CN109880629A - A kind of preparation method of soil remediation material - Google Patents
A kind of preparation method of soil remediation material Download PDFInfo
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Abstract
The present invention relates to soil remediation fields, are related to a kind of preparation method of soil remediation material.The natural attapulgite clay of the present invention is after peracid treatment, remove dolomite, the impurity such as calcium carbonate, weaken original intermolecular bonding force, duct is dredged, equally distributed gap is formd on surface, not only improve the absorption property of soil remediation material, also activation duct is provided for the load of nano zero valence iron, polyethyleneimine, which is tightly adsorbed on silica gel internal pore surface, may make up nanofiltration membrane, heavy metal ion is set to be adsorbed concentration, it being capable of efficient absorption heavy metal ion, Zero-valent Iron can increase the effective surface area of nano particle and enhance active site, strengthening electronic transfer, to improve adsorption efficiency, and Zero-valent Iron can exchange heavy metal in soil after being oxidized, metabolic pathway induction changes after the fixed iron ion of Rhodococcus coprophilus, secret out of more degradation soil organic pollutants, it has broad application prospects.
Description
Technical field
The present invention relates to soil remediation fields, are related to a kind of preparation method of soil remediation material.
Background technique
Currently, due to the development of industry and transportation, such as the exploitation of shale oil gas, the exploitation benefit of oil and coal
With the production of founding the factory in various chemical plant, soil pollution annoyings the developing countries and regions of developed country and high speed development, soil
Earth reparation becomes the challenge that these areas must solve.Country advanced for environmental protection, it is total that soil remediation industry accounts for environmental protection industry
The 30%~50% of volume, and currently substantially blank, market demand notch are very big for China.
The reason of causing soil pollution has very much, such as industrial sludge, agricultural garbage, sewage irrigation, pollutant in atmosphere
Sedimentation and a large amount of mineral chemical fertilizer and pesticide etc. using containing heavy metal.Soil after pollution will lead to crop production reduction, or even draw
Rise agricultural product in pollutant it is exceeded, be detrimental to health.
Soil remediation refers mainly to the method transfer using physics, chemistry and biology, absorbs, the dirt in degradation and conversion soil
Object is contaminated, so that its concentration is reduced to acceptable level, or convert poisonous and hazardous pollutant to harmless substance.Soil remediation is not
It is only capable of removing the heavy metal ion in soil, moreover it is possible to promote crop nutrition content to absorb, caused by because of excessive application chemicals
Certain reparation and improvement result are played in soil damage.
Heavy metal pollution at present and persistence organic pollutant (POPs) are serious to soil harm, in organic pollutant more
Common and concerned POPs mainly has PAHs, PBDEs, PCBs etc..These organic pollutants can enter big through a variety of ways
In gas and water body and soil, by a series of Transport And Transformations, potential threat is formed to organism and human health.
Many processing modes require to improve repairing effect using organic renovation agent.Organic renovation agent is primarily referred to as containing
A kind of compound of carbon, hydrogen plays a part of to be complexed in the reparation of heavy metal pollution of soil, shuts off, fixes heavy metal contaminants,
And the organic renovation agent in part is to biology also certain detoxication.It continues to bring out, answers with new technology with advances in technology
New formulation for soil pollution reparation is increasing, and important function has been played in soil environment protection.
But this single recovery technique shows its defective in the application.In-situ chemical passivating technique is because of its operation letter
Just, drop cadmium is quick, at present using more.Its principle of in-situ chemical passivating technique is that a certain amount of passivation is applied into soil
Agent, the effects of generating precipitating, absorption using the ionic state heavy metal in passivator and soil, be complexed, by the heavy metal in soil
It is the lower form of bioavailability by the higher Morphological Transitions of bioavailability, reduces the mobility and poison of heavy metal
Property, avoid the injury to human health.In using chemical passivation technology governance heavy metals in farmland pollution course, if infused simply
Weight its passivation effect to heavy metal, be passivated agent material selection in terms of ignore its secondary pollution or because blunt
Agent use and cause the very big change to this specific environment of agricultural land soil, cause native plants to be difficult to adapt to and can not be normal
Growth or existence.
Currently, various organic pollutants and various heavy metal contaminants in soil can be removed simultaneously by needing to invent, and
And the organic matter in soil is not damaged, and the cost of soil remediation is low, easy to use.
