CN107876010B - Curing agent for bisphenol A contaminated soil and preparation method and application thereof - Google Patents
Curing agent for bisphenol A contaminated soil and preparation method and application thereof Download PDFInfo
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- CN107876010B CN107876010B CN201711075539.3A CN201711075539A CN107876010B CN 107876010 B CN107876010 B CN 107876010B CN 201711075539 A CN201711075539 A CN 201711075539A CN 107876010 B CN107876010 B CN 107876010B
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Abstract
The invention discloses a curing agent for bisphenol A contaminated soil and a preparation method and application thereof. The curing agent is litchi branch biochar. Also discloses a preparation method of the litchi branch biochar curing agent. The method is characterized in that the soil polluted by the bisphenol A is mixed with a litchi branch biochar curing agent to carry out bisphenol A immobilization. The litchi branch biochar-doped soil immobilized bisphenol A can effectively utilize waste resources, change waste into valuable, is simple to operate, has an obvious effect, is relatively low in cost compared with other immobilizing agents, and can improve soil, so that the litchi branch biochar-doped soil immobilized bisphenol A has high practicability and application value.
Description
Technical Field
The invention relates to a curing agent for bisphenol A contaminated soil and a preparation method and application thereof.
Background
Endocrine disruptors have become a new class of organic pollutants in recent years. Bisphenol A, a typical pollutant of endocrine disruptors, has a chemical structure similar to that of estradiol and diethylstilbestrol, has the same effect as other environmental hormones, can imitate or infect endogenous estrogen, plays the role of estrogen analogue, and can generate adverse effects on various aspects of reproduction, growth and development, nervous system, immune system and the like of organisms even if the concentration is ng/L. Bisphenol A is poorly recognized as being susceptible to degradation under aerobic conditions, but is capable of remaining for a long period of time and causing damage, such as in deep soil, and groundwater, under anoxic or anaerobic conditions. Therefore, studies for reducing the migration of bisphenol A in the environment are necessary.
At present, the control of the pollution migration of bisphenol A in soil mainly focuses on the relevant researches of removing bisphenol A in soil such as biodegradation method, chemical method, physical in-situ fixation method and the like. The biodegradation method is usually used for degrading soil bisphenol A by pseudomonas putida, brevibacterium and the like, but the biodegradation method has a plurality of defects, such as: when in-situ treatment is carried out on bisphenol A pollution of deep soil, as the used bacterial strains are mostly aerobic, the biodegradation process needs to be continuously supplemented with soil oxygen; meanwhile, the microorganisms used in the biodegradation method need the prerequisite steps of separation, purification, culture and the like, and the applied microorganisms also need to consider the ecological influence on the original indigenous microorganisms. The researchers degrade bisphenol A in soil by electrochemical method, and achieve the purpose of reducing the biotoxicity of bisphenol A by directly reacting with a high-reactivity electrode or reacting with HO & free radicals with strong oxidizing property generated by a positive pole, and the technology is relatively expensive in practical application cost and relatively high in requirements on soil environment. In addition, the researchers also treat the polluted bisphenol A soil by a chemical leaching method, but when the method is used for treating the large-area soil pollution, the treatment process is relatively complicated, secondary pollution is generated, and the problem of leaving is caused. Compared with biological treatment and chemical treatment, the physical in-situ immobilization method is a research hotspot due to simple operation, low cost and obvious treatment effect.
In situ immobilization is a technology for in situ treatment of pollutants, and the treatment of contaminated soil using the same is currently considered as a potentially effective treatment method. Due to strong polarity and high water solubility, bisphenol A is easy to migrate and transform under the action of surface runoff such as rainfall and the like to enter surface water or underground water. If the external conditions are properly changed to change unstable bisphenol A into a stable state, the capacity of bisphenol A to migrate from soil to water can be reduced, thereby reducing the environment-friendly effect of bisphenol APotential hazards of (1). By doping a proper amount of chemical reagents, organic matters and the like into the soil, the mobility and toxicity of pollutants are reduced, so that the bisphenol A in the soil is immobilized. In practical operation, the immobilization technology is mainly focused on the study of heavy metal pollution of soil, such as: by immobilising heavy metal ions Pb in soil doped with apatite or struvite2+. However, although the research on the soil bisphenol a is carried out, the experimental data is not close to the actual situation, so that the soil bisphenol a fixing technology is not applied to the practice.
