CN114106842A - Composite material for degrading polycyclic aromatic hydrocarbon in soil and preparation method and application thereof - Google Patents
Composite material for degrading polycyclic aromatic hydrocarbon in soil and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a composite material for degrading polycyclic aromatic hydrocarbon in soil and a preparation method and application thereof, and belongs to the field of agricultural environment technology polluted soil remediation materials. Carrying out high-temperature pyrolysis on the kelp residue powder to obtain biochar, modifying the biochar, mixing and adsorbing the biochar material and bacterial liquid to complete the fixation of the biochar on microorganisms, and separating to obtain a product. The biochar microbial composite material prepared by the invention is used for degrading polycyclic aromatic hydrocarbon in soil, and compared with the method of applying degrading bacteria to soil alone, the biochar microbial composite material has the advantages of better degrading effect, simple material preparation process and low cost, and realizes waste recycling.
Description
Technical Field
The invention belongs to the field of agricultural environment technology polluted soil restoration materials, and particularly relates to a composite material for degrading polycyclic aromatic hydrocarbons in soil, and a preparation method and application thereof.
Background
Polycyclic aromatic hydrocarbon is an organic pollutant widely distributed in the environment, has persistence, bioaccumulation and high toxicity of teratogenicity, carcinogenesis and mutagenesis, and researches show that polycyclic aromatic hydrocarbon finally flows into soil and can be transferred through food chains, and finally causes influence which is difficult to estimate on the ecological environment and human beings.
In-situ bioremediation has the advantages of environmental friendliness, simplicity and high efficiency, but is limited by labor cost; ectopic bioremediation, such as bioaugmentation, can reduce cost and improve bioavailability, but still needs to solve the problem that degrading bacteria are affected by indigenous microorganisms.
The immobilization technology can shield the competitive action of indigenous microorganisms and the invasion action of adverse soil conditions, thereby accelerating the removal of polycyclic aromatic hydrocarbons in soil, wherein, the adsorption method is simple and easy to implement, the conditions are mild, and the method plays an important role in the interaction of microorganisms and carriers.
The biomass material has strong adsorption capacity to persistent organic pollutants, and can be easily modified into an adsorbent serving as a carrier for fixing microorganisms due to the fact that China is a big agricultural country, the agricultural waste is extremely large in production amount and low in utilization rate.
The biochar is a porous solid material prepared by pyrolyzing waste biomass under an anoxic condition, and the surface of the biochar has a large number of polar functional groups, a special microstructure and physicochemical properties, so that the biochar has great potential in environmental pollution remediation; however, the method has the characteristics of being not fine enough in preparation process, limited in the number of surface functional groups, difficult to disperse and the like, and the characteristics of the biochar are optimized by carrying out surface modification on the biochar through some treatment means.
The biochar immobilization method adopted in the prior art is an adsorption method, and the adsorption method depends on molecular acting force of biochar and polycyclic aromatic hydrocarbon and physical adsorption of degradation bacteria, so the acting force is not firm enough and is easy to fall off.
Disclosure of Invention
The charcoal-carried microbe is an improvement on microbe applied alone, and can raise microbe concentration, raise the toxicity resistance, tolerance and reusability of single microbe, fix the dominant bacteria strain screened from natural world onto charcoal, solve the problem of degrading microbe being affected by indigenous microbe easily, raise degrading effect and degrading speed to eliminate toxic matter and thus improve the effect of original system in eliminating organic matter difficult to degrade. The biochar is prepared from the waste biomass materials, so that the cost is saved, and the waste recycling can be realized.
The invention aims to provide a composite material for degrading polycyclic aromatic hydrocarbons in soil, a preparation method and application thereof, which can adsorb polycyclic aromatic hydrocarbons in soil and degrade the polycyclic aromatic hydrocarbons by fixed microorganisms while repairing soil polycyclic aromatic hydrocarbon pollution by charcoal.
