CN109794216A - A kind of preparation of nano adsorption material and its application in repairing heavy metal in soil pollution - Google Patents

A kind of preparation of nano adsorption material and its application in repairing heavy metal in soil pollution Download PDF

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CN109794216A
CN109794216A CN201910147609.4A CN201910147609A CN109794216A CN 109794216 A CN109794216 A CN 109794216A CN 201910147609 A CN201910147609 A CN 201910147609A CN 109794216 A CN109794216 A CN 109794216A
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adsorbent material
soil
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刘学平
李静玲
刘敏毅
柳燕梅
肖自强
余根鼎
刘志鹏
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Fujian University of Technology
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Abstract

The invention belongs to field of material technology, and in particular to a kind of nanometer Fe3O4@SiO2The preparation of adsorbent material and its application in repairing heavy metal in soil pollution.The present invention is, with cetyl trimethylammonium bromide (CTAB) for template, the Fe with preferable absorption property to be prepared using sol-gel method respectively using silica-base materials such as cullet, mine tailings, flyash, diatomite, bentonites as raw material3O4@SiO2Hydrophobic material can be used for the reparation of the heavy metal contaminants such as Cd in soil and water body.While realizing reclamation of solid wastes, soil pollution repair materials of good performance can be prepared.

Description

A kind of nano adsorption material is prepared and its in repairing heavy metal in soil pollution Using
Technical field
The invention belongs to field of material technology, and in particular to a kind of nanometer Fe3O4@SiO2The preparation of adsorbent material and its Application in repairing heavy metal in soil pollution.
Background technique
According to " the national Soil Pollution Investigation bulletin " of publication in 2014, soil total exceeding standard rate in China's is 16.1%, For pollution type based on inorganic heavy metal pollutant, exceeded digit accounts for the 82.8% of all exceeded points.For raw with the mankind Closely bound up arable soil living, 19.4% heavy metals exceeding standard.Therefore, under conditions of not changing soil original structure, how fastly Heavy metal contaminants in fast effective removal soil, become the Hot Contents of current research.
The toxicity of heavy metal in soil is related with its form, by applying passivator to reduce the biological effectiveness of heavy metal As research hotspot in recent years.In-situ chemical passivating method is in cost and can preferably meet heavy-metal contaminated soil on the time It repairs and requires, be more applicable for the improvement of farmland pollution soil, especially combined contamination soil, and to passivator in this technology Selection be crucial.The materials such as clay mineral, phosphate, silicate, diatomite, zeolite, charcoal, humic acid can be applied to Heavy metal pollution of soil reparation, the common feature of such material are that have unique three-dimensional space framework, and surface has a large amount of The highly developed gap structure such as micropore, cavity, channel, makes it have huge specific surface area, has very big suction to ion Attached capacity and exchange capacity, it is considered to be preferable heavy metal pollution repair materials.But natural surroundings material repairing effect is not high The shortcomings that also limit its popularization and application.
With the development of nano material subject, mesoporous nano SiO2There is better passivation effect to heavy metal.Have more Report mesoporous SiO2Application in water body medium: mesoporous SiO2There is preferable adsorption effect to heavy metal ion, especially passes through The mesoporous SiO of functional modification2Better choice is adsorbed with to heavy metal ion.Also some scholars report in soil To the passivation effect of heavy metal contaminants in medium: mesoporous SiO2There is certain passivation effect to heavy metal-polluted soil, can effectively drop Low soil exchangeable species, the concentration of carbonate combine state and iron and manganese oxides reference state, hence it is evident that inhibit heavy metal in the soil Migration and bioactivity.But mesoporous SiO2Heavy metal contaminants can not be removed from soil, be only capable of reducing the life of heavy metal Object activity.
The present invention passes through the modified mesoporous SiO of load Fe2Magnetism, Fe can be made it have3O4@SiO2Heavy metal pollution can be carried Object is separated with the realization of soil particle.And due to higher dispersibility, repairing effect is better than mesoporous nano SiO2.But existing skill Art scheme: there has been no prepare Fe using cullet3O4@SiO2Adsorbent material and the registration for being applied to repairing heavy metal in soil pollution.
