% in sequence. Therefore, several biochar can promote the passivation of lead in the lead-containing soil from an exchangeable state to a residue state, wherein the KBC700 has the best effect.
As shown in the figure 2, in each group of crowndaisy chrysanthemum collected in the pot experiment, the lead content in the normal soil group is very low, the crowndaisy chrysanthemum is a plant which can greatly enrich Pb (II) in the lead-added soil, and the crowndaisy chrysanthemum planted in the lead-containing soil has higher lead content. After BC700 and KBC 400-700 series biochar are added into lead-containing soil, Pb (II) in the harvested crowndaisy chrysanthemum is reduced, wherein the reduction is more remarkable after the KBC700 is added. The corn stalk biochar is added into the lead-containing soil to inhibit the absorption of Pb (II) in the soil by the garland chrysanthemum.
As can be seen from FIG. 3, after the potting experiment, the content of Pb (II) in the leaded soil without biochar is significantly lower than that of the leaded soil with biochar, because in the process of the potting experiment, the lead in the soil can be migrated out through the enrichment effect and the transpiration effect of the garland chrysanthemum, and the lead content in the soil with biochar from corn stalks is less reduced than that before the potting experiment (417.65mg/kg), which indicates that the biochar of BC700 and KBC 400-700 series can improve the stability of Pb in the leaded soil and reduce the migration of Pb in the nature, and the stabilizing effect of KBC700 is significantly higher than that of other biochar.
Comparative example 3 preparation of nitric acid modified corn stalk biochar
The BC700 is put into a nitric acid solution with the mass concentration of 20% (the solid-to-liquid ratio is 1: 10), intermittently shaken for 24h at the temperature of 60 ℃, filtered, washed by distilled water for a plurality of times until the pH value is about 7, and put into a vacuum drying oven with the temperature of 105 ℃ for drying for 48h, which is marked as NBC.
Comparative example 4 preparation of Sulfur-adding modified corn stalk biochar
Adding the BC700 into Na with the mass concentration of 3%2Soaking in S solution (solid-to-liquid ratio of 1: 100) at 60 deg.C for 24 hr, stirring intermittently, shaking at 60 deg.C for 2 hr, drying, heating to 700 deg.C at 5 deg.C/min in a tubular furnace under nitrogen atmosphere of 350mL/min, roasting for 2 hr, cooling to room temperature, washing with distilled water to neutrality, and cooling to 10 deg.CAnd drying in a drying oven at 5 ℃ for 48h, and recording as SBC.
Preparing lead nitrate solution with Pb (II) concentration of 50mg/L by removing Pb (II) from corn straw biochar and different modified corn straw biochar in water, respectively filling 50mL of solution into sealed glass conical bottles, respectively adding about 0.1g of the modified corn straw biochar and BC700 and background electrolyte NaNO into the solution3Has a concentration of 0.01 mol.L-1With dilute HNO3And NaOH is used for adjusting the pH value of the solution to be 6.8, the solution is oscillated for 24 hours at the rotating speed of 100r/min in a water bath at the temperature of 25 ℃, supernatant liquid is taken for measuring the concentration of metal Pb (II), and the removal rates of the modified corn straw biochar of the example 1, the comparative example 3 and the comparative example 4 and the biochar of the comparative example 1 to the water body Pb (II) are calculated, and are shown in figure 4.
The removal effect of the three modified corn stalk biochar NBC, SBC, KBC and BC700 on Pb (II) in the aqueous solution is shown in figure 4. Under the same adsorption condition, the removal rate of NBC and SBC to Pb (II) exceeds BC700 after 24h, which can reach 94.61% and 87.22%, while the removal rate of alkali-modified KBC to Pb (II) is greatly reduced to 60.58% compared with BC 700. Therefore, the alkali modified corn stalk biochar is only suitable for treating Pb (II) in soil, and therefore, the alkali modified corn stalk biochar is not suitable for removing Pb (II) in aqueous solution.
The above description is only exemplary of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (4)

1. A preparation method of biochar for reducing the Pb (II) enrichment effect of vegetables on soil is characterized by comprising the following steps:
(1) cleaning and drying corn straws, cutting the corn straws into straw sections of 8cm-12cm, soaking the corn straw sections in a potassium hydroxide solution with the mass concentration of 10% for 24 hours, and drying the corn straw sections at the temperature of 60 ℃ to constant weight;
(2) carrying out anaerobic carbonization on the soaked straw sections in the step (1) for 180min at 500-700 ℃ under the protection of nitrogen, and cooling to room temperature in a furnace;
(3) and (3) grinding the biochar obtained in the step (2), sieving the biochar by a 100-mesh sieve, washing the biochar by deionized water until the biochar is neutral, drying the biochar, and sieving the biochar by the 100-mesh sieve to obtain the biochar for reducing the enrichment effect of the vegetables on Pb (II) in the soil.
2. The method for preparing biochar for reducing the Pb (II) enrichment effect of vegetables on soil as claimed in claim 1, wherein the carbonization temperature is 700 ℃ during anaerobic carbonization.
3. The method for preparing biochar for reducing the Pb (II) enrichment effect of vegetables on soil according to claim 1, wherein the temperature is uniformly increased at a speed of 10 ℃/min when the temperature is increased in a tubular atmosphere furnace.
4. Use of biochar as claimed in claim 1 for reducing adsorption of pb (ii) in soil by vegetables.
CN201911173834.1A 2019-11-26 2019-11-26 Preparation method and application of biochar for reducing enrichment effect of vegetables on Pb (II) in soil Pending CN110975805A (en)

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