CN113056981A - Method for inhibiting release of polycyclic aromatic hydrocarbons in bottom mud of rice and crab co-culture rice field by using rice straw biochar - Google Patents
Method for inhibiting release of polycyclic aromatic hydrocarbons in bottom mud of rice and crab co-culture rice field by using rice straw biochar Download PDFInfo
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Abstract
A method for inhibiting the release of polycyclic aromatic hydrocarbons in bottom mud of a rice and crab co-farming rice field by using rice straw biochar relates to a method for inhibiting the release of polycyclic aromatic hydrocarbons in soil polluted by medium and light polycyclic aromatic hydrocarbons. The invention aims to solve the problem that polycyclic aromatic hydrocarbons in bottom sediment are released and migrated to the overlying water due to crab biological disturbance in a rice-crab co-farming system. The method comprises the following steps: the rice straw biochar is used as an inhibitor to be applied to the bottom sediment of the rice and crab co-culture rice field with moderate and mild polycyclic aromatic hydrocarbon pollution. The advantages are that: first, the bottom sludge contaminants adsorb to the biochar particles, reducing the flux of released contaminants to the overlying water and surrounding areas. And secondly, the environmental pollution is reduced, the sustainable utilization of soil resources is promoted, and the method conforms to the idea of circular economy and the principle of 'treating waste by waste'. And thirdly, the effects of improving soil, enhancing the soil water retention capacity and promoting the growth and development of crops are achieved. The method is mainly used for inhibiting the release of the polycyclic aromatic hydrocarbons in the bottom mud of the rice and crab co-farming paddy field polluted by medium and light polycyclic aromatic hydrocarbons.
Description
Technical Field
The invention relates to a method for inhibiting the release of polycyclic aromatic hydrocarbon in soil polluted by medium and light polycyclic aromatic hydrocarbon.
Background
The Heilongjiang province is one of three famous black soil zones in the world, the soil has high organic matter content, the land conditions are at the top of the whole country, and meanwhile, the Heilongjiang province is one of typical cold areas in China, the climate of the Heilongjiang province is temperate continental monsoon climate, the frost-free freezing period in the whole year is between 100 and 150 days, the average temperature in the year is between 5 ℃ below zero and 5 ℃, the winter is long, the temperature difference between day and night is obvious, and the temperature of the bottom mud and the soil in the rice field is low, so that a plurality of cold area planting technologies are born, wherein the rice and crab co-working technology in the comprehensive planting mode of the rice field is used as a novel ecological agricultural technology, the development in the Heilongjiang province is rapid.
Polycyclic aromatic hydrocarbon is a persistent organic pollutant with strong toxicity and widely existing in soil, and has great harm to ecological environment and human health. In the rice and crab co-farming system, polycyclic aromatic hydrocarbons can enter a food chain through a series of ways such as soil-water-plant, soil-water-animal and the like, and finally harm human health and ecological safety, so that the inhibition of the release of the polycyclic aromatic hydrocarbons in the bottom sediment of the rice field in the rice and crab co-farming system under the condition of northeast cold regions is an important means for reducing ecological risks and environmental pollution, and has important significance for reducing the ecological risks of farmland systems in northeast alpine regions, developing green agriculture and guaranteeing food safety.
Disclosure of Invention
The invention aims to solve the problem of polycyclic aromatic hydrocarbon in bottom sediment of a rice and crab co-farming system that is released and migrated upwards due to crab biological disturbance, and provides a method for inhibiting polycyclic aromatic hydrocarbon release in bottom sediment of a rice and crab co-farming rice field by using rice straw biochar.
A method for inhibiting the release of polycyclic aromatic hydrocarbons in bottom mud of a rice and crab co-culture rice field by using rice straw biochar is specifically completed according to the following steps:
the method is characterized in that rice straw biochar is used as an inhibitor to be applied to bottom mud of a medium-light polycyclic aromatic hydrocarbon-polluted rice and crab co-farming rice field, and the application amount of the inhibitor is 1000 kg/mu-1500 kg/mu.
Further, if rice straw biochar is continuously applied to the same moderate and light polycyclic aromatic hydrocarbon-polluted rice and crab co-culture rice field for multiple years to serve as an inhibitor, the application amount of the inhibitor in the first year is 1000 kg-1500 kg/mu, the application amount of the inhibitor in the second year is 600 kg-1000 kg/mu, the application amount of the inhibitor in the third year is 300 kg/mu-500 kg/mu, and the application amount of the inhibitor in each year from the fourth year is 300 kg/mu.
The principle and the advantages of the invention are as follows:
the polycyclic aromatic hydrocarbon in the bottom mud of the rice field can diffuse and pollute the surrounding area along with water flow after migrating to overlying water, and simultaneously enters the human body through a food chain to destroy the ecological environment and harm the health of the human body, while the biomass charcoal is a porous solid granular substance which is generated by high-temperature cracking of carbon-rich biomass under the anaerobic or anoxic condition, has a rich pore structure and a larger specific surface area, is highly aromatic and is rich in carbon, and is a multifunctional material. After the biomass carbon is added into the bottom sediment, the adsorption of bottom sediment pollutants to the biomass carbon particles can be effectively promoted due to the large specific surface area and adsorption performance of the biomass carbon, so that organic pollutants (polycyclic aromatic hydrocarbons, such as phenanthrene) in the environment are fixed, the flux of pollution released by the organic pollutants to the overlying water and surrounding areas is reduced, the enrichment of polycyclic aromatic hydrocarbons by rice and crabs in a rice and crab co-working system is further reduced, the environmental pollution is reduced, and the food safety is guaranteed.