Summary of the invention
The purpose of the present invention is to provide a kind of nanometer Fes3O4@SiO2The preparation of adsorbent material and its rehabilitating soil a huge sum of money Belong to the application in pollution.The present invention is respectively with silica-base materials such as cullet, mine tailings, flyash, diatomite, bentonites for original Material is prepared using sol-gel method with preferable adsorptivity with cetyl trimethylammonium bromide (CTAB) for template The Fe of energy3O4@SiO2Hydrophobic material can be used for the reparation of the heavy metal contaminants such as Cd in soil and water body.Realizing that solid is useless While object recycling, soil pollution repair materials of good performance can be prepared.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of nanometer Fe3O4@SiO2The preparation method of adsorbent material, comprising the following steps:
1. the preparation of silicon source: silica-base material being pulverized, is sieved with 100 mesh sieve, 10g is taken to be placed in a beaker, adds 25wt% sulfuric acid 50mL, in 90 DEG C of stirring and pickling 6h, centrifugal filtration;Filter residue, which is placed in iron crucible, is added 10~20g sodium hydroxide, stirs evenly, And it is covered with 0.5 ~ 1g sodium hydroxide;500 DEG C of calcining 1h in Muffle furnace are placed in, are dissolved after calcining with 10 ~ 50mL waste water, from Heart filtering, filtrate are spare as silicon source.
2. the preparation of source of iron: taking the FeCl of 24g3•6H2The FeCl of O and 9.6g2•4H2O is dissolved in 50mL deionized water, is made It is spare for source of iron.
③Fe3O4@SiO2Preparation: will 1. and 2. be mixed and added into 5g cetyl trimethylammonium bromide (CTAB), and add water To 150mL, stirring is to being completely dissolved;After hydrochloric acid solution is added dropwise pH is adjusted to 8, have black solid precipitation, continue to stir 18h;It is transferred in the ptfe autoclave with stainless steel protection set, it is closed to be placed in 100 DEG C of crystallization 2h in baking oven, it takes out cold But to room temperature, black solid becomes brownish red;Neutrality is filtered and is washed till, solid is placed in crucible, is placed in Muffle furnace and is forged for 550 DEG C 3h is burnt to get nanometer Fe3O4@SiO2
The silica-base material is one of cullet, mine tailings, bentonite, diatomite or several.
Wherein using cullet as silica-base material, acid cleaning process can be omitted.
According to silica-base material SiO2Content determines whole sodium hydroxide additive amounts, SiO2It is 1: 2 with NaOH mass ratio.
Step 3. according to SiO in silica-base material2Content determine, Fe3O4With SiO2Molar ratio between 1: 17.5~1: Between 70.
The non-modified silica-base material such as cullet of the present invention, since specific surface area is small, adsorption capacity is very poor, right The heavy metal contaminants such as the Cd in water, and such as can be to environmental danger without proper treatment without obvious clean-up effect;By modification, SiO2It is coated on Fe3O4On, form Fe3O4@SiO2Composite nano materials have cellular structure and bigger serface, to a huge sum of money The adsorption capacity for belonging to pollutant greatly improves, and has magnetism, can be separated from soil by magnetic separation;Work as Fe3O4With SiO2 Compositely proportional (molar ratio) between 1: 17.5~1: 70 when, primary repair is more than to the remediation efficiency of the heavy metals such as Cd in water 90%, the passivation effect to the heavy metals such as biologically effective state Cd in soil is more than 20%, and better than commercial nano silica (MCM- 41) and self-control MCM-41.Therefore by the Fe3O4@SiO2Composite material, which is applied to rehabilitating soil and heavy metal pollution of water body, has weight Big meaning.