Summary of the invention
Present invention mainly solves the technical issues of, it is single for current soil remediation material efficacy, to heavy metal in soil
The poor defect of the decomposition efficiency of adsorption effect and organic pollutant, provides a kind of preparation method of soil remediation material.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of soil remediation material the preparation method comprises the following steps:
Modified silica-gel to be immersed in the polyethylenimine solution that mass fraction is 20%, impregnates 10~12min, filtering removes filtrate,
Collection obtains Bio-sil, and Bio-sil is laid down into funnel filtering surface, will load the clay and the red ball of thermophilic excrement of nano zero valence iron
Bacterium powder is 20 ︰ 1 mixing, then the water-dispersible water slurry for being configured to mass fraction and being 5% in mass ratio, which is fallen
Enter to lay in the funnel of Bio-sil, carry out filtering and washing, takes out Bio-sil, be granulated after dry and silica-gel sphere is made to get soil
Earth repair materials；
Modified silica-gel the preparation method comprises the following steps:
(1) taking 100~120mL mass fraction is that 30% sodium silicate solution pours into the three-necked flask with blender, uses quality
The salt slow acid that score is 10% adjusts pH to 6~7, starts blender, stirs 30~40min with 350~400r/min revolving speed,
Microwave oscillation handles 3~5min, obtains nano-sized hydrosol, nano-sized hydrosol is put into baking oven and is heated to 80~85 DEG C,
Dry 3~4h, obtains nanometer silica gel；
(2) it weighs 200~220g nanometer silica gel to be placed in the Loprazolam aqueous solution that 400~450mL mass fraction is 40%, control
Temperature processed is 50~55 DEG C, stirs 20~30min, obtains activated silica gel, activated silica gel and r-chloropropyl trimethoxyl silane are pressed
Mass ratio is 2 ︰ 1 mixing, obtains reaction mass, 200~250g reaction mass is placed in 400~420mL dimethylbenzene and reacts 40
~45min obtains modified silica-gel, spare；
Load nano zero valence iron clay the preparation method comprises the following steps:
(1) it by attapulgite clay with salt acid dip 2~3 days, is then shaken in ultrasonic treatment machine with the frequency ultrasound of 25~30kHz
Swing 20~30min, filtering removal filtrate, then deionized water repeated flushing is used, set temperature is subsequently placed into as 200~300 DEG C
Dry 3~4h, crosses 200 meshes, obtains activated clay in baking oven；
(2) activated clay and green-vitriol are mixed, is added in the conical flask equipped with deionized water, mechanical stirring 20~
It uses magnetic stirrer after 25min instead, and is passed through nitrogen protection, taper is added in above-mentioned sodium borohydride solution dropping funel
In bottle, control dropping funel drop speed is 4~5mL/min, and 40~45min of reduction reaction obtains reduzate；
(3) above-mentioned reduzate is placed in supercentrifuge and is centrifugated with the revolving speed of 4500~5000r/min, collect lower layer
Obtained solid is washed 3~4 times with dehydrated alcohol and is placed on vacuum in the vacuum oven that set temperature is 50~60 DEG C by solid
Dry 6~7h, sieving obtain the clay of load nano zero valence iron.
The clay and Rhodococcus coprophilus powder mixing mass ratio for loading nano zero valence iron are 20 ︰ 1.
Filtering and washing process, pressure is maintained at 0.25~0.30MPa when should control suction filtration, and further can be to more in funnel
Hole silica gel carries out turn-over, and clay and bacterium powder is enable uniformly to be adsorbed in Silica Surface.
Setting microwave oscillation frequency when microwave oscillation is handled in the preparation method of modified silica-gel in the preparation method of modified silica-gel
Rate is 23~25kHz.
Activated silica gel and r-chloropropyl trimethoxyl silane mixing mass ratio are 2 ︰ 1 in the preparation method of modified silica-gel.
The salt acid mass fraction for loading dipping attapulgite clay in the clay preparation method of nano zero valence iron is 5%, clay warp
Cleaning solution should be in neutrality after crossing deionized water repeated flushing.