Secondly, as a big agricultural country in China, the total grain yield in the whole country in 2020 is 13390 jin, the yield is kept above 1.3 trillion jin for 6 consecutive years, meanwhile, as a byproduct in the grain production process, crop straws are increased along with the increase of the grain yield, the total amount of various crop straws per year can reach 10.4 million tons, wherein the rice straws account for 22.44 percent of the total amount of the crop straws, as the rural living standard is improved, the specific gravity of the rice straws and the like used as living fuel is greatly reduced, so that most of the rice straws are directly discarded after being burnt, and the direct burning of the straws not only can generate a large amount of various harmful gases such as CO, nitric oxide, polycyclic aromatic hydrocarbon and the like, but also can damage the soil structure, change the physical properties of the soil, damage the soil fertility and cause the quality reduction of farmlands, and the rice straws are prepared into the rice straw biochar adsorbing material through a unique treatment mode, can reduce environmental pollution, promote the sustainable utilization of soil resources, and accord with the idea of circular economy and the principle of 'treating waste by waste'.
And meanwhile, as the inside of the charcoal contains a large amount of carbon and plant nutrients, the charcoal has a good fixing effect on carbon and nitrogen, and can promote a stable carbon library when added into the soil, thereby playing roles in improving the soil, enhancing the water retention capacity of the soil and promoting the growth and development of crops.
Drawings
FIG. 1 is an SEM image of rice straw biochar of experiment group 1 at 1000 times;
FIG. 2 is an SEM image of 3000 times of rice straw biochar in experimental group 1;
FIG. 3 is a SEM image of rice straw biochar in experimental group 1 at 5000 times;
FIG. 4 is a graph showing the adsorption effect of rice straw biochar, wherein B is a curve of the amount of added rice straw biochar per unit adsorption amount, and A is a curve of the amount of added rice straw biochar per unit adsorption rate;
FIG. 5 is a photograph of a microcosm object constructed by Experimental group 6;
FIG. 6 is a photograph of the overwater physical object taken at 6h in experimental group 6;
FIG. 7 is a photograph of the blank control group 2 taken at 6h with an overlying water object;
FIG. 8 is a graph showing the change in Total Suspended Solids (TSS) content in overburden water of an attapulgite control group, wherein A represents the change in Total Suspended Solids (TSS) content in overburden water of an experimental group 6, B represents the change in Total Suspended Solids (TSS) content in overburden water of a blank control group 2, and C represents the change in Total Suspended Solids (TSS) content in overburden water of a blank control group 2;
FIG. 9 is a bar graph showing the change of the content of phenanthrene in the dissolved state in overlying water for the blank control group 2, A is a bar graph showing the change of the content of phenanthrene in the dissolved state in overlying water for the experimental group 6, B is a bar graph showing the change of the content of phenanthrene in the dissolved state in overlying water for the attapulgite control group.
Detailed Description
The first embodiment is as follows: the embodiment is a method for inhibiting the release of polycyclic aromatic hydrocarbons in bottom mud of a rice and crab co-farming paddy field by using rice straw biochar, which is specifically completed according to the following steps:
the method is characterized in that rice straw biochar is used as an inhibitor to be applied to bottom mud of a medium-light polycyclic aromatic hydrocarbon-polluted rice and crab co-farming rice field, and the application amount of the inhibitor is 1000 kg/mu-1500 kg/mu.
According to the embodiment, the biochar material prepared from the rice straws is used as an inhibitor for inhibiting the release of the polycyclic aromatic hydrocarbon in the bottom mud of the rice and crab co-farming paddy field, compared with other agricultural straws, the rice straws are the most common biomass raw material in an agricultural ecological system, and meanwhile, the rice straws are extremely soft, easy to pretreat and convenient to compress and form. The rice straw biochar not only has higher specific surface area, but also has rich functional groups on the surface, and can adsorb and fix organic pollutants in soil, the addition of the rice straw biochar to the bottom sediment of the rice field also increases the content of organic matters in the bottom sediment, changes the original sediment-water distribution coefficient, greatly reduces the diffusion and release of the pollutants in the soil, ensures that hydrophobic organic pollutants (polycyclic aromatic hydrocarbons such as phenanthrene) are not easily desorbed and released into overlying water, further achieves the aim of inhibiting the release of the polycyclic aromatic hydrocarbons in the bottom sediment, and effectively relieves the enrichment and accumulation of the organic pollutants in animals and plants. The content of organic carbon, the content of humic acid and fulvic acid, and the content of available nutrients in soil are increased to different degrees by adding the rice straw biochar, meanwhile, the rice straw biochar is alkaline and high in stability, can be applied to improving the acidic environment of soil, and is applied to inhibiting the release of polycyclic aromatic hydrocarbon of organic pollutants in bottom mud of a rice field as a biochar material, so that the pollution degree of agricultural soil is reduced, the food safety is guaranteed, the comprehensive utilization rate of agricultural straw resources is improved, and the energy and environmental pressure are relieved.
In the embodiment, the crabs in the medium-light polycyclic aromatic hydrocarbon polluted rice-crab co-farming rice field are eriocheir sinensis crabs, and the specification of the crabs is 120 to 200 crabs per kg.
The second embodiment is as follows: the present embodiment differs from the first embodiment in that: if rice straw biochar is continuously applied to the same medium-light polycyclic aromatic hydrocarbon-polluted rice and crab co-culture rice field for multiple years to serve as an inhibitor, the application amount of the inhibitor in the first year is 1000 kg-1500 kg/mu, the application amount of the inhibitor in the second year is 600 kg-1000 kg/mu, the application amount of the inhibitor in the third year is 300 kg/mu-500 kg/mu, and the application amount of the inhibitor in the fourth year is 300 kg/mu each year. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the rice straw biochar is prepared by the following steps:
and (3) putting the pretreated rice straws into a muffle furnace, carbonizing at 500 ℃ for 1h, taking out after the temperature is reduced to room temperature, grinding in a grinder, and sieving with a 60-mesh sieve to obtain the rice straw biochar.