Remarkable advantage of the invention is:
(1) preparation method simple process of the present invention, easily controllable, low in cost;
(2) raw material of the invention can be wide with silica-base materials, sources such as cullet, mine tailings, flyash, diatomite, bentonites It is general, and cullet, mine tailings, flyash etc. belong to solid waste, such as can generate significant damage, this hair to environment without processing The recycling of bright achievable silicon substrate solid waste;
(3) Fe prepared by the present invention3O4@SiO2Composite material, by SiO2It is coated on Fe3O4On, remain Nano-meter SiO_22Hole Road structure and bigger serface, increase magnetism, considerably increase its separability in the soil, are applied to rehabilitating soil weight Metallic pollution inhibits the separation that heavy metal and soil are realized while bioavailability of heavy metals;Because utilizing Nano-meter SiO_22 Repairing heavy metal in soil pollution is only capable of inhibiting heavy metal biological activity, can not remove heavy metal from soil, the present invention can make Part heavy metal contaminants are separated with soil, and efficiency is better than Nano-meter SiO_22
(4) Fe prepared by the present invention3O4@SiO2Composite material has the heavy metal contaminants in soil and water body good Repairing effect, and nanometer Fe3O4Presence inhibit Nano-meter SiO_22Reunion, make its dispersibility improve, the reparation to pollutant Effect is better than commercialization SiO2(MCM-41) and self-control MCM-41.
Detailed description of the invention
Fig. 1 is the Fe for different Si, Fe ratios (molar ratio) prepared3O4@SiO2Photo;
The SiO that Fig. 2 is prepared2With Fe3O4@SiO2XRD diffraction pattern;
Fig. 3 Fe3O4@SiO2Nitrogen adsorption-desorption isotherm and pore-size distribution;
Fig. 4 Fe3O4@SiO2Solid powder specific surface area;
SiO in Fig. 5 water phase2With Fe3O4@SiO2Particle diameter distribution;
Fig. 6 nanometer Fe3O4@SiO2To the repairing effect of different initial Cd concentration water bodys;
Fig. 7 nanometer Fe3O4@SiO2To a repairing effect of biologically effective state Cd pollutant in soil.
Specific embodiment
Further to disclose rather than the present invention is limited, the present invention is described in further detail below in conjunction with example.
Embodiment 1
A kind of nanometer Fe3O4@SiO2The preparation method of adsorbent material, comprising the following steps:
1. the preparation of silicon source: cullet is pulverized, is sieved with 100 mesh sieve, takes 10g to be placed in iron crucible and 19g sodium hydroxide is added, It stirs evenly, and is covered with 1g sodium hydroxide;500 DEG C of calcining 1h in Muffle furnace are placed in, are dissolved after calcining with 50mL waste water, Centrifugal filtration, filtrate are spare as silicon source.
2. the preparation of source of iron: taking the FeCl of 24g3•6H2The FeCl of O and 9.6g2•4H2O is dissolved in 50mL deionized water, is made It is spare for source of iron.
③Fe3O4@SiO2Preparation: will 1. and 2. be mixed and added into 5g cetyl trimethylammonium bromide (CTAB), and add water To 150mL, stirring is to being completely dissolved;After hydrochloric acid solution is added dropwise pH is adjusted to 8, have black solid precipitation, continue to stir 18h;It is transferred in the ptfe autoclave with stainless steel protection set, it is closed to be placed in 100 DEG C of crystallization 2h in baking oven, it takes out cold But to room temperature, black solid becomes brownish red;Neutrality is filtered and is washed till, solid is placed in crucible, is placed in Muffle furnace and is forged for 550 DEG C 3h is burnt to get nanometer Fe3O4@SiO2
Embodiment 2
1. the preparation of silicon source: by certain bauxite gangue (SiO2Content 51wt%) it pulverizes, it sieves with 100 mesh sieve, 10g is taken to be placed in burning In cup, add 25wt% sulfuric acid 50mL, in 90 DEG C of stirring and pickling 6h, centrifugal filtration;Filter residue, which is placed in iron crucible, is added 10g hydroxide Sodium stirs evenly, and is covered with 0.5g sodium hydroxide;500 DEG C of calcining 1h in Muffle furnace are placed in, 50mL waste water is used after calcining Dissolution, centrifugal filtration, filtrate are spare as silicon source.
2. the preparation of source of iron: taking the FeCl of 24g3•6H2The FeCl of O and 9.6g2•4H2O is dissolved in 50mL deionized water, is made It is spare for source of iron.