Loading activated clay and green-vitriol mixing mass ratio in the clay preparation method of nano zero valence iron is preferably 2 ︰
5, sodium borohydride solution is obtained by being dissolved in prepare in 500mL deionized water by 4~5g sodium borohydride.
The clay preparation method high speed centrifuge speed for loading nano zero valence iron is 4500~5000r/min, and load is received
The clay of rice Zero-valent Iron is chosen to obtain through 200 meshes.
The beneficial effects of the present invention are:
(1) sodium silicate solution microwave oscillation is prepared nanometer silica gel by the present invention, then with Loprazolam activated in water solution nanometer silica gel,
By activated silica gel and r-chloropropyl trimethoxyl silane hybrid reaction, chloromethylation is carried out, modified silica-gel is obtained, by attapulgite clay
With sonic oscillation processing is carried out after hydrochloric acid impregnating active, activated clay is washed and is dried to obtain, then by activated clay and seven water
Ferric sulfate mixing, and so that nano zero valence iron is carried on attapulgite clay with sodium borohydride solution reduction, modified silica-gel is immersed poly-
In aziridine solution, Bio-sil is obtained, water slurry is made in the clay for loading nano zero valence iron and Rhodococcus coprophilus powder
To Bio-sil pressurization filtering and washing, soil remediation material is prepared, the present invention is mentioned using natural attapulgite clay crystal
The absorption property of high soil remediation material, it is interacted due to electrostatic attraction and hydrogen bond, it is difficult to which dissociation and dispersion are changed by acid
Property slightly mention to increase its surface area, the shearing force and cavitation generated using sonic oscillation reduces electrostatic attraction and hydrogen bond is mutual
The dissociation of stick crystalline substance beam is realized in effect, and attapulgite clay itself is that brilliant beam is arranged as by bar-like single crystal close parallel, brilliant beam and phase
Mutually aggregation forms attapulgite clay particle, and surface forming part hole, the activated clay monocrystalline arrangement obtained after slightly mentioning is more
Independent dispersion, surface porosity is porous, this is because after peracid treatment, the impurity such as removal dolomite, calcium carbonate are weakened original
Intermolecular bonding force, duct are dredged, and are formd equally distributed gap on surface, are not only increased the suction of soil remediation material
Attached performance also provides activation duct for the load of nano zero valence iron；
(2) modified silica-gel is soaked in polyethylenimine solution by the present invention can obtain chelate adsorption, and polyethyleneimine is
A kind of water solubility polyamine, possesses a large amount of amido atom in linear macromolecule chain, polyethyleneimine is tightly adsorbed on silica gel hole
Inner surface can generate very strong chelation to metal ion, and Bio-sil is coated on load nanometer zero after filtering and washing
The surface of clay of valence iron constitutes nanofiltration membrane, can adsorb and be combined with other heavy metal cations in solution, make heavy metal ion
Be adsorbed concentration, can efficient absorption heavy metal ion, and organic pollutant will not be discharged, due to existing in attapulgite clay
A large amount of hydroxy functional group, when soil remediation material of the invention is imposed in the soil containing heavy metal ion, hydroxyl and metal
Complexing occurs for ion, and there are a large amount of NA for attapulgite clay interlayer+、K+、Mg2+Commutative inorganic cation is by metal ion
Replace occur ion exchange, or its surface carry out adsorption reaction, from lime fixative absorption fixation principle it is different, it by
Soil pH influence is smaller, and attapulgite clay passes through modified, the Si in tetrahedral structure4+By Al3+Substitution displacement, leads to bumps
Stick clay is negatively charged, and electrostatic interaction can occur when contacting with positively charged heavy metal ion, the suction to heavy metal contaminants
Attached activity improves, and nano zero valence iron of the present invention is by the material of appearance iron oxide shell package metallic iron core, metallic iron core
Electron-withdrawing group strength can be reduced, surface iron hydroxide provides coordination and electrostatic attraction and absorption charged ion function, possesses thin
Have the shortcomings that deficient in stability and easy to reunite while partial size and high surface area, influences the using effect of nano zero valence iron, be
The reunion for avoiding particle, distributes it to solid supported in attapulgite clay, can increase the effective surface area of nano particle
And enhance active site, strengthening electronic transfer, to improve adsorption efficiency, and Zero-valent Iron be oxidized after can exchange in soil
Heavy metal, metabolic pathway induction changes after Rhodococcus coprophilus fixes iron ion, secrets out of more degradation soil organic contaminations
Object has broad application prospects.