The technical scheme adopted by the invention is as follows:
a preparation method of a composite material for degrading polycyclic aromatic hydrocarbons in soil comprises the following steps:
(1) pretreating kelp residue powder, then performing high-temperature pyrolysis, grinding a pyrolysis product into powder, and sieving to obtain biochar;
(2) preparing a ferric chloride solution, mixing and stirring the ferric chloride solution and the biochar at normal temperature, centrifuging, filtering, washing, drying, performing high-temperature pyrolysis, grinding a pyrolysis product into powder, and sieving to obtain a modified kelp residue biochar material;
(3) mixing the modified kelp residue biochar material prepared in the step (2) and polycyclic aromatic hydrocarbon degrading bacteria liquid according to the weight ratio of 0.5-1 g: after inoculation with the mass-volume ratio of 50-100 mL, shake culturing is carried out on a shaking table, and then the fixation of the biochar on the microorganisms is completed;
(4) and (4) separating the biochar in the step (3) to obtain the composite material for degrading the polycyclic aromatic hydrocarbon in the soil. Further, in the above technical scheme, the polycyclic aromatic hydrocarbon degrading bacteria comprise the following components in a ratio of 1-10% v/v: 1-10% v/v: 1-10% v/v of a mixture of Stenotrophomonas maltophilia SY-1, Bacillus (Bacillus sp.) SY-2 and Ochrobactrum tritici (Ochrobactrum tritici) SY-3; the strain preservation number of the Stenotrophomonas maltophilia SY-1 is CCTCC M2020310, the strain preservation number of the Bacillus (Bacillus sp.) SY-2 is CCTCC M2020309, and the strain preservation number of the Ochrobactrum tritici (Ochrobactrum tritici) SY-3 is CCTCC M2020308.
Further, in the above technical scheme, the kelp residue powder in step (1) is degummed kelp powder; the pretreatment comprises washing with water, drying and crushing.
Further, in the technical scheme, the high-temperature pyrolysis temperature in the step (1) and the high-temperature pyrolysis temperature in the step (2) are both 400-500 ℃, and the high-temperature pyrolysis time is 1-2 hours; and (3) screening the screen in the step (1) and the step (2) to obtain the screen with the aperture of 50-150 meshes.
Further, in the technical scheme, the concentration of the ferric chloride solution in the step (2) is 2-4 mol/L, and the mixing and stirring time is 1-3 h.
Further, in the above technical scheme, the shaking table in the step (3) is shake-cultured at 30-37 ℃, the rotation speed is 150-180 r/min, and the culture time is 12-24 h.
Further, in the above technical solution, the method for separating the biochar in step (3) in step (4) includes: and (4) standing the solution obtained in the step (3), and removing the supernatant after the charcoal is precipitated.
The method specifically comprises the following steps: standing the cultured solution for 10min to precipitate biochar in the solution as much as possible, and after finishing, slightly sucking off the supernatant along the edge by using a pipette.
The composite material for degrading the polycyclic aromatic hydrocarbon in the soil is prepared according to the preparation method.
Further, in the above technical scheme, the polycyclic aromatic hydrocarbon includes benzopyrene.
An application of the composite material in degrading polycyclic aromatic hydrocarbon polluted soil.
The invention has the beneficial effects that:
the biochar microbial composite material prepared by the invention can prevent microbes from being adversely affected by the environment, avoids the factor of death of exogenous microbes caused by external conditions as far as possible, and has simple preparation process and low cost.
In addition, the charcoal has the characteristic of adsorbing polycyclic aromatic hydrocarbons in soil, and the polycyclic aromatic hydrocarbons can be degraded while adsorbing the polycyclic aromatic hydrocarbons by enriching the polycyclic aromatic hydrocarbons, so that the effective concentration of microorganisms is improved; in addition, the biochar is used as a habitat of external degrading bacteria, so that the number and activity of inoculated microorganisms are greatly increased, and the stability of microbial cells is also increased.
In addition, common agricultural waste materials are used as raw materials of the biochar, so that the cost is low, the waste recycling is realized, and the related environmental problems are solved; and the preparation condition is mild, and the operation is simple.
Drawings
FIG. 1 is SEM scanning electron micrographs of a biochar material (A) and a modified biochar material (B).
FIG. 2 shows EDS spectra of the biochar material (A) and the modified biochar material (B).
FIG. 3 is an FTIR spectrum of a biochar material and a modified biochar material.
FIG. 4 is a thermodynamic curve of the adsorption of polycyclic aromatic hydrocarbons by the composite material of the present invention.
FIG. 5 is a graph showing the adsorption kinetics of the composite material of the present invention to polycyclic aromatic hydrocarbons.