The biochar is a carbon material which is rich in pore structure, high in carbon content and high in aromatization and is produced by pyrolyzing carbon-rich biomass under the condition of oxygen limitation, and in recent years, the biochar is mainly used for carbon fixation, soil fertility improvement and crop yield increase, and has a good adsorption and fixation effect on heavy metals and organic matters in water, soil or sediments due to the fact that the biochar has high pH, high porosity and rich oxygen-containing functional groups. Biochar is receiving wide attention as a novel environmental functional material. Meanwhile, researches show that the lignin and cellulose in the wood material are higher than other types of raw materials, so that the yield, the specific surface area and the quantity of generated functional groups of the prepared wood material are relatively high, and the adsorption effect on organic pollutants is relatively good.
The litchi is used as the original fruit in south China, the total planting area is about 900 ten thousand mu, and the residual branch quantity of the fruit trees trimmed every year is about 6.5 multiplied by 105t. While 80% of the spent routes of these branches are focused on burning firewood. With the acceleration of the rural urbanization process, the traditional fuel mode gradually disappears, the consumption and the use of the residual branches are gradually reduced, a large number of residual branches are stacked, and serious adverse effects are brought. Meanwhile, the residual branches have a plurality of pathogenic bacteria and are easy to generate bacteria when being stacked in the open air, so that soil and water sources are polluted, and the living environment of farmers is influenced. Therefore, the stump treatment and resource utilization of the fruit tree stumps are required.
Disclosure of Invention
The invention aims to provide a curing agent for bisphenol A contaminated soil and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
a curing agent for bisphenol A contaminated soil is litchi branch biochar.
A preparation method of a curing agent for bisphenol A contaminated soil comprises the following steps:
1) cleaning, drying and cutting waste litchi branches to obtain a biomass raw material;
2) pyrolyzing the biomass raw material in an anaerobic atmosphere, grinding the obtained solid product, and sieving to obtain the curing agent.
In the step 1) of the preparation method of the curing agent, the cutting is to cut the waste litchi branches into branch sections with the length of 1 cm-2 cm.
In the step 2) of the preparation method of the curing agent, the anaerobic atmosphere is one of nitrogen, helium, neon, argon, krypton and xenon.
In the step 2) of the preparation method of the curing agent, the pyrolysis specific conditions are as follows: the heating rate is 4 ℃/min to 6 ℃/min, the final pyrolysis temperature is 550 ℃ to 650 ℃, and the pyrolysis time is 1.5h to 2.5 h.
In the step 2) of the preparation method of the curing agent, the mesh number of the sieving screen is 50-100 meshes.
A method for immobilizing bisphenol A in soil comprises mixing bisphenol A-contaminated soil with the above-mentioned solidifying agent to immobilize bisphenol A.
In the fixing method, the doping amount of the curing agent is 1-5% of the mass of the bisphenol A polluted soil.
The invention has the beneficial effects that:
the litchi branch biochar-doped soil immobilized bisphenol A can effectively utilize waste resources, change waste into valuable, is simple to operate, has an obvious effect, is relatively low in cost compared with other immobilizing agents, and can improve soil, so that the litchi branch biochar-doped soil immobilized bisphenol A has high practicability and application value.
Specifically, the method comprises the following steps:
1. according to the analysis of the adsorption experiment result, the addition of the litchi branch biochar improves the adsorption capacity of 230.5-486.46% of soil, and the adsorption capacity of black soil or moisture soil is obviously enhanced.
2. Through simulating the most serious soil leaching situation of soil, the desorption process of bisphenol A is effectively inhibited by the litchi branch biochar-doped polluted soil, leaching is carried out at the maximum soil permeation rate, and after 20-hour continuous leaching desorption tests, about 90% or more of bisphenol A in black soil or moisture soil is still fixed in the two types of soil doped with litchi branch biochar, so that the adsorption and fixation capacity is improved by 304.09% -349.47% compared with that of an undoped comparative sample.