Specific embodiment
Taking 100~120mL mass fraction is that 30% sodium silicate solution pours into the three-necked flask with blender, uses matter
Measure score be 10% salt slow acid adjust pH to 6~7, start blender, with 350~400r/min revolving speed stirring 30~
40min, microwave oscillation handle 3~5min, set microwave oscillation frequency as 23~25kHz, obtain nano-sized hydrosol, by nanometer water
Colloidal sol, which is put into baking oven, is heated to 80~85 DEG C, and dry 3~4h obtains nanometer silica gel；Weigh 200~220g nanometer silica gel
It is placed in the Loprazolam aqueous solution that 400~450mL mass fraction is 40%, controlled at 50~55 DEG C, stirring 20~
30min obtains activated silica gel, with r-chloropropyl trimethoxyl silane is in mass ratio that 2 ︰ 1 are mixed by activated silica gel, obtains reactant
200~250g reaction mass is placed in 40~45min of reaction in 400~420mL dimethylbenzene, obtains modified silica-gel by material, spare；
By salt acid dip 2~3 days that attapulgite clay mass fraction is 5%, then with 25~30kHz in ultrasonic treatment machine
Frequency ultrasound vibrate 20~30min, filtering removal filtrate then is in neutrality, then with deionized water repeated flushing to cleaning solution
It is put into dry 3~4h in the baking oven that set temperature is 200~300 DEG C, 200 meshes is crossed, obtains activated clay；By activated clay and
Green-vitriol is 2 ︰ 5 according to mass ratio, is added in the conical flask equipped with deionized water, changes after 20~25min of mechanical stirring
With magnetic stirrer, and it is passed through nitrogen protection, 4~5g sodium borohydride is taken to be dissolved in prepare in 500mL deionized water and obtain
Above-mentioned sodium borohydride solution dropping funel is added in conical flask sodium borohydride solution, control dropping funel drop speed for 4~
5mL/min, 40~45min of reduction reaction, obtains reduzate；Above-mentioned reduzate is placed in supercentrifuge with 4500~
The revolving speed of 5000r/min is centrifugated, and collects lower layer's solid, obtained solid is washed 3~4 times with dehydrated alcohol and is placed on setting
It is dried in vacuo 6~7h in the vacuum oven that temperature is 50~60 DEG C, crosses 200 meshes, obtains the clay of load nano zero valence iron；
Modified silica-gel is immersed in the polyethylenimine solution that mass fraction is 20%, impregnate 10~12min, filtering removal filtrate is collected
Bio-sil is obtained, Bio-sil is laid down into funnel filtering surface, the clay and Rhodococcus coprophilus powder of nano zero valence iron will be loaded
It is mixed in mass ratio for 20 ︰ 1, then the water-dispersible water slurry for being configured to mass fraction and being 5%, which is poured into paving
It sets in the funnel of Bio-sil, filtering and washing is carried out with the pressure of 0.25~0.30MPa, take out Bio-sil, be granulated after dry
Silica-gel sphere is made to get soil remediation material.