③Fe3O4@SiO2Preparation: will 1. and 2. be mixed and added into 5g cetyl trimethylammonium bromide (CTAB), and add water To 150mL, stirring is to being completely dissolved;After hydrochloric acid solution is added dropwise pH is adjusted to 8, have black solid precipitation, continue to stir 18h;It is transferred in the ptfe autoclave with stainless steel protection set, it is closed to be placed in 100 DEG C of crystallization 2h in baking oven, it takes out cold But to room temperature, black solid becomes brownish red;Neutrality is filtered and is washed till, solid is placed in crucible, is placed in Muffle furnace and is forged for 550 DEG C 3h is burnt to get nanometer Fe3O4@SiO2
Embodiment 3
1. the preparation of silicon source: by bentonite (SiO2Content 86wt%) it pulverizes, it sieves with 100 mesh sieve, 10g is taken to be placed in a beaker, add 25wt% sulfuric acid 50mL, in 90 DEG C of stirring and pickling 6h, centrifugal filtration;Filter residue, which is placed in iron crucible, is added 17g sodium hydroxide, stirring Uniformly, and with 0.5g sodium hydroxide it covers;500 DEG C of calcining 1h in Muffle furnace are placed in, are dissolved after calcining with 50mL waste water, from Heart filtering, filtrate are spare as silicon source.
2. the preparation of source of iron: taking the FeCl of 24g3•6H2The FeCl of O and 9.6g2•4H2O is dissolved in 50mL deionized water, is made It is spare for source of iron.
③Fe3O4@SiO2Preparation: will 1. and 2. be mixed and added into 5g cetyl trimethylammonium bromide (CTAB), and add water To 150mL, stirring is to being completely dissolved;After hydrochloric acid solution is added dropwise pH is adjusted to 8, have black solid precipitation, continue to stir 18h;It is transferred in the ptfe autoclave with stainless steel protection set, it is closed to be placed in 100 DEG C of crystallization 2h in baking oven, it takes out cold But to room temperature, black solid becomes brownish red;Neutrality is filtered and is washed till, solid is placed in crucible, is placed in Muffle furnace and is forged for 550 DEG C 3h is burnt to get nanometer Fe3O4@SiO2
Repairing performance test method:
1. 100 mesh nylon mesh are crossed in 60 DEG C of pedotheque drying, grinding.Existed using European Community's canonical measure and detection office (SM&T) It is standardized on the basis of Tessier method and improved method-improvement BCR fractional extraction method is to heavy metals such as Cd in soil The forms such as biologically effective state extract, obtain extracting solution;Using " resolution of soils and sediments metallic element total amount is micro- Wave resolution method " (HJ 832-2017) clear up the heavy metals such as Cd in soil, digestion solution is obtained to measure its total amount.
2. measuring the weight such as Cd in extracting solution, digestion solution or water sample using icp ms (ICP-MS) The content of metal.
Fig. 1 is the Fe for different Si, Fe ratios (molar ratio) prepared3O4@SiO2, (a) is pure Nano-meter SiO_22, white powder End, it is nonmagnetic;(b)~(f) is compound Fe3O4Fe afterwards3O4@SiO2, Si, Fe molar ratio is respectively as follows: 70: 1,35: 1,23.3: 1, 17.5: 1,7: 1, brown ceramic powder, with Fe3O4The increase of content, product colour are deepened, and magnetism is reinforced.
The SiO that Fig. 2 is prepared2With Fe3O4@SiO2XRD diffraction pattern, with standard X-ray diffraction standard card compare :(a) For SiO2, 2θ=23.3 ° there are an apparent wide diffraction maximum, this is the characteristic diffraction peak of amorphous silica, without other Miscellaneous peak illustrates the Nano-meter SiO_2 prepared2Pure free from admixture.It (b) is Fe3O4@SiO2, 2θIt is=23.3 ° apparent wide there are one Diffraction maximum, this is the characteristic diffraction peak of amorphous silica;2θ=35.4 ° there are a sharp diffraction maximum, be Fe3O4 Characteristic peak, the peak type is sharp, illustrates Fe3O4Structure is than more complete;Without other miscellaneous peaks, illustrate the nanometer Fe prepared3O4@SiO2 Pure free from admixture.