FIG. 6 is a first order kinetics fitting curve of the composite material of the present invention to benzopyrene.
FIG. 7 is a second order kinetics fitting curve of the composite material of the present invention to benzopyrene.
FIG. 8 shows the degradation rate of the composite material of the present invention to a benzopyrene solution with a mass concentration of 100mg/L at different times.
FIG. 9 shows the degradation rate of the composite material of the present invention to a benzopyrene solution with a mass concentration of 50mg/L at different times.
FIG. 10 shows the degradation rate of benzopyrene in the actual contaminated soil at different times.
Detailed Description
The following non-limiting examples will allow one of ordinary skill in the art to more fully understand the present invention, but are not intended to limit the invention in any way.
Example 1
A preparation method of a composite material for degrading polycyclic aromatic hydrocarbons in soil comprises the following steps:
(1) washing the residue powder (degummed herba Zosterae Marinae powder) with water, oven drying, pulverizing, and placing in a tubular furnace2Carrying out high-temperature pyrolysis for 1h at 450 ℃ under protection, grinding a pyrolysis product into powder, and sieving the powder with a 100-mesh sieve to obtain biochar;
(2) preparing ferric chloride into a solution to obtain a ferric chloride solution, wherein the concentration of the ferric chloride solution is 3mol/L, mixing and stirring the ferric chloride solution and the biochar obtained in the step (1) at normal temperature, centrifuging, filtering, washing, drying, and then placing the modified material in a tube furnace N2Pyrolyzing at 450 ℃ for 1h under protection, grinding the pyrolysis product into powder, and sieving with a 100-mesh sieve to obtain a modified kelp residue biochar material;
(3) mixing the modified kelp residue biochar material prepared in the step (2) with bacterial liquid according to the weight ratio of 1 g: after inoculation with the mass-volume ratio of 100mL, shake culturing is carried out for 12h on a shaking table with the culture temperature of 30 ℃ and the rotating speed of 170r/min, thus finishing the fixation of the biochar to the microorganism and obtaining the composite material capable of degrading the polycyclic aromatic hydrocarbon in the soil.
The bacterial liquid is prepared by culturing polycyclic aromatic hydrocarbon degrading bacteria in an inorganic salt culture medium for 48 hours, wherein the polycyclic aromatic hydrocarbon degrading bacteria are functional bacteria which are obtained by screening rhizosphere soil of rice planted in farmland near an oil field in a certain city of Liaoning province and take xanthomonas, bacillus and ochrobactrum as advantages.
The polycyclic aromatic hydrocarbon degrading bacteria comprise the following components in a concentration ratio of 1-10% v/v: 1-10% v/v: 1-10% v/v of narrow-leaved single-leaved malt (Stenotrophomonas maltophilia) SY-1 (strain preservation number CCTCC M2020310), Bacillus (Bacillus sp.) SY-2 (strain preservation number CCTCC M2020309) and Ochrobactrum tritici (Ochrobactrum tritici) SY-3 (strain preservation number CCTCC M2020308).
The inorganic salt culture medium comprises: using 100mL of mineral salts medium as an example, 0.56g K2HPO4·3H2O、0.17g KH2PO4、0.21g NH4Cl, 0.3g NaCl, 0.01g yeast powder and 100mL double distilled water. In addition, in order to culture the polycyclic aromatic hydrocarbon degrading bacteria, polycyclic aromatic hydrocarbon mother liquor is added into an empty bottle after sterilization, and after acetone is completely volatilized, an inorganic salt culture medium and the polycyclic aromatic hydrocarbon degrading bacteria are added into a conical bottle.