The preparation of modified silica-gel: taking 100mL mass fraction is that 30% sodium silicate solution pours into three mouthfuls of burnings with blender
In bottle, pH to 6 is adjusted with the salt slow acid that mass fraction is 10%, starts blender, 30min is stirred with 350r/min revolving speed, it is micro-
Wave oscillation treatment 3min sets microwave oscillation frequency as 23kHz, obtains nano-sized hydrosol, nano-sized hydrosol is put into baking oven
80 DEG C are heated to, dry 3h obtains nanometer silica gel；
200g nanometer silica gel is weighed to be placed in the Loprazolam aqueous solution that 400mL mass fraction is 40%, controlled at 50 DEG C,
20min is stirred, activated silica gel is obtained, with r-chloropropyl trimethoxyl silane is in mass ratio that 2 ︰ 1 are mixed by activated silica gel, is obtained instead
Material is answered, 200g reaction mass is placed in 400mL dimethylbenzene and reacts 40, obtains modified silica-gel, it is spare；
Load the preparation of the clay of nano zero valence iron:
It is then super with the frequency of 25kHz in ultrasonic treatment machine by salt acid dip 2 days that attapulgite clay mass fraction is 5%
Sound oscillation 20min, filtering removal filtrate, then be in neutrality with deionized water repeated flushing to cleaning solution, it is subsequently placed into set temperature
For 3h dry in 200 DEG C of baking ovens, 200 meshes are crossed, activated clay is obtained；
According to mass ratio it is 2 ︰ 5 by activated clay and green-vitriol, is added in the conical flask equipped with deionized water, machinery stirs
Magnetic stirrer is used instead after mixing 20min, and is passed through nitrogen protection, and 4g sodium borohydride is taken to be dissolved in 500mL deionized water
Preparation obtains sodium borohydride solution, and above-mentioned sodium borohydride solution dropping funel is added in conical flask, control dropping funel drop
Speed is 4mL/min, and reduction reaction 40min obtains reduzate；
Above-mentioned reduzate is placed in supercentrifuge and is centrifugated with the revolving speed of 4500r/min, lower layer's solid is collected, by institute
Solid wash to be placed on for 3 times in the vacuum oven that set temperature is 50 DEG C with dehydrated alcohol and is dried in vacuo 6h, 200 mesh of mistake
Sieve obtains the clay of load nano zero valence iron；
The preparation of soil remediation material:
Modified silica-gel is immersed in the polyethylenimine solution that mass fraction is 20%, impregnate 10min, filtering removal filtrate is collected
Bio-sil is obtained, Bio-sil is laid down into funnel filtering surface, the clay and Rhodococcus coprophilus powder of nano zero valence iron will be loaded
It is mixed in mass ratio for 20 ︰ 1, then the water-dispersible water slurry for being configured to mass fraction and being 5%, which is poured into paving
It sets in the funnel of Bio-sil, filtering and washing is carried out with the pressure of 0.25MPa, take out Bio-sil, be granulated after dry and silicon is made
Glueballs is to get soil remediation material.
The preparation of modified silica-gel: taking 115mL mass fraction is that 30% sodium silicate solution pours into three mouthfuls of burnings with blender
In bottle, pH to 7 is adjusted with the salt slow acid that mass fraction is 10%, starts blender, 35min is stirred with 360r/min revolving speed, it is micro-
Wave oscillation treatment 4min sets microwave oscillation frequency as 24kHz, obtains nano-sized hydrosol, nano-sized hydrosol is put into baking oven
83 DEG C are heated to, dry 4h obtains nanometer silica gel；
210g nanometer silica gel is weighed to be placed in the Loprazolam aqueous solution that 430mL mass fraction is 40%, controlled at 53. DEG C,
25min is stirred, activated silica gel is obtained, with r-chloropropyl trimethoxyl silane is in mass ratio that 2 ︰ 1 are mixed by activated silica gel, is obtained instead
Material is answered, 230g reaction mass is placed in 410mL dimethylbenzene and reacts 43min, obtains modified silica-gel, it is spare；
Load the preparation of the clay of nano zero valence iron:
It is then super with the frequency of 28kHz in ultrasonic treatment machine by salt acid dip 3 days that attapulgite clay mass fraction is 5%
Sound oscillation 25min, filtering removal filtrate, then be in neutrality with deionized water repeated flushing to cleaning solution, it is subsequently placed into set temperature
For 4h dry in 250 DEG C of baking ovens, 200 meshes are crossed, activated clay is obtained；
According to mass ratio it is 2 ︰ 5 by activated clay and green-vitriol, is added in the conical flask equipped with deionized water, machinery stirs
Magnetic stirrer is used instead after mixing 23min, and is passed through nitrogen protection, and 5g sodium borohydride is taken to be dissolved in 500mL deionized water
Preparation obtains sodium borohydride solution, and above-mentioned sodium borohydride solution dropping funel is added in conical flask, control dropping funel drop
Speed is 5mL/min, and reduction reaction 43min obtains reduzate；
Above-mentioned reduzate is placed in supercentrifuge and is centrifugated with the revolving speed of 4800r/min, lower layer's solid is collected, by institute
Solid wash to be placed on for 4 times in the vacuum oven that set temperature is 55 DEG C with dehydrated alcohol and is dried in vacuo 7h, 200 mesh of mistake
Sieve obtains the clay of load nano zero valence iron；
The preparation of soil remediation material:
Modified silica-gel is immersed in the polyethylenimine solution that mass fraction is 20%, impregnate 11min, filtering removal filtrate is collected
Bio-sil is obtained, Bio-sil is laid down into funnel filtering surface, the clay and Rhodococcus coprophilus powder of nano zero valence iron will be loaded
It is mixed in mass ratio for 20 ︰ 1, then the water-dispersible water slurry for being configured to mass fraction and being 5%, which is poured into paving
It sets in the funnel of Bio-sil, filtering and washing is carried out with the pressure of 0.28MPa, take out Bio-sil, be granulated after dry and silicon is made
Glueballs is to get soil remediation material.