The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the present embodiment is different from the third embodiment in that: the rice straw after pretreatment is finished according to the following steps:
cleaning rice straws by using water to remove impurities, naturally drying for 1 day, drying by using an oven at the temperature of 75 ℃ to constant weight, taking out and shearing according to the length of 3cm to obtain the pretreated rice straws.
The rest is the same as the third embodiment.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the rice biomass charcoal is applied in a soil plowing stage before rice transplanting, and the application depth is 0-5 cm. The rest is the same as the first to fourth embodiments.
The invention is not limited to the above embodiments, and one or a combination of several embodiments may also achieve the object of the invention.
The following tests are adopted to verify the effect of the invention:
firstly, self-preparing contaminated test soil, adding rice straw biochar as an inhibitor, and analyzing the inhibition effect of the addition of the rice straw biochar on the release of bottom sediment polycyclic aromatic hydrocarbon-phenanthrene in overlying water, wherein the specific operation is as follows:
the contaminated test soil is prepared according to the following steps: preparing a phenanthrene toxicant: wetting a 50mL volumetric flask by using methanol, then putting 50mg of phenanthrene into the volumetric flask, sucking the methanol by using a pipette until the volume of the solution in the volumetric flask reaches 1/3, horizontally shaking until the phenanthrene is uniformly dispersed, sucking the methanol by using the pipette until the volume reaches a scale mark, and then transferring to a 50mL brown blue-covered bottle to obtain a phenanthrene toxicant, wherein the concentration of the phenanthrene in the phenanthrene toxicant is 1000 mg/L; ②, contamination: putting 100g of dry and uncontaminated soil into a black barrel, firstly transferring 10mL of phenanthrene toxicant into a 20mL glass spray bottle by using a liquid transfer gun, then spraying the phenanthrene toxicant into 100g of dry and uncontaminated soil by using the glass spray bottle, mechanically stirring for 1h in a ventilated kitchen in a dark place to completely volatilize methanol in the phenanthrene toxicant, then putting the mixture into a refrigerator, and aging for 3d at the temperature of 4 ℃ to obtain contaminated and tested soil.
The rice straw biochar is prepared by the following steps: firstly, cleaning and removing impurities from rice straws by using water, naturally drying for 1 day, drying by using an oven at the temperature of 75 ℃ to constant weight, taking out and shearing according to the length of 3cm to obtain pretreated rice straws; secondly, putting the pretreated rice straws into a muffle furnace, carbonizing at 500 ℃ for 1h, taking out after the temperature is reduced to room temperature, then putting into a grinder for grinding, and sieving by a 60-mesh sieve to obtain the rice straw biochar.
Experimental group 1: adding 21g of contamination test soil into a brown glass conical flask, and mixing according to a soil-water ratio of 1.4: adding 15mL of tap water into 1 to prepare simulated bottom mud, adding 0.021g of rice straw biochar, uniformly mixing, plugging, sealing by a preservative film, placing in a constant-temperature oscillator, oscillating at 25 ℃ in a dark place at the rotation speed of 200rpm for 12 hours, transferring into a centrifuge tube, centrifuging for 20 minutes by a 7000r/min centrifuge, and filtering by using a 0.22-micron glass fiber filter membrane to obtain a filtrate to be detected.
Experimental group 2: the difference between this experimental group and experimental group 1 is: the adding amount of the rice straw biochar is 0.063 g. The other processing was the same as in example 1.
Experimental group 3: the difference between this experimental group and experimental group 1 is: the adding amount of the rice straw biochar is 0.105 g. The other processing was the same as in example 1.
Experimental group 4: the difference between this experimental group and experimental group 1 is: the adding amount of the rice straw biochar is 0.158 g. The other processing was the same as in example 1.
Experimental group 5: the difference between this experimental group and experimental group 1 is: the adding amount of the rice straw biochar is 0.21 g. The other processing was the same as in example 1.
Blank control group: no inhibitor was added:
adding 21g of contamination test soil into a brown glass conical flask, and mixing according to a soil-water ratio of 1.4: adding 15mL of tap water into 1 to prepare simulated bottom mud, plugging a cover, sealing a preservative film, placing the simulated bottom mud in a constant-temperature oscillator, oscillating the simulated bottom mud at the rotation speed of 200rpm for 12 hours at the temperature of 25 ℃ in a dark place, transferring the simulated bottom mud into a centrifuge tube, centrifuging the centrifuged product for 20 minutes by a 7000r/min centrifuge, and filtering the centrifuged product by a 0.22-micron glass fiber filter membrane to obtain a filtrate to be detected.
FIG. 1 is an SEM image of rice straw biochar of experiment group 1 at 1000 times; FIG. 2 is an SEM image of 3000 times of rice straw biochar in experimental group 1; FIG. 3 is a SEM image of rice straw biochar in experimental group 1 at 5000 times; the scanning electron microscope can directly show the surface morphology of the material, can analyze and observe element composition and internal three-dimensional morphology, and can see that the rice straw biochar has a rough surface and more irregular pore channels under the magnification of 1k times, the rice straw biochar has a smooth and regular internal structure and a clear peripheral outline and rich pore channel structures under the magnification of 3k times, and more grid-shaped structures are uniformly distributed in the pore channels under the magnification of 5k times, so that the original biomass structure is damaged and porous carbon frame structures such as carbonized lignin and the like are formed due to the evaporation of internal moisture at the cracking temperature, and the loose and porous structure of the rice straw biochar can provide more adsorption sites for the physical adsorption of organic pollutants and fix the adsorption sites in the pore channels, thereby achieving the purpose of adsorbing organic pollutants.