Through detection, the specific surface area of the product kelp residue modified biochar is 11.7279m2·g-1The pore volume is 0.048768cm3·g-1The pore diameter is 14.5915 nm. FIG. 1 is SEM scanning electron micrographs of a biochar material (A) and a modified biochar material (B). The biochar material is obtained in the step (1), the modified biochar material is obtained in the step (2), and the description of the biochar material and the modified biochar material is the same as that in the embodiment of the invention. As can be seen from FIG. 1, the modified biochar has a porous structure, and has smaller pores and increased number, so that the surface area of the biochar is increased, and the adsorption capacity of the biochar to benzo (a) pyrene is improved; on the other hand, the method is beneficial to the diffusion of benzopyrene in the pores of the biochar, and shortens the time required by adsorption. FIG. 2 shows EDS spectra of the biochar material (A) and the modified biochar material (B). As can be seen from FIG. 2, the spectrum of the modified biochar has increased iron element compared with the unmodified biochar, which indicates that the ferric chloride is successfully loaded on the biochar after the modification treatment. FIG. 3 is an FTIR spectrum of the biochar material (A) and the modified biochar material (B). As can be seen in FIG. 3, the modified biochar is 1116cm-1The band appeared in (A) is caused by C-O stretching vibration, and 1425cm-1Then is reacted with methyl (-CH)3) Is related to the stretching vibration of 3402cm-1The band at (A) shows a strong broad absorption peak due to stretching vibration of hydroxyl group (O-H bond), and furthermore, 564cm-1The band of (B) is mainly due to stretching vibration of Fe-O bond, which is weak or absent in FT-IR spectrum of BC, proving Fe3O4The presence of particles.
Example 2 thermodynamic curves for adsorption
The biochar material prepared in the step (1) in the example 1 is used for adsorption experiments on the water solution containing the polycyclic aromatic hydrocarbon, and the specific steps are as follows:
adding 10mL CaCl into a 30mL brown bottle2And NaN3Preparing a background solution, adding benzopyrene mother liquor to prepare 2mg/L, 6mg/L, 10mg/L, 14mg/L, 18mg/L, 22mg/L, 24mg/L, 30mg/L, 42mg/L, 50mg/L and 56mg/L benzopyrene solutions, respectively adding 0.02g of biochar material into a small brown bottle, adsorbing for 72 hours at normal temperature, transferring the solution into a centrifuge tube after finishing adsorption, centrifuging for 20min at 4500r/min, taking a supernatant, and adding the supernatant into an upper clear solutionAdding 20mL of n-hexane solution into the solution, vortex and shake for 5min, hand-hold shake for 5min, and ultrasonic treatment for 30 min. Standing for layering, collecting the upper organic layer, sampling with needle tube, filtering with 0.22 μm filter membrane to obtain water sample, measuring benzopyrene concentration in the water sample with liquid chromatography, and repeating the experiment with attached figure 4.
Fig. 4 is a thermodynamic curve of adsorption of the biochar material on the polycyclic aromatic hydrocarbon, and as can be seen from fig. 4, the adsorption capacity of the biochar material on the polycyclic aromatic hydrocarbon is increased and then decreased, and finally tends to be stable, and the maximum adsorption amount is 55.14 mg/L.
Example 3 adsorption kinetics curves
The biochar material prepared in the step (1) in the example 1 is used for adsorption experiments on the water solution containing the polycyclic aromatic hydrocarbon, and the specific steps are as follows:
adding 10mL CaCl into a 30mL brown bottle2And NaN3Preparing a background solution, adding a benzopyrene mother solution to prepare a benzopyrene solution with the mass concentration of 10mg/L, adding 0.02g of biochar material into a small brown bottle respectively, adsorbing for 15min, 30min, 45min, 60min, 120min, 240min and 360min at normal temperature, transferring the solution into a centrifuge tube after the completion of the adsorption, centrifuging for 20min at 4500r/min, taking a supernatant, adding 20mL of n-hexane solution into the supernatant, carrying out vortex oscillation for 5min, carrying out hand shaking for 5min, and carrying out ultrasound for 30 min. Standing for layering and stabilizing, collecting the upper organic layer, sampling with needle tube, filtering with 0.22 μm filter membrane to obtain water sample, measuring benzopyrene concentration in the water sample with liquid chromatography, and repeating the experiment with attached figure 5, figure 6 and figure 7.
FIG. 5 is a curve of the adsorption kinetics of the biochar material to polycyclic aromatic hydrocarbons, and it can be seen from FIG. 5 that the adsorption of the biochar material to benzopyrene is divided into a fast adsorption stage (0-45min), a slow adsorption stage (45-240min) and an equilibrium adsorption stage (240-360min), and saturated adsorption can be achieved in 240 min; fig. 6 and 7 are a first-order kinetics fitting curve and a second-order kinetics fitting curve of the biochar material to benzopyrene, which are obtained by analysis, and the adsorption of the biochar material to benzopyrene accords with the second-order kinetics curve, which shows that the adsorption of polycyclic aromatic hydrocarbon on the biochar material is mainly chemical adsorption, and pi-pi interaction of the biochar and the polycyclic aromatic hydrocarbon is caused by pi bonds in aromatic functional groups.