Fig. 3 is Fe3O4@SiO2Nitrogen adsorption-desorption isotherm and graph of pore diameter distribution, (a) are Fe3O4@SiO2Nitrogen is inhaled Attached-desorption isotherm (b) is Fe3O4@SiO2Pore-size distribution.Fe3O4@SiO2Nitrogen adsorption-desorption isotherm is Lang Gemiaoer IV Type thermoisopleth, shows Fe3O4@SiO2Belong to typical mesoporous substance.It can be seen that adsorbance is with pressure in low-pressure area Increase slowly, N2Molecule is adsorbed on mesoporous inner surface with single layer to multilayer.When relative pressure is 0.3 to 0.4, Fe is carried3O4@ SiO2Capillary condensation N2Molecule fills up mesoporous, and adsorbance is sharply increased with relative pressure, when relative pressure further increases When, N2Molecule is adsorbed on mesoporous outer surface with single layer to multilayer.From the size degree of critical point value and prominent more part Steep and height can effectively judge the size and distribution situation in aperture.As can be seen from the figure critical point numeric ratio Larger, the curve for more section of dashing forward is not only high but also steep, this illustrates Fe3O4@SiO2Most probable pore size is big and pore-size distribution is narrow, concentrates on 4nm Left and right.In higher section of relative pressure p/p0Under, adsorbance is uprushed again, this is because capillary condensation occurs for adsorbate, works as institute When having hole to agglomerate, absorption is only carried out on the external surface area much smaller than internal surface area, and the desorption of the curve and absorption are not It is overlapped, is also due to and hysteresis caused by capillary condensation occurs.
Fig. 4 is to measure Fe using specific surface area measuring instrument3O4@SiO2The specific surface area of solid powder, the results showed that, this hair The nanometer Fe of bright synthesis3O4@SiO2Specific surface area is suitable with commercialization MCM-41 specific surface area, with the increase ratio of material Fe content Surface area is slightly reduced, but magnetic enhancement, is enhanced with the magnetic separation separating property of soil.
Fig. 5 is to measure the SiO prepared using laser testing instrument2With Fe3O4@SiO2Particle diameter distribution in water phase, as a result Show nanometer Fe3O4@SiO2Partial size not because of compound Fe3O4Its partial size is set to become larger, partial size becomes smaller instead, this is because Fe3O4 Presence, increase the repulsion between nanoparticle, it is suppressed that SiO2Reuniting effect, increase in the soil liquid or water body Dispersibility.And dispersibility is directly proportional to its specific surface area and absorption property, therefore nanometer Fe3O4@SiO2Absorption property better than pure Nano-meter SiO_22
Fig. 6 tests the nanometer Fe of preparation3O4@SiO2Repairing initial concentration is respectively 5,50 μ gL-1Cd polluted-water, The nanometer Fe of the different mol ratio of preparation3O4@SiO2Remediation efficiency be all larger than commercial Nano-meter SiO_22(MCM-41), to heavy metal Repairing performance it is good, remediation efficiency can be more than 90%.
Fig. 7 is the nanometer Fe that different quality is added into soil3O4@SiO2To the reparation effect of biologically effective state Cd pollutant Fruit, additive amount (soil and Fe3O4@SiO2Mass ratio) it is respectively as follows: 1: 0.5,1: 1.0,1: 1.5,1: 2.0.Nanometer is added into soil Fe3O4@SiO2It carries out after once repairing, the content of biologically effective state Cd is reduced in soil, and remediation efficiency is about 25%, nanometer Fe3O4@SiO2The influence of additive amount is little, can be by adding on a small quantity, and the mode repeatedly repaired improves remediation efficiency.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with Modification, is all covered by the present invention.

Claims (9)

1. a kind of nanometer Fe3O4@SiO2The preparation method of adsorbent material, it is characterised in that: using silica-base material as raw material, with 16 Alkyl trimethyl ammonium bromide CTAB is template, and the Fe with preferable absorption property is prepared using sol-gel method3O4@ SiO2Hydrophobic material.