The content of the phenanthrene in the dissolved state in the filtrate to be detected obtained by the experimental group 1-5 and the content of the phenanthrene in the dissolved state in the filtrate to be detected obtained by the blank control group are detected by a high performance liquid chromatograph, and the test results are shown in table 1.
TABLE 1
The adsorption effect curve graph of the rice straw biochar is drawn by taking the addition of the rice straw biochar as an abscissa and taking the unit adsorption amount and the adsorption rate in table 1 as an ordinate, as shown in fig. 4, fig. 4 is the adsorption effect curve graph of the rice straw biochar, wherein B represents the addition of the rice straw biochar-a unit adsorption amount curve, and A represents the addition of the rice straw biochar-an adsorption rate curve; as can be seen from fig. 4 and table 1, under the same sampling time, with the content of phenanthrene in the dissolved state in the overlay water in the control group without adding rice straw biochar as the initial concentration, the content of phenanthrene in the dissolved state in the overlay water in different amounts of rice straw biochar added has significant difference. The adsorption rate of the rice straw biochar to the phenanthrene in the dissolved state in the overlying water is increased along with the increase of the addition amount of the biochar, when the mass ratio of the rice straw biochar to the contaminated test soil is increased from 0 to 0.1:100, the adsorption rate of the rice straw biochar to the phenanthrene in the dissolved state in the water is increased to 52.47%, and when the mass ratio of the rice straw biochar to the contaminated test soil is 0.5:100, the adsorption rate of the rice straw biochar to the phenanthrene in the dissolved state in the water is increased to 86.68%, which is mainly because when the addition amount of the rice straw biochar is increased, the total adsorption point position and the specific surface area are both increased, so that the adsorption efficiency is improved. And with the increase of the addition amount of the rice straw biochar, the unit adsorption amount of the rice straw biochar shows a gradual reduction trend, when the mass ratio of the rice straw biochar to the soil to be tested is increased from 0.1:100 to 1:100, the unit adsorption amount of the rice straw biochar is reduced from 151.79 mu g/g to 27.62 mu g/g, mainly because aggregation occurs in the biochar along with the addition of the biochar, the diffusion of dissolved phenanthrene adsorbed in the biochar to the surface of the biochar is prevented, and the unit adsorption amount of the biochar is reduced. When the mass ratio of the rice straw biochar to the contamination test soil is 0.5:100, if the content of the rice straw biochar is continuously increased, the content change of the phenanthrene in a dissolved state in water is not obvious, the adsorption efficiency of the rice straw biochar tends to be smooth, the unit adsorption amount, the adsorption rate, the economic cost and the like are comprehensively considered, and in the research, the rice straw biochar with the mass ratio of the rice straw biochar to the contamination test soil of 0.5:100 is taken as the optimal addition amount for inhibiting the release of PAHs in the sediment.
Second, microcosm simulation test:
the method is characterized in that the actual rice and crab co-culture rice field environment is simulated by designing a microcosm, the effect of adding rice straw biochar on inhibiting the release of dissolved phenanthrene in rice and crab co-culture sediment to overlying water at different time scales is analyzed, a transparent cuboid glass cylinder with the length, width and height of 250mm 160mm 180mm is adopted as the microcosm for carrying out experiments, and specific experimental groups and treatment modes are as follows:
experimental group 6: the method for inhibiting the release of the polycyclic aromatic hydrocarbon in the bottom mud of the rice and crab co-farming paddy field by using the rice straw biochar is specifically completed according to the following steps:
firstly, preparing phenanthrene polluted bottom mud: preparing a phenanthrene toxicant: adding 50mL of methanol into a 250mL volumetric flask, then adding 0.5g of powdered phenanthrene, oscillating until the powdered phenanthrene is completely dissolved, and fixing the volume to a scale mark by adopting a methanol-water mixed solution to obtain the phenanthrene toxicant; the methanol-water mixed solution is formed by mixing methanol and water, and the volume ratio of the methanol to the water is 12: 5; preparing contaminated test soil: uniformly spraying 250mL of phenanthrene toxicant exposure agent into 5kg of soil, mechanically stirring for 1h in a fume hood, and then placing for 2d in a dark place to obtain contaminated test soil, wherein the concentration of phenanthrene pollution in the contaminated test soil is 100 mg/kg; thirdly, aerating tap water, standing for 2d at normal temperature to obtain water to be added, adding 2L of water to be added into the contaminated soil to be tested obtained in the first step, and uniformly mixing to obtain phenanthrene contaminated bottom mud;
secondly, preparing rice straw biochar: firstly, cleaning and removing impurities from rice straws by using water, naturally drying for 1 day, drying by using an oven at the temperature of 75 ℃ to constant weight, taking out and shearing according to the length of 3cm to obtain pretreated rice straws; secondly, putting the pretreated rice straws into a muffle furnace, carbonizing at 500 ℃ for 1h, taking out the rice straws after the temperature is reduced to room temperature, grinding the rice straws in a grinder, and sieving the rice straws with a 60-mesh sieve to obtain rice straw biochar;
adding the phenanthrene-polluted bottom mud into the microcosm, wherein the depth of the phenanthrene-polluted bottom mud is 8cm, adding the rice straw biochar according to the mass ratio of the rice straw biochar to the soil to be tested infected in the step one, namely 0.5:100, uniformly mixing the rice straw biochar from the surface layer of the phenanthrene-polluted bottom mud to the depth of 5cm, and adding water until the height of the water layer of the upper water is 2 cm;
and fourthly, selecting the tested animals and plants: firstly, adopting pre-cultured rice with the same growth vigor and good growth condition as a test plant, taking 3 plants as one hole, and transplanting the test plant into the microcosm; secondly, adopting eriocheir sinensis as the tested crabs, domesticating for 2 weeks before the experiment, lighting for 12h/12h, keeping the temperature at room temperature, not feeding during the experiment, taking out two crabs, placing the crabs in the microcosm, and weighing 10g of each crab on average;
fifthly, sampling: taking the tested crabs placed in the microcosm as the starting time of the experiment, collecting 500mL of the overlying water by adopting brown glass sampling bottles at 6h, 12h, 24h, 2d, 4d, 7d, 15d and 30d respectively, supplementing water with the same amount as the collected water after each collection, and storing the collected overlying water in a refrigerator at the temperature of 4 ℃ for later use.