The preparation of modified silica-gel: taking 120mL mass fraction is that 30% sodium silicate solution pours into three mouthfuls of burnings with blender
In bottle, pH to 7 is adjusted with the salt slow acid that mass fraction is 10%, starts blender, 40min is stirred with 400r/min revolving speed, it is micro-
Wave oscillation treatment 5min sets microwave oscillation frequency as 25kHz, obtains nano-sized hydrosol, nano-sized hydrosol is put into baking oven
85 DEG C are heated to, dry 4h obtains nanometer silica gel；
220g nanometer silica gel is weighed to be placed in the Loprazolam aqueous solution that 450mL mass fraction is 40%, controlled at 55 DEG C,
30min is stirred, activated silica gel is obtained, with r-chloropropyl trimethoxyl silane is in mass ratio that 2 ︰ 1 are mixed by activated silica gel, is obtained instead
Material is answered, 250g reaction mass is placed in 420mL dimethylbenzene and reacts 45min, obtains modified silica-gel, it is spare；
Load the preparation of the clay of nano zero valence iron:
It is then super with the frequency of 30kHz in ultrasonic treatment machine by salt acid dip 3 days that attapulgite clay mass fraction is 5%
Sound oscillation 30min, filtering removal filtrate, then be in neutrality with deionized water repeated flushing to cleaning solution, it is subsequently placed into set temperature
For 4h dry in 300 DEG C of baking ovens, 200 meshes are crossed, activated clay is obtained；
According to mass ratio it is 2 ︰ 5 by activated clay and green-vitriol, is added in the conical flask equipped with deionized water, machinery stirs
Magnetic stirrer is used instead after mixing 25min, and is passed through nitrogen protection, and 5g sodium borohydride is taken to be dissolved in 500mL deionized water
Preparation obtains sodium borohydride solution, and above-mentioned sodium borohydride solution dropping funel is added in conical flask, control dropping funel drop
Speed is 5mL/min, and reduction reaction 45min obtains reduzate；
Above-mentioned reduzate is placed in supercentrifuge and is centrifugated with the revolving speed of 5000r/min, lower layer's solid is collected, by institute
Solid wash to be placed on for 4 times in the vacuum oven that set temperature is 60 DEG C with dehydrated alcohol and is dried in vacuo 7h, 200 mesh of mistake
Sieve obtains the clay of load nano zero valence iron；
The preparation of soil remediation material:
Modified silica-gel is immersed in the polyethylenimine solution that mass fraction is 20%, impregnate 12min, filtering removal filtrate is collected
Bio-sil is obtained, Bio-sil is laid down into funnel filtering surface, the clay and Rhodococcus coprophilus powder of nano zero valence iron will be loaded
It is mixed in mass ratio for 20 ︰ 1, then the water-dispersible water slurry for being configured to mass fraction and being 5%, which is poured into paving
It sets in the funnel of Bio-sil, filtering and washing is carried out with the pressure of 0.30MPa, take out Bio-sil, be granulated after dry and silicon is made
Glueballs is to get soil remediation material.
Comparative example 1: it is essentially identical with the preparation method of example 2, it has only the difference is that lacking modified silica-gel.
Comparative example 2: it is essentially identical with the preparation method of example 2, it has only the difference is that replacing load nanometer using bentonite
The clay of Zero-valent Iron.
Comparative example 3: the soil remediation material of Zhenjiang company production.
Reference standard " soil environment monitoring technical specification " executes.