Example 4 degradation of polycyclic aromatic hydrocarbons in Water by biochar Material and modified biochar Material
Adding 4mL of inorganic salt culture medium and 1mL of bacterial liquid into a 20mL small brown bottle, then respectively adding benzopyrene mother liquor to prepare benzopyrene solution with the mass concentration of 100mg/L, then respectively adding 0.01g of biochar material and modified biochar material, simultaneously using a sample without biochar as a blank reference, placing the benzopyrene mother liquor on a shaking table with the culture temperature of 31 ℃ and the vibration rate of 170r/min to culture for 4d, 7d, 10d and 14d, then adding an equal-volume reagent, fully oscillating and extracting for 5min by using a vortex mixer, sampling by using a needle tube, filtering by using a 0.22 mu m filter membrane to obtain an organic sample, determining the concentration of benzopyrene in a water sample by using liquid chromatography, repeating the experiment, and obtaining the attached figure 8.
FIG. 8 shows the degradation rate of the modified biochar material to a benzopyrene solution with a mass concentration of 100mg/L at different times. As can be seen from FIG. 8, compared with the case of adding the degrading bacteria alone, the degrading effect of the charcoal material loaded with the degrading bacteria is better, and can reach 35.82% at 14d, which is 3.94% higher than that of adding the degrading bacteria alone; the degradation effect of the modified biochar material is better than that of the biochar material, and the degradation rate at 14d is improved by 5.42%.
Example 5 degradation of polycyclic aromatic hydrocarbons at different concentrations in Water by biochar Material and modified biochar Material
Adding 4mL of inorganic salt culture medium and 1mL of bacterial liquid into a 20mL small brown bottle, then respectively adding benzopyrene mother liquor to prepare a benzopyrene solution with the mass concentration of 50mg/L, then respectively adding 0.01g of biochar material and modified biochar material, simultaneously using a sample without biochar as a blank reference, placing the materials on a shaking table with the culture temperature of 31 ℃ and the vibration rate of 170r/min to culture for 4d, 7d, 10d and 14d, then adding a double-volume n-hexane reagent, fully oscillating and extracting for 5min by using a vortex mixer, sampling by using a needle tube, filtering by using a 0.22 mu m filter membrane to obtain an organic sample, measuring the concentration of benzopyrene in a water sample by using liquid chromatography, and repeating the experiment, wherein the attached figure 9 shows that the concentration of benzopyrene in the water sample is measured.
FIG. 9 shows the degradation rate of the modified biochar material to a benzopyrene solution with a mass concentration of 50mg/L at different times. As can be seen from FIG. 9, compared with the case of adding the degrading bacteria alone, the degrading effect of the charcoal material loaded with the degrading bacteria is better, and can reach 50.32% at 14d, which is 10.42% higher than that of applying the degrading bacteria alone; the degradation effect of the modified biochar material is better than that of the biochar material, and the degradation rate at 14d can reach 60.77%.
Example 6 degradation of polycyclic aromatic hydrocarbons in actual contaminated soil by biochar materials and modified biochar materials
Adding 3g of actual contaminated soil into a 20mL small brown bottle, regulating 0D to 1.0 after the degradation bacteria are centrifugally resuspended, then respectively adding 0.06g of biochar material and modified biochar material, 0.5mL of ultrapure water and 1mL of resuspended bacterial liquid into the small brown bottle, simultaneously taking a sample without biochar as a blank control, placing all samples into a constant-temperature incubator to degrade for 4D, 7D, 10D and 14D respectively, and adding 1mL of resuspended bacterial liquid every 2D in the period, so as to ensure that the total volume of the added bacterial liquid is 6 mL; using a dichloromethane/acetone 1/1 ratio mixed solution as an extracting agent, adding 5mL of the extracting agent into each sample, manually oscillating for 5min, fully oscillating and extracting for 5min by using a vortex mixer, performing ultrasonic treatment for 30min, repeating the operation for 3 times, and taking supernate; transferring the combined extract liquor to a round-bottom flask, adjusting the rotary evaporation temperature to 35 ℃ to perform a suspension evaporation experiment, adding 2mL of acetone when the organic solvent is completely volatilized, manually shaking the flask, re-extracting, sampling by using a needle tube, filtering by using a 0.22-micrometer filter membrane to obtain an organic sample, measuring the concentration of benzopyrene in a water sample by using liquid chromatography, and repeating the experiment, wherein the attached figure 10 shows that the concentration of benzopyrene in the water sample is low.