3. The litchi branch biochar enhances the stability of bisphenol A in soil, reduces the bioavailability of bisphenol in the soil, and realizes the immobilization of bisphenol A in the soil.
Drawings
FIG. 1 is a schematic view of a scanning electron microscope of litchi branch biochar;
FIG. 2 is a schematic view of an apparatus for adsorption and immobilization testing;
FIG. 3 is a graph showing the adsorption effect of the adsorption test;
FIG. 4 is a graph showing the effect of immobilization in the immobilization test.
Detailed Description
A curing agent for bisphenol A contaminated soil is litchi branch biochar.
A preparation method of a curing agent for bisphenol A contaminated soil comprises the following steps:
1) cleaning, drying and cutting waste litchi branches to obtain a biomass raw material;
2) pyrolyzing the biomass raw material in an anaerobic atmosphere, grinding the obtained solid product, and sieving to obtain the curing agent.
Preferably, in the step 1) of the preparation method of the curing agent, the drying is specifically air-drying for 5-10 days, and then drying for 60-80 hours at 75-85 ℃.
Preferably, in the step 1) of the preparation method of the curing agent, the cutting is to cut the waste litchi branches into branch sections with the length of 1 cm-2 cm.
Preferably, in the step 2) of the preparation method of the curing agent, the anaerobic atmosphere is one of nitrogen, helium, neon, argon, krypton and xenon; further preferably, in the step 2) of the method for preparing the curing agent, the anaerobic atmosphere is a nitrogen atmosphere.
Preferably, in step 2) of the preparation method of the curing agent, the specific conditions of pyrolysis are as follows: the heating rate is 4 ℃/min to 6 ℃/min, the final pyrolysis temperature is 550 ℃ to 650 ℃, and the pyrolysis time is 1.5h to 2.5 h.
Preferably, in the step 2) of the preparation method of the curing agent, the mesh number of the sieving screen is 50-100 meshes; further preferably, in step 2) of the preparation method of the curing agent, the mesh number of the sieving screen is 100 meshes.
A method for immobilizing bisphenol A in soil comprises mixing bisphenol A-contaminated soil with the above-mentioned solidifying agent to immobilize bisphenol A.
Preferably, in the fixing method, the doping amount of the curing agent is 1-5% of the mass of the bisphenol A polluted soil; more preferably, in the fixing method, the doping amount of the curing agent is 3-5% of the mass of the bisphenol A polluted soil.
The present invention will be described in further detail with reference to specific examples.
In the bisphenol A contaminated soil of the example of the present invention, the soil types were black soil or moist soil, wherein the average organic matter content of the black soil was 2.78 wt%, and the average organic matter content of the moist soil was 0.6 wt%.
Preparation of litchi branch biochar curing agent
The preparation method of the curing agent comprises the following steps:
(1) collecting litchi branch waste as a preparation raw material;
(2) cleaning to remove soil particles attached to the surface, and air-drying for 1 week;
(3) drying for 72 hours at 80 ℃, and cutting into 1-2 cm sections as standby biomass;
(4) filling the standby biomass in a 200mL ceramic crucible, covering the ceramic crucible with a cover, placing the ceramic crucible in an atmosphere protection box type furnace, and preparing the biochar by adopting an anaerobic slow pyrolysis method, wherein the process parameters are as follows: heating to 600 ℃ in an atmosphere box furnace at the heating rate of 5 ℃/min, carrying out constant-temperature continuous pyrolysis for 2 hours, and continuously introducing 100mL/min nitrogen in the preparation process;
(5) and taking out the biochar after the biochar is naturally cooled to room temperature, grinding the biochar, screening the biochar by a 100-mesh standard sieve, and sealing the biochar in a brown wide-mouth bottle for later use.
FIG. 1 is a scanning electron microscope schematic diagram of litchi branch biochar. As can be seen from figure 1, the prepared litchi branch biochar has a loose and porous structure. Meanwhile, the biomass charcoal has low ash content and high yield of 6.30 percent, and has high specific surface area (187.76 m) compared with common biochar2·g-1) And the pore diameter (2.17nm) is larger than the molecular diameter of bisphenol A.