It is excavated using excavator to soil to be repaired is polluted, by the heavy metal pollution in example 1~3 and comparative example
Soil remediation material is added to heavy metal pollution acid soil and applies the mixing of 2cm thickness, conserves 100 days, carries out sampling prison
It surveys.
1 performance measurement result of table
2 performance measurement result of table
According to data in table 1, table 2 it is found that soil remediation material produced by the present invention is for heavy metal pollution in polluted soil
There is very strong repairing effect with organic pollutant, adsorption effect is good, and it is more comprehensive to the repair function of soil, it can be effectively improved
Soil environment has wide prospect of the application.
Claims (8)
1. a kind of preparation method of soil remediation material, it is characterised in that specific preparation step are as follows:
Modified silica-gel to be immersed in the polyethylenimine solution that mass fraction is 20%, impregnates 10~12min, filtering removes filtrate,
Collection obtains Bio-sil, and Bio-sil is laid down into funnel filtering surface, will load the clay and the red ball of thermophilic excrement of nano zero valence iron
Bacterium powder is 20 ︰ 1 mixing, then the water-dispersible water slurry for being configured to mass fraction and being 5% in mass ratio, which is fallen
Enter to lay in the funnel of Bio-sil, carry out filtering and washing, takes out Bio-sil, be granulated after dry and silica-gel sphere is made to get soil
Earth repair materials；
The specific preparation step of the modified silica-gel are as follows:
(1) taking 100~120mL mass fraction is that 30% sodium silicate solution pours into the three-necked flask with blender, uses quality
The salt slow acid that score is 10% adjusts pH to 6~7, starts blender, stirs 30~40min with 350~400r/min revolving speed,
Microwave oscillation handles 3~5min, obtains nano-sized hydrosol, nano-sized hydrosol is put into baking oven and is heated to 80~85 DEG C,
Dry 3~4h, obtains nanometer silica gel；
(2) it weighs 200~220g nanometer silica gel to be placed in the Loprazolam aqueous solution that 400~450mL mass fraction is 40%, control
Temperature processed is 50~55 DEG C, stirs 20~30min, obtains activated silica gel, activated silica gel and r-chloropropyl trimethoxyl silane are pressed
Mass ratio is 2 ︰ 1 mixing, obtains reaction mass, 200~250g reaction mass is placed in 400~420mL dimethylbenzene and reacts 40
~45min obtains modified silica-gel, spare；
The clay of the described load nano zero valence iron it is specific the preparation method comprises the following steps:
(1) it by attapulgite clay with salt acid dip 2~3 days, is then shaken in ultrasonic treatment machine with the frequency ultrasound of 25~30kHz
Swing 20~30min, filtering removal filtrate, then deionized water repeated flushing is used, set temperature is subsequently placed into as 200~300 DEG C
Dry 3~4h, crosses 200 meshes, obtains activated clay in baking oven；
(2) activated clay and green-vitriol are mixed, is added in the conical flask equipped with deionized water, mechanical stirring 20~
It uses magnetic stirrer after 25min instead, and is passed through nitrogen protection, taper is added in above-mentioned sodium borohydride solution dropping funel
In bottle, control dropping funel drop speed is 4~5mL/min, and 40~45min of reduction reaction obtains reduzate；
(3) above-mentioned reduzate is placed in supercentrifuge and is centrifugated with the revolving speed of 4500~5000r/min, collect lower layer
Obtained solid is washed 3~4 times with dehydrated alcohol and is placed on vacuum in the vacuum oven that set temperature is 50~60 DEG C by solid
Dry 6~7h, sieving obtain the clay of load nano zero valence iron.
2. a kind of preparation method of soil remediation material according to claim 1, it is characterised in that: described is negative
The clay and Rhodococcus coprophilus powder mixing mass ratio for carrying nano zero valence iron are 20 ︰ 1.
3. a kind of preparation method of soil remediation material according to claim 1, it is characterised in that: the filtering and washing
Process, pressure is maintained at 0.25~0.30MPa when should control suction filtration, and further can carry out turn-over to Bio-sil in funnel,
Clay and bacterium powder is set uniformly to be adsorbed in Silica Surface.