Fig. 5 is a photograph of a microcosm object constructed by experimental group 6.
Attapulgite control group: the difference between this experiment and experiment group 6 is: humic acid modified attapulgite is adopted to replace rice straw biochar in the experimental group 6 as an inhibitor; the humic acid modified attapulgite in the experiment is prepared according to the method provided by the Chinese published patent of a method for inhibiting the release of polycyclic aromatic hydrocarbons in the bottom mud of a rice and crab co-culture paddy field with medium and light polycyclic aromatic hydrocarbon pollution (application number: 202010740952.2), and the specific process is as follows:
the humic acid modified attapulgite is prepared by the following steps:
firstly, attapulgite pretreatment: firstly, crushing attapulgite to obtain attapulgite powder, and then sequentially carrying out acid modification and thermal modification on the attapulgite powder to obtain pretreated attapulgite; the specific process of acid modification is as follows: adding attapulgite powder into a hydrochloric acid solution with the mass fraction of 70%, performing ultrasonic dispersion at the temperature of 20 ℃ for 2 hours, then washing the attapulgite powder to be neutral by using ultrapure water, and finally performing vacuum drying at the temperature of 105 ℃ to constant weight to obtain acid-modified attapulgite; the mass ratio of the attapulgite powder to the hydrochloric acid solution with the mass fraction of 70% is 1: 15; the thermal modification comprises the following specific processes: calcining the acid modified attapulgite at the temperature of 550-850 ℃ for 2h, naturally cooling to room temperature, and sieving with a 200-mesh sieve to obtain pretreated attapulgite;
preparing a humic acid solution: weighing 5g of humic acid powder, dissolving the humic acid powder into 1L of NaOH solution with the concentration of 0.1mol/L, magnetically stirring the solution for 24 hours at the temperature of 80 ℃, filtering the solution by using a 0.45 mu m mixed fiber filter membrane by using a suction filtration device, adjusting the pH value of the obtained filtrate to be neutral by using HCl, then taking the filtrate out of a 1L narrow-mouth bottle, and diluting the filtrate to the concentration of 800mg/L to obtain a humic acid solution;
③ modifying: adding the pretreated attapulgite into a humic acid solution, placing on a water bath constant temperature oscillator, oscillating for 3 hours at the temperature of 25 ℃ at 250r/min, performing solid-liquid separation by a centrifugal machine, performing cold drying on a solid product obtained by separation, crushing and sieving to obtain humic acid modified attapulgite; the volume ratio of the mass of the pretreated attapulgite to the humic acid solution is 3g:100 mL.
Blank control group 2: no inhibitor was added:
firstly, preparing phenanthrene polluted bottom mud: preparing a phenanthrene toxicant: adding 50mL of methanol into a 250mL volumetric flask, then adding 0.5g of powdered phenanthrene, oscillating until the powdered phenanthrene is completely dissolved, and fixing the volume to a scale mark by adopting a methanol-water mixed solution to obtain the phenanthrene toxicant; the methanol-water mixed solution is formed by mixing methanol and water, and the volume ratio of the methanol to the water is 12: 5; preparing contaminated test soil: uniformly spraying 250mL of phenanthrene toxicant exposure agent into 5kg of soil, mechanically stirring for 1h in a fume hood, and then placing for 2d in a dark place to obtain contaminated test soil, wherein the concentration of phenanthrene pollution in the contaminated test soil is 100 mg/kg; thirdly, aerating tap water, standing for 2d at normal temperature to obtain water to be added, adding 2L of water to be added into the contaminated soil to be tested obtained in the first step, and uniformly mixing to obtain phenanthrene contaminated bottom mud;
secondly, adding the phenanthrene polluted bottom mud into the microcosm, wherein the depth of the phenanthrene polluted bottom mud is 8cm, and adding water until the height of an overlying water layer is 2 cm;
selecting test animals and plants: firstly, adopting pre-cultured rice with the same growth vigor and good growth condition as a test plant, taking 3 plants as one hole, and transplanting the test plant into the microcosm; secondly, adopting eriocheir sinensis as the tested crabs, domesticating for 2 weeks before the experiment, lighting for 12h/12h, keeping the temperature at room temperature, not feeding during the experiment, taking out two crabs, placing the crabs in the microcosm, and weighing 10g of each crab on average;
fourthly, sampling: taking the tested crabs placed in the microcosm as the starting time of the experiment, collecting 500mL of the overlying water by adopting brown glass sampling bottles at 6h, 12h, 24h, 2d, 4d, 7d, 15d and 30d respectively, supplementing water with the same amount as the collected water after each collection, and storing the collected overlying water in a refrigerator at the temperature of 4 ℃ for later use.
FIG. 6 is a photograph of the overwater physical object taken at 6h in experimental group 6; FIG. 7 is a photograph of the blank control group 2 taken at 6h with an overlying water object; as is apparent from fig. 6 and 7, the water quality of the overlying water sample taken by the blank control group 2 is clearer than that of the overlying water sample taken by the experimental group 6, because the biochar of the rice straw is added in the experimental group 6, and the biochar added in the sediment is diffused into the overlying water to a certain extent due to the disturbance of the crabs, so that the content of suspended solids in the water is increased.