Second, adsorption test
The test for measuring the adsorption capacity of the litchi branch charcoal-doped soil to the bisphenol A is as follows:
(1) placing the mixture of the litchi branch biochar and the soil in a mass ratio of 4:100 into a 100mL glass beaker, and fully stirring the mixture by a glass rod until the mixture is uniformly mixed.
(2) Uniformly filling 7g of soil doped with litchi branch biochar into a hard glass tube with the inner diameter of 2cm and the length of 7cm, paving a layer of 0.45-micrometer glass fiber filter membrane at the bottom of the column before filling the soil sample, and then paving a layer of quartz sand. The bisphenol A aqueous solution is driven by a peristaltic pump to enter the test soil sample at the maximum penetration rate of 0.2mL/min of the test soil sample, so as to simulate the condition that the bisphenol A is adsorbed by the soil in reality.
(3) Performing adsorption reaction at 25 deg.C for 30 hr, collecting column effluent every 30 min, filtering column effluent with 0.45 μm glass fiber membrane, and determining bisphenol A concentration in the effluent by high performance liquid chromatography. The maximum adsorption was calculated as follows:
Cads=C0-C formula (1)
CadsBisphenol A immobilized adsorption concentration, mg/L;
C0-inlet water concentration, mg/L;
c, effluent concentration, mg/L;
q is volume flow, L/h;
qads-loading soil sample adsorption capacity, mg/kg;
D1degree of increase in bisphenol A adsorption,%.
Meanwhile, a soil sample which is not doped with litchi branch biochar is adopted to carry out a comparative adsorption experiment, and the steps are the same as above.
The schematic diagram of the adsorption test apparatus is shown in FIG. 2. Bisphenol A in the aqueous solution is an artificially synthesized estrogen-like hormone. The soil type is black soil or moist soil, wherein the black soil has relatively higher organic matter content compared with other domestic types of soil, the organic matter content of the moist soil is far smaller than that of the black soil, and other physicochemical indexes of the two types of soil are not very different.
FIG. 3 is a graph showing the adsorption effect of the adsorption test. The maximum adsorption amounts of bisphenol A calculated by the formulas (1) to (3) are 47.51mg/kg (black soil), 18.17mg/kg (moist soil), 156.81mg/kg (black soil + litchi branch biochar) and 106.56mg/kg (moist soil + litchi branch biochar). Therefore, the adsorption capacity of the bisphenol A is obviously increased after the litchi branch biochar is doped in the two types of soil, the adsorption capacity of the black soil bisphenol A is increased by 230.05% and the adsorption capacity of the moisture soil bisphenol A is increased by 486.46% in the two types of soil with the litchi branch biochar doping ratio of 4%, which indicates that the adsorption capacity of the soil on the bisphenol A is obviously enhanced by adding the litchi branch biochar.
Third, curing test
The specific test for measuring the bisphenol A fixed quantity of the bisphenol A contaminated soil by the litchi branch charcoal is as follows:
(1) 0.0100g of bisphenol A solid is weighed and dissolved in 100mL of acetone, and added into 100g of soil, and the mixture is fully stirred uniformly so that the pollution concentration reaches 100mg/kg, so as to simulate the serious condition that the bisphenol A pollutes the soil. And (3) placing in a ventilated kitchen, adding 4% of biochar by mass into the test contaminated soil after acetone is completely evaporated and disappears after 48 hours, and fully and uniformly mixing. Keeping the humidity of the soil doped with the litchi branch biochar at 60%, drying for later use after 2 months, and determining the concentration of bisphenol A in the bisphenol A-polluted soil doped with the litchi branch biochar before testing.
(2) Weighing 7g of polluted soil doped with litchi branch biochar, uniformly filling the polluted soil into a hard glass column with the inner diameter of 2cm and the length of 7cm, and driving 0.01mol/LCaCl by a peristaltic pump at the volume flow of 0.2mL/min2The solution desorbs the contaminated sample and collects the effluent every 30 minutes.