4. a kind of preparation method of soil remediation material according to claim 1, it is characterised in that: the modified silica-gel
Specific preparation step (1) described in modified silica-gel specific preparation step (1) in microwave oscillation
Microwave oscillation frequency is set when processing as 23~25kHz.
5. a kind of preparation method of soil remediation material according to claim 1, it is characterised in that: the modified silica-gel
Specific preparation step (2) in activated silica gel and r-chloropropyl trimethoxyl silane mixing mass ratio be 2 ︰ 1.
6. a kind of preparation method of soil remediation material according to claim 1, it is characterised in that: the load nanometer
The salt acid mass fraction of dipping attapulgite clay is 5% in the specific preparation method of the clay of Zero-valent Iron (1), and clay passes through deionization
Cleaning solution should be in neutrality after water repeated flushing.
7. a kind of preparation method of soil remediation material according to claim 1, it is characterised in that: the load nanometer
Activated clay and green-vitriol mixing mass ratio are preferably 2 ︰ 5, sodium borohydride in the specific preparation method of the clay of Zero-valent Iron (2)
Solution is obtained by being dissolved in prepare in 500mL deionized water by 4~5g sodium borohydride.
8. a kind of preparation method of soil remediation material according to claim 1, it is characterised in that: the load nanometer
The specific preparation method of the clay of Zero-valent Iron (3) high speed centrifuge speed is 4500~5000r/min, loads nano zero valence iron
Clay is chosen to obtain through 200 meshes.
Priority Applications (1)
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110592066A (en) * | 2019-09-06 | 2019-12-20 | 北京林业大学 | Charcoal-loaded nano zero-valent iron coupled phosphate solubilizing bacterium immobilized pellet and preparation method and application thereof |
| CN113457617A (en) * | 2021-08-20 | 2021-10-01 | 兰州交通大学 | Preparation method of modified attapulgite loaded vulcanized nano zero-valent iron heavy metal adsorbent, product and application thereof |
| CN114212895A (en) * | 2021-12-13 | 2022-03-22 | 水生藻安生物科技（武汉）有限公司 | Composition and device for treating acidic iron ore waste liquid and preparation method thereof |
| CN114686240A (en) * | 2022-03-28 | 2022-07-01 | 浙江卓锦环保科技股份有限公司 | Reducing agent for heavy metal contaminated soil and use method thereof |
| CN116282039A (en) * | 2022-12-19 | 2023-06-23 | 石河子大学 | Method for removing boron impurities in trichlorosilane |
| CN116855254A (en) * | 2023-07-03 | 2023-10-10 | 江苏莘野生物科技有限公司 | Long-acting controllable acid soil conditioner and preparation method thereof |
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2019
- 2019-02-20 CN CN201910127099.4A patent/CN109880629A/en not_active Withdrawn
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110592066A (en) * | 2019-09-06 | 2019-12-20 | 北京林业大学 | Charcoal-loaded nano zero-valent iron coupled phosphate solubilizing bacterium immobilized pellet and preparation method and application thereof |
| CN113457617A (en) * | 2021-08-20 | 2021-10-01 | 兰州交通大学 | Preparation method of modified attapulgite loaded vulcanized nano zero-valent iron heavy metal adsorbent, product and application thereof |
| CN114212895A (en) * | 2021-12-13 | 2022-03-22 | 水生藻安生物科技（武汉）有限公司 | Composition and device for treating acidic iron ore waste liquid and preparation method thereof |
| CN114212895B (en) * | 2021-12-13 | 2024-06-14 | 水生藻安生物科技（武汉）有限公司 | Composition and device for treating acidic iron ore waste liquid and preparation method thereof |
| CN114686240A (en) * | 2022-03-28 | 2022-07-01 | 浙江卓锦环保科技股份有限公司 | Reducing agent for heavy metal contaminated soil and use method thereof |
| CN116282039A (en) * | 2022-12-19 | 2023-06-23 | 石河子大学 | Method for removing boron impurities in trichlorosilane |
| CN116855254A (en) * | 2023-07-03 | 2023-10-10 | 江苏莘野生物科技有限公司 | Long-acting controllable acid soil conditioner and preparation method thereof |
| CN116855254B (en) * | 2023-07-03 | 2024-06-07 | 江苏莘野生物科技有限公司 | Long-acting controllable acid soil conditioner and preparation method thereof |
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