Determination of total suspended solids content (TSS) of water body:
the total suspended solid content (TSS) in water is one of important indexes for measuring the water pollution degree, and in order to explore whether the biochar added with the rice straws can pollute the water, the suspended solid content (TSS) in the overlying water body in the experimental group 6, the attapulgite control group and the blank control group 2 is analyzed and determined, and the specific operation steps are as follows:
putting a filter membrane which is dried and clean at room temperature into a weighing bottle, measuring and counting the mass of the filter membrane, measuring 50mL of an overlying water sample which is fully and uniformly mixed, sucking and filtering the filter membrane to enable all water to pass through the filter membrane with the aperture of 0.45 mu m, continuously washing the filter membrane twice with 10mL of distilled water each time, continuously sucking and filtering to remove trace water, stopping sucking and filtering, carefully taking out the filter membrane with suspended matters, putting the filter membrane into the original weighing bottle with constant weight, putting the filter membrane into an oven, drying the filter membrane to constant weight at 103-105 ℃, putting the filter membrane into a dryer, cooling the filter membrane to room temperature, weighing the filter membrane, repeatedly drying, cooling and weighing the filter membrane until the weight difference between two times of weighing is less than 0.003g, wherein the difference between the two times of the filter membrane filtration is the mass of total suspended solids in the.
FIG. 8 is a graph showing the change in Total Suspended Solids (TSS) content in overburden water of an attapulgite control group, wherein A represents the change in Total Suspended Solids (TSS) content in overburden water of an experimental group 6, B represents the change in Total Suspended Solids (TSS) content in overburden water of a blank control group 2, and C represents the change in Total Suspended Solids (TSS) content in overburden water of a blank control group 2; as can be seen from the figure, the TSS content in the overlying water of the three treatments is higher and the difference is not large before the sampling time is 1d, which is mainly because the investment time of the crabs is shorter, the biological activity of the crabs is higher, and the life activities such as building nests and the like are more violent, so that the suspended particles and soil particles in the water body are more, and the water quality is more turbid; after 1d, along with the gradual sedimentation of sediments, the crab nest is completely constructed, the activity of the crab nest is gradually reduced, the TSS content difference of different treatment groups is obvious, when the sampling time is 4d, the TSS content of overlying water of the blank control group 2 is 83.5mg/L, the TSS content in the experimental group 6 is 26% higher than that in the blank control group 2, and the TSS content in the attapulgite control group is 98.6% higher than that in the blank control group 2; when the sampling time is 7d, the TSS content in the experimental group 6 slightly increases, which may be caused by that some crab biological disturbance transfers sediment particles to the overlying water again before sampling to increase the TSS content, after 15d, the TSS content of the overlying water under the three treatments gradually tends to be stable, the TSS content of the overlying water in the white control group 2 is reduced to 60.6mg/L at the 30 th d, the TSS content of the overlying water in the experimental group 6 is only higher than 23% compared with the TSS content of the overlying water in the blank control group 2, and the TSS content of the overlying water in the attapulgite control group is higher than 129.2% compared with the TSS content of the overlying water in the blank control group 2 and slightly increases. Generally speaking, the TSS content of a control group taking humic acid modified attapulgite as an inhibitor at each time point is obviously higher than that of an experimental group taking rice straw biochar as an inhibitor, so that compared with humic acid modified attapulgite, the addition of the rice straw biochar does not cause serious pollution and damage to water quality, secondary pollution caused by the addition of the inhibitor to a water body is avoided, and the development requirement of ecological cycle agriculture in China and the development process of green agriculture are met.
And (3) determination of phenanthrene in a water body dissolved state:
centrifuging the collected overlying water sample by a centrifuge at 6000r/min for 20min, filtering the water sample by a 0.45-micron glass fiber filter membrane into a beaker, pouring the water sample into a separating funnel for liquid-liquid extraction, adding 5g of NaCl and 25mL of dichloromethane, shaking by hand to extract for 10min, standing for layering, and collecting the lower extraction liquid. Extracting twice with 10mL of dichloromethane addition each time to ensure complete extraction, pouring the combined extract into a glass test tube with cotton and anhydrous sodium sulfate at the bottom for elution, pouring into a rotary evaporator for rotary evaporation after no fine water drops appear in the eluent, (the temperature is 40 ℃, the rotating speed is 70r/min), pouring all the rotary evaporation liquid out when the volume is less than 1mL, flushing the rotary evaporation bottle with methanol, pouring the flushing liquid into the glass tube together, accurately metering the volume to 5mL with methanol, extracting 1mL of liquid, and dripping into a liquid chromatography sample bottle for high performance liquid chromatography to test, wherein the test result is shown in figure 9:
FIG. 9 is a bar graph showing the change of the content of phenanthrene in a dissolved state in overlying water for the blank control group 2, A is a bar graph showing the change of the content of phenanthrene in a dissolved state in overlying water for the experimental group 6, B is a bar graph showing the change of the content of phenanthrene in a dissolved state in overlying water for the attapulgite control group; as can be seen from the figure, in the initial stage of the experiment, the rice straw biochar and the humic acid modified attapulgite both show extremely high adsorption effects, when the sampling time is 12 hours, the content of the phenanthrene in the water-soluble state of the upper cover in the blank control group 2 is 236.37 mug/L, the content of the experiment group 6 is 52.00 mug/L, the adsorption rate to the phenanthrene in the water-soluble state reaches 78%, and the adsorption rate to the phenanthrene in the water-soluble state of the upper cover in the attapulgite control group is 71% by the content of 68.41 mug/L, which is because the mass transfer driving force caused by the concentration difference of the phenanthrene in the water-inhibiting material in the initial two phases of the water-inhibiting material and the adsorption sites on the surface of the biochar are related, the concentration of the phenanthrene in the water in the initial stage of the experiment is the largest, the driving force of the internal mass transfer is large, so that the inhibiting material in the initial stage has a large adsorption amount to the phenanthrene, the adsorption rate of the stage is relatively slow because the adsorption sites on the surface of the rice straw biochar and the humic acid modified attapulgite gradually reach saturation, the dissolved phenanthrene in the overlying water gradually diffuses from surface layer pores to the inside and further reacts with the internal active sites; the adsorption effect of the test group 6 reaches the highest at the 4 th day, the removal rate of the dissolved phenanthrene in water reaches 82.69%, the content of the dissolved phenanthrene in the test group 6 at different sampling times is obviously lower than that of the attapulgite control group at the same sampling time, after the 7 th day, the content of the dissolved phenanthrene in the attapulgite control group is increased rather than that in the blank control group 2, because the adsorption point on the surface of the humic acid modified attapulgite gradually reaches saturation, the phenanthrene in the internal adsorption complete pore channel is desorbed and released from the surface into the overlying water body, the desorption and re-release phenomena are more obvious along with the change of time, and the content of the dissolved phenanthrene in the attapulgite control group at the 30 th day is higher than 91.4% relative to that in the blank control group 2. From the whole view, although the rice straw biochar and the humic acid modified attapulgite show a certain inhibition effect on the release of polycyclic aromatic hydrocarbons in the bottom sediment into the overlying water, the inhibition effect of the rice straw biochar on the polycyclic aromatic hydrocarbons and phenanthrene is obviously higher than that of the humic acid modified attapulgite, the adsorption effect is more stable, and an obvious desorption process is not shown relative to the humic acid modified attapulgite, so that the secondary pollution caused by the release of the humic acid modified attapulgite into the water due to adsorption saturation is avoided, therefore, the rice straw biochar is obviously better than the humic acid modified attapulgite in the effects and stability of influencing water quality and inhibiting the release of the polycyclic aromatic hydrocarbons and phenanthrene into the water.
The reason that the rice straw biochar can obviously inhibit the release of polycyclic aromatic hydrocarbon-phenanthrene in bottom sediment into an overlying water body mainly comprises the following aspects: (1) the rice straw biochar has compact structure and rough surface, can expose more active points, and has densely arranged granular substances distributed on the surface layer because the rice straw surface has a layer of compact tissue and epidermis, and epidermal cells are rich in SiO2The composition of the silicon cells and the subelement cells is more beneficial to the generation and the proceeding of the adsorption reaction, so the surface adsorption of the rice straw biochar has larger contribution to inhibiting the phenanthrene in the bottom mud from being released into the overlying water; (2) the biochar serving as a soil conditioner can obviously improve the pH value of the sediment soil in a short time, and the pH value is increased, so that the dissoluble phenanthrene which is easy to migrate in the sediment can be combined, the mobility of organic matters in the sediment is influenced, the formation of soil aggregates is promoted, the sediment of the sediment is reacted with the dissoluble phenanthrene, the content of the dissoluble phenanthrene released into an overlying water body in the sediment of the sediment is further reduced, and the biological effectiveness of the dissoluble phenanthrene is reduced. The content of the soluble phenanthrene in the 7 th covering water is slightly increased compared with that in the 15 th covering water, because the adsorption point position and the total adsorption amount on the surface of the rice straw biochar are basically saturated, part of biochar is desorbed, so that the soluble phenanthrene on the surface of the biochar is re-diffused into the water body, the content of the soluble phenanthrene in the covering water is slightly increased, but the content is only increased by 1.94 mug/L, which shows that the adsorption effect of the biomass carbon on the dissolved phenanthrene is firmer, most of the dissolved phenanthrene is still fixed on the surface of the biomass carbon, and the adsorption stability is higher, so that secondary pollution to a water body caused by desorption is avoided.
Polycyclic aromatic hydrocarbon is an organic matter widely existing in the environment, the residual concentration and the form of polycyclic aromatic hydrocarbon in the soil are deeply influenced by the adsorption, desorption, conversion, degradation and other environmental behaviors of polycyclic aromatic hydrocarbon in agricultural soil, and compared with polycyclic aromatic hydrocarbon in other forms, polycyclic aromatic hydrocarbon is easier to migrate to the surrounding environment and influence the ecological safety of the surrounding environment. Experiments prove that the content of soluble phenanthrene in the overlying water can be remarkably reduced by the rice straw biochar, the rice straw biochar is added into sediment sediments as an adsorbing material to effectively inhibit phenanthrene in the sediment from migrating and releasing into the overlying water, meanwhile, the influence of the addition of the biochar on the water quality of the overlying water body is small, the adsorbing effect is stable, and secondary harm caused by desorption and release to the surrounding environment is not easy to occur.
Example 1: a method for inhibiting the release of polycyclic aromatic hydrocarbons in bottom mud of a rice and crab co-culture rice field by using rice straw biochar is specifically completed according to the following steps:
the method comprises the step of applying rice straw biochar serving as an inhibitor to bottom mud of a medium-light polycyclic aromatic hydrocarbon-polluted rice and crab co-culture rice field, wherein the application amount of the inhibitor is 1200 kg/mu.
In the embodiment, the crabs in the medium-light polycyclic aromatic hydrocarbon polluted rice-crab co-farming rice field are eriocheir sinensis crabs, and the specification of the crabs is 120 to 200 crabs per kg.