FIG. 10 shows the degradation rate of the biochar material and the modified biochar material to benzopyrene in the actual contaminated soil at different times. As can be seen from FIG. 10, compared with the method of adding the degrading bacteria alone, the degrading effect of the charcoal material loaded with the degrading bacteria is better, and can reach 76.07% in 14d, which is 17.07% higher than that of adding the degrading bacteria alone; the degradation effect of the modified biochar material is better than that of the biochar material, the degradation rate at 14d can reach 86.98%, and the degradation rate is improved by 27.98% compared with that of the biochar material which is applied alone.
Claims (10)
1. The preparation method of the composite material for degrading the polycyclic aromatic hydrocarbon in the soil is characterized by comprising the following steps:
(1) pretreating kelp residue powder, then performing high-temperature pyrolysis, grinding a pyrolysis product into powder, and sieving to obtain biochar;
(2) preparing a ferric chloride solution, mixing and stirring the ferric chloride solution and the biochar at normal temperature, centrifuging, filtering, washing, drying, performing high-temperature pyrolysis, grinding a pyrolysis product into powder, and sieving to obtain a modified kelp residue biochar material;
(3) mixing the modified kelp residue biochar material prepared in the step (2) and polycyclic aromatic hydrocarbon degrading bacteria liquid according to the weight ratio of 0.5-1 g: after inoculation with the mass-volume ratio of 50-100 mL, shake culturing is carried out on a shaking table, and then the fixation of the biochar on the microorganisms is completed;
(4) and (4) separating the biochar in the step (3) to obtain the composite material for degrading the polycyclic aromatic hydrocarbon in the soil.
2. The method of claim 1, wherein the polycyclic aromatic hydrocarbon-degrading bacteria comprises a mixture of the polycyclic aromatic hydrocarbon-degrading bacteria and the aromatic hydrocarbon-degrading bacteria in a ratio of 1-10% v/v: 1-10% v/v: 1-10% v/v of a mixture of Stenotrophomonas maltophilia SY-1, Bacillus (Bacillus sp.) SY-2 and Ochrobactrum tritici (Ochrobactrum tritici) SY-3; the strain preservation number of the Stenotrophomonas maltophilia SY-1 is CCTCC M2020310, the strain preservation number of the Bacillus (Bacillus sp.) SY-2 is CCTCC M2020309, and the strain preservation number of the Ochrobactrum tritici (Ochrobactrum tritici) SY-3 is CCTCC M2020308.
3. The production method according to claim 1, wherein the kelp residue powder in step (1) is degummed kelp powder; the pretreatment comprises washing with water, drying and crushing.
4. The preparation method according to claim 1, wherein the high-temperature pyrolysis temperature in step (1) and step (2) is 400-500 ℃, and the high-temperature pyrolysis time is 1-2 h; and (3) screening the screen in the step (1) and the step (2) to obtain the screen with the aperture of 50-150 meshes.
5. The preparation method according to claim 1, wherein the concentration of the ferric chloride solution in the step (2) is 2-4 mol/L, and the mixing and stirring time is 1-3 h.
6. The preparation method according to claim 1, wherein the shaking culture in step (3) is performed at 30-37 ℃ and at a rotation speed of 150-180 r/min for 12-24 h.
7. The method of claim 1, wherein the step (4) of separating the biochar of step (3) comprises: and (4) standing the solution obtained in the step (3), and removing the supernatant after the charcoal is precipitated.
8. The composite material for degrading polycyclic aromatic hydrocarbons in soil prepared by the preparation method of any one of claims 1 to 7.
9. The composite material of claim 8, wherein the polycyclic aromatic hydrocarbon comprises benzopyrene.
10. Use of the composite material of claim 8 or 9 for degrading polycyclic aromatic hydrocarbon contaminated soil.
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| 蒋旭涛等: "铁改性生物炭对磷的吸附及磷形态的变化特征", 《农业环境科学学报》 * |
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