(3) Performing desorption reaction at 25 ℃ for 20 hours, filtering the collected effluent by a 0.45-micron glass fiber filter membrane, and measuring the concentration of bisphenol A in the effluent by using high performance liquid chromatography, wherein the immobilized adsorption rate of bisphenol A in the soil doped with litchi branch biochar is calculated as follows:
qdesthe desorption amount of the soil sample doped with the litchi branch biochar is mg/kg;
q0-contaminated sample bisphenol a concentration, mg/kg;
D2immobilized adsorption rate of bisphenol A,%.
Meanwhile, a soil sample which is not doped with litchi branch biochar is adopted to carry out a comparison and fixation experiment, and the steps are the same as above.
The schematic diagram of the device for the fixation test is shown in figure 2.
FIG. 4 is a graph showing the effect of immobilization in the immobilization test. The desorption amounts calculated by the formulas (4) to (5) are 64.86mg/kg (black soil), 75.46mg/kg (moist soil), 8.23mg/kg (black soil + litchi branch biochar) and 10.04mg/kg (moist soil + litchi branch biochar) respectively until 20 hours. The desorption amount of the two types of polluted soil doped with the litchi branch biochar is obviously reduced. The initial effluent concentration of the soil not doped with the litchi branch biochar can reach 41.67mg/L at most in the experiment, and the initial effluent concentration of the soil doped with the litchi branch biochar is less than 0.56 mg/L. The retention rates of the bisphenol A in the comparison group are respectively polluted black soil (22.49%) and polluted moisture soil (19.69%), and the retention rates of the bisphenol A in the experimental group are respectively polluted black soil (90.88%) restored by litchi branch biochar and polluted moisture soil (88.50%) restored by litchi branch biochar. Compared with an undoped comparison sample, the adsorption and fixation capacity is improved by 304.09-349.47%. The litchi branch biochar doped with the litchi branch effectively improves the fixing capacity of soil to the bisphenol A, and the adsorption and fixation of the two types of soil can reach 90% or more, namely, the litchi branch biochar for resource utilization enhances the stability of the bisphenol A in the soil, reduces the bioavailability of the bisphenol A in the soil, and achieves the aim of bisphenol A immobilization.
In conclusion, the method has the advantages of effective utilization of waste resources, waste recycling, simple operation, relatively low cost compared with other fixatives, high bisphenol A adsorption rate, good immobilization effect and the like. The soil adsorption capacity is improved to 230.5-486.46%, the bisphenol A immobilized adsorption rate of the immobilized adsorption to the soil sample can reach 90% or more, and the bisphenol A desorption process is effectively inhibited. The method not only makes full use of the waste resources of the branches and the residual branches of the litchi, but also effectively reduces the possibility of migration pollution of the bisphenol A in the soil to the underground water body, realizes the immobilization of the bisphenol A in the soil, improves the soil, and has high practicability and application value.
Claims (1)
1. A method for immobilizing bisphenol A in soil, comprising: mixing the bisphenol A contaminated soil with a curing agent to carry out bisphenol A immobilization;
the doping amount of the curing agent is 1-5% of the mass of the bisphenol A polluted soil;
the soil is black soil or moist soil;
the curing agent is litchi branch biochar;
the curing agent is prepared by the following preparation method:
1) cleaning, drying and cutting waste litchi branches to obtain a biomass raw material;
2) pyrolyzing a biomass raw material in an anaerobic atmosphere, grinding an obtained solid product, and sieving to obtain a curing agent;
in the step 1), the cutting is to cut the waste litchi branches into branch sections with the length of 1 cm-2 cm;
in the step 2), the anaerobic atmosphere is one of nitrogen, helium, neon, argon, krypton and xenon;
in the step 2), the pyrolysis conditions are as follows: the heating rate is 4 ℃/min to 6 ℃/min, the final pyrolysis temperature is 550 ℃ to 650 ℃, and the pyrolysis time is 1.5h to 2.5 h;
in the step 2), the mesh number of the sieving screen is 50-100 meshes.
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CN109174001A (en) * | 2018-10-17 | 2019-01-11 | 南方科技大学 | A kind of modified method lichee charcoal preparation and reduce oestrone in water body using it of calcium |
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