The preparation process of the rice straw biochar in the embodiment is as follows: firstly, cleaning and removing impurities from rice straws by using water, naturally drying for 1 day, drying by using an oven at the temperature of 75 ℃ to constant weight, taking out and shearing according to the length of 3cm to obtain pretreated rice straws; secondly, putting the pretreated rice straws into a muffle furnace, carbonizing at 500 ℃ for 1h, taking out after the temperature is reduced to room temperature, then putting into a grinder for grinding, and sieving by a 60-mesh sieve to obtain the rice straw biochar.
The rice biomass charcoal is applied in the soil plowing stage before rice transplanting, and the application depth is 0-5 cm.
In the initial stage of the medium and light polycyclic aromatic hydrocarbon polluted rice and crab co-cultivation paddy field of the embodiment 1, the overlying water is collected, the water body dissolved phenanthrene is measured, the content of the overlying water dissolved phenanthrene is 37.659ng/L, the overlying water is collected after the crab is placed in the position 7d, and the water body dissolved phenanthrene is measured, and the content of the overlying water dissolved phenanthrene is 6.026 ng/L.
Example 2: the present embodiment differs from embodiment 1 in that: the application amount of the inhibitor is 600 kg/mu. The rest is the same as in example 1.
In the initial stage of the medium and light polycyclic aromatic hydrocarbon polluted rice and crab co-cultivation paddy field of the embodiment 2, the overlying water is collected, the phenanthrene in the water body dissolution state is measured, the content of the phenanthrene in the overlying water dissolution state is 45.397ng/L, the overlying water is collected after the crabs are placed in the 7 th day, and the content of the phenanthrene in the water body dissolution state is measured, wherein the content of the phenanthrene in the overlying water dissolution state is 14.527 ng/L.
Example 3: the present embodiment differs from embodiment 1 in that: the application amount of the inhibitor is 800 kg/mu. The rest is the same as in example 1.
In the initial stage of the medium and light polycyclic aromatic hydrocarbon polluted rice and crab co-cultivation paddy field of the embodiment 3, the overlying water is collected, the phenanthrene in the water body dissolution state is measured, the content of the phenanthrene in the overlying water dissolution state is 42.436ng/L, the overlying water is collected after the crabs are placed in the position 7d, and the content of the phenanthrene in the water body dissolution state is measured, wherein the content of the phenanthrene in the overlying water dissolution state is 10.949 ng/L.
Example 4: the present embodiment differs from embodiment 1 in that: the application amount of the inhibitor is 1000 kg/mu. The rest is the same as in example 1.
In the initial stage of the medium and light polycyclic aromatic hydrocarbon polluted rice and crab co-cultivation paddy field of the embodiment 4, the overlying water is collected, the phenanthrene in the water body dissolution state is measured, the content of the phenanthrene in the overlying water dissolution state is 33.037ng/L, the overlying water is collected after the crabs are placed in the 7 th place, and the content of the phenanthrene in the water body dissolution state is measured, wherein the content of the phenanthrene in the overlying water dissolution state is 6.178 ng/L.
Example 5: the present embodiment differs from embodiment 1 in that: the application amount of the inhibitor is 1500 kg/mu. The rest is the same as in example 1.
At the beginning of the medium and light polycyclic aromatic hydrocarbon polluted rice and crab co-farming paddy field of the example 5, the overlying water is collected, the phenanthrene in the water body dissolved state is measured, the content of the phenanthrene in the overlying water dissolved state is 30.136ng/L, the overlying water is collected at the 7 th day when the crabs are put in the paddy field, and the content of the phenanthrene in the water body dissolved state is measured, wherein the content of the phenanthrene in the overlying water dissolved state is 4.129 ng/L.
Claims (5)
1. A method for inhibiting the release of polycyclic aromatic hydrocarbons in bottom mud of a rice and crab co-culture rice field by using rice straw biochar is characterized by comprising the following steps:
the method is characterized in that rice straw biochar is used as an inhibitor to be applied to bottom mud of a medium-light polycyclic aromatic hydrocarbon-polluted rice and crab co-farming rice field, and the application amount of the inhibitor is 1000 kg/mu-1500 kg/mu.
2. The method for inhibiting the release of the polycyclic aromatic hydrocarbons in the bottom sediment of the rice-crab co-cropping rice fields by using the rice straw biochar as the inhibitor is characterized in that if the rice straw biochar is continuously applied to the same moderate and light polycyclic aromatic hydrocarbon-polluted rice-crab co-cropping rice field for multiple years, the inhibitor is applied at 1000 kg/mu to 1500 kg/mu in the first year, 600 kg/mu to 1000 kg/mu in the second year, 300 kg/mu to 500 kg/mu in the third year, and 300 kg/mu in the fourth year.
3. The method for inhibiting the release of polycyclic aromatic hydrocarbons in the bottom sediment of the rice and crab co-culture paddy field by using the rice straw biochar as claimed in claim 1 or 2, wherein the rice straw biochar is prepared by the following steps:
and (3) putting the pretreated rice straws into a muffle furnace, carbonizing at 500 ℃ for 1h, taking out after the temperature is reduced to room temperature, grinding in a grinder, and sieving with a 60-mesh sieve to obtain the rice straw biochar.
4. The method for inhibiting the release of the polycyclic aromatic hydrocarbons in the bottom sediment of the rice and crab co-farming paddy field by using the biochar of the rice straws as claimed in claim 3, wherein the pretreated rice straws are finished by the following steps:
cleaning rice straws by using water to remove impurities, naturally drying for 1 day, drying by using an oven at the temperature of 75 ℃ to constant weight, taking out and shearing according to the length of 3cm to obtain the pretreated rice straws.
5. The method for inhibiting the release of the polycyclic aromatic hydrocarbons in the bottom mud of the rice and crab co-farming paddy field by using the rice straw biochar as claimed in claim 1, wherein the rice biomass charcoal is applied at the soil plowing stage before rice transplanting, and the application depth is 0-5 cm.
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