2. a kind of nanometer Fe according to claim 13O4@SiO2The preparation method of adsorbent material, it is characterised in that: specific The following steps are included:
1. the preparation of silicon source: silica-base material being pulverized, is sieved with 100 mesh sieve, 10g is taken to be placed in a beaker, adds 25wt% sulfuric acid 50mL, in 90 DEG C of stirring and pickling 6h, centrifugal filtration;Filter residue, which is placed in iron crucible, is added 10~20g sodium hydroxide, stirs evenly, And it is covered with 0.5 ~ 1g sodium hydroxide;It is placed in Muffle furnace and calcines, dissolved after calcining with 10 ~ 50mL waste water, centrifugal filtration, Filtrate is spare as silicon source;
2. the preparation of source of iron: taking the FeCl of 24g3•6H2The FeCl of O and 9.6g2•4H2O is dissolved in 50mL deionized water, as source of iron It is spare;
③Fe3O4@SiO2Preparation: will 1. and 2. be mixed and added into 5g cetyl trimethylammonium bromide CTAB, add water to 150mL, stirring is to being completely dissolved;After hydrochloric acid solution is added dropwise pH is adjusted to 8, have black solid precipitation, continue to stir 18h;It is transferred in the ptfe autoclave with stainless steel protection set, closed to be placed in crystallization in baking oven, taking-up is cooled to room Temperature, black solid become brownish red;Neutrality is filtered and is washed till, solid is placed in crucible, is placed in Muffle furnace and is calcined to get nanometer Fe3O4@SiO2
3. a kind of nanometer Fe according to claim 13O4@SiO2The preparation method of adsorbent material, it is characterised in that: step 1. silica-base material described in is one of cullet, mine tailings, bentonite, diatomite or several.
4. a kind of nanometer Fe according to claim 13O4@SiO2The preparation method of adsorbent material, it is characterised in that: step According to silica-base material SiO in 1.2Content determines whole sodium hydroxide additive amounts, SiO2It is 1: 2 with NaOH mass ratio.
5. a kind of nanometer Fe according to claim 13O4@SiO2The preparation method of adsorbent material, it is characterised in that: step The actual conditions calcined in 1. are as follows: 500 DEG C of calcining 1h.
6. a kind of nanometer Fe according to claim 13O4@SiO2The preparation method of adsorbent material, it is characterised in that: step According to SiO in silica-base material in 3.2Content determine, Fe3O4With SiO2Molar ratio between 1: 17.5~1: 70.
7. a kind of nanometer Fe according to claim 13O4@SiO2The preparation method of adsorbent material, it is characterised in that: step 3. middle crystallization specifically: closed to be placed in 100 DEG C of crystallization 2h in baking oven.
8. a kind of nanometer Fe according to claim 13O4@SiO2The preparation method of adsorbent material, it is characterised in that: step 3. calcining is specially 550 DEG C of calcining 3h in.
9. a kind of nanometer Fe of method preparation as described in claim 13O4@SiO2Adsorbent material is polluted in repairing heavy metal in soil In application.
CN201910147609.4A 2019-02-27 2019-02-27 A kind of preparation of nano adsorption material and its application in repairing heavy metal in soil pollution Pending CN109794216A (en)

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CN111013526B (en) * 2019-11-18 2022-02-11 昆明理工大学 Antimony tailing based adsorption material and preparation method and application thereof
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CN111872101B (en) * 2020-07-23 2021-12-14 西南科技大学 Method for treating strontium in soil by using montmorillonite/carbonate mineralized bacteria aggregates
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CN112480930A (en) * 2020-12-10 2021-03-12 广东省科学院资源综合利用研究所 Preparation method of magnetic soil heavy metal restoration agent, heavy metal restoration agent and application
CN113265258A (en) * 2021-05-03 2021-08-17 黑龙江顿丰微纳米硅科技开发有限公司 Additive capable of reducing heavy metals in soil
CN113403083A (en) * 2021-05-08 2021-09-17 华南师范大学 Magnetic soil remediation agent for soil polluted by heavy metals and preparation method and application thereof
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CN113621376A (en) * 2021-07-21 2021-11-09 湖南农业大学 Soil conditioner, preparation method thereof and soil conditioning method
CN113617329A (en) * 2021-08-18 2021-11-09 上海海洋大学 Mesoporous Fe3O4One-step preparation of composite adsorbent and application thereof in treating As (III) -containing aqueous solution
CN114789193A (en) * 2022-02-17 2022-07-26 青岛理工大学 Method for repairing arsenic and antibiotic contaminated soil by bacteria and magnetic diatomite
CN114797792A (en) * 2022-05-25 2022-07-29 浙江树人学院 Preparation method and application of magnetic biochar-based composite adsorbent
CN114797792B (en) * 2022-05-25 2023-10-24 浙江树人学院 Preparation method and application of magnetic biochar-based composite adsorbent

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