CN108329920A - The regeneration method of magnetic soil renovation agent - Google Patents

The regeneration method of magnetic soil renovation agent Download PDF

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Publication number
CN108329920A
CN108329920A CN201711449323.9A CN201711449323A CN108329920A CN 108329920 A CN108329920 A CN 108329920A CN 201711449323 A CN201711449323 A CN 201711449323A CN 108329920 A CN108329920 A CN 108329920A
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soil
magnetic
renovation agent
particle
soil renovation
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CN201711449323.9A
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CN108329920B (en
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石佳奇
祝欣
王磊
陈樯
黄剑波
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Nanjing Institute of Environmental Sciences MEP
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Nanjing Institute of Environmental Sciences MEP
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K17/00Soil-conditioning materials or soil-stabilising materials
    • C09K17/40Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B09DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09CRECLAMATION OF CONTAMINATED SOIL
    • B09C1/00Reclamation of contaminated soil
    • B09C1/08Reclamation of contaminated soil chemically

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Soil Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention belongs to technical field of soil remediation, more particularly to a kind of regeneration method of magnetic soil renovation agent, wherein magnetic soil renovation agent is with recessed soil for carrier, the compound of magnetic nano-particle, nano calcium oxide is loaded, be added containing mass fraction be 6 10% dihydric phosphate and mass fraction be 0.15 0.45% little Hua gold pick one's ears plain mixed solution, it is heated to 60 80 DEG C, ultrasound is after 24 hours, take solid matter, after the solid matter is eluted with pure water again, high-temperature calcination 50 80 minutes under the conditions of 380 420 DEG C again, it is cooling, that is, complete regeneration;It is high to the removal efficiency of chlorobenzene and metal cadmium ion when being repaired again applied to chlorobenzene and the dual contaminated soil of metal cadmium ion by regenerated magnetic soil renovation agent, with good repairing effect, and can still be separated and recovered by magnetic field, Reusability greatlys save cost.

Description

The regeneration method of magnetic soil renovation agent
Technical field
The invention belongs to technical field of soil remediation, and in particular to a kind of regeneration method of magnetic soil renovation agent.
Background technology
Soil was natural collecting post and the purified treatment place of all kinds of wastes originally, and soil receives pollutant, not table Show that soil is contaminated, only when each pollutant accommodated in soil is excessive, influence and be more than the self-purification capacity of soil, To in hygiene and produce harmful influence on epidemiology, just show that soil is contaminated.Cause soil pollution The reason of it is very much, it is a large amount of to use the mines containing heavy metal if pollutant settles in industrial sludge, agricultural garbage, sewage irrigation, air Matter chemical fertilizer and pesticide etc..
Often by soil-repairing agent, existing soil-repairing agent often has a single function, and soil is caused to be repaiied for the reparation of soil Compound method is complicated, and is difficult to reclaiming, and cost is higher.
Invention content
The present invention solves the above-mentioned technical problems in the prior art, provides a kind of regeneration side of magnetic soil renovation agent Method.
To solve the above problems, technical scheme is as follows:
A kind of regeneration method of magnetic soil renovation agent, wherein magnetic soil renovation agent are to be loaded for carrier with recessed soil The compound of magnetic nano-particle, nano calcium oxide, regeneration includes the following steps,
S1, surface soil will be removed for the magnetic soil renovation agent after soil remediation;
S2, mixed solution is added into the magnetic soil renovation agent handled well, contains mass fraction in the mixed solution The little Hua gold that dihydric phosphate and mass fraction for 6-10% are 0.15-0.45% is picked one's ears, and (4 β-acetoxyl groups-puppet is cured element Wooden alkane -11 (13)-alkene -12, the 8 α-lactone of wound), it is heated to 60-80 DEG C, after 2-4 hours ultrasonic, takes solid matter;
S3, after the solid matter is eluted with pure water, it is cold then high-temperature calcination 50-80 minutes under the conditions of 380-420 DEG C But, that is, regeneration is completed.
Preferably, the magnetic nano-particle is magnetic ferroferric oxide nano-particles or magnetic nickel nano particle.
Preferably, the method for surface soil being removed described in step 1 is that pure water is added in magnetropism soil-repairing agent, ultrasound 1-2 hours.
Preferably, be added pure water, it is 1-2 hour ultrasonic the step of repetition 2-5 times.
Preferably, the dihydric phosphate is potassium dihydrogen phosphate or sodium dihydrogen phosphate.
Preferably, the volume ratio of magnetic soil renovation agent and mixed solution described in step 2 is 1:2.5-3.5.
Preferably, the magnetic soil renovation agent is made by the following method:
S1, recessed native raw material is taken, is ground, the recessed soil particle after grinding is 500 mesh;
The hydrogen peroxide solution that mass fraction is 28-32% is added in S2, the recessed soil particle obtained by step 1, ultrasonic disperse is equal It is even, concentrated ammonia liquor is added, adjusting pH is 10-11, is warming up to 60-70 DEG C, is reacted 2-4 hours;The quality of recessed soil particle and hydrogen peroxide Than being 1:2;
S3, it keeps temperature to be 60-70 DEG C, under high-speed stirred, SG-Si602 (N- (β-ammonia is added in step 2 gained system Ethyl)-aminopropyltriethoxy dimethoxysilane), magnetic nano-particle is added, and vinegar acid for adjusting pH is 4-5, continues to stir 2-4 After hour, 220-240 DEG C of high-temperature calcination 7-8 hours obtains blocks of solid;The mass ratio of SG-Si602 and recessed soil particle is 1: 54;The mass ratio of magnetic nano-particle and recessed soil particle is 1:14;
S4, the blocks of solid is soaked into solution, the solution is that mass fraction is 1% calcium chloride and mass fraction For 6% aqueous povidone solution, it is warming up to 80-90 DEG C, carries out ultrasound, the condition of ultrasonic reaction is:Power 400- 600W, frequency 36KHz, time are 30-60 minutes, and addition mass fraction is 1% weak aqua ammonia, continues ultrasound, removes solvent, takes Solid is dried, and crushes, the magnetic soil renovation agent of 40-60 mesh is made.
Compared with the existing technology, advantages of the present invention is as follows,
The present invention provides a kind of regeneration methods of magnetic soil renovation agent, can will be repaiied for the magnetic soil of soil remediation Multiple agent regeneration, and magnetic soil healer properties will not be reduced, by regenerated magnetic soil renovation agent, it is applied to chlorobenzene again It is high to the removal efficiency of chlorobenzene and metal cadmium ion when being repaired with the dual contaminated soil of metal cadmium ion, there is good repair Multiple effect, and can still be separated and recovered by magnetic field, Reusability greatlys save cost.
Specific implementation mode
Embodiment 1:
Prepare magnetic soil renovation agent
S1, recessed native raw material is taken, is ground, the recessed soil particle after grinding is 500 mesh;
The hydrogen peroxide solution that mass fraction is 28-32% is added in S2, the recessed soil particle obtained by step 1, ultrasonic disperse is equal It is even, concentrated ammonia liquor is added, adjusting pH is 10-11, is warming up to 60-70 DEG C, is reacted 2-4 hours;The quality of recessed soil particle and hydrogen peroxide Than being 1:2;
S3, it keeps temperature to be 60-70 DEG C, under high-speed stirred, SG-Si602 is added in step 2 gained system, magnetic is added Property nano nickel particles, and vinegar acid for adjusting pH is 4-5, and after continuing stirring 2-4 hours, 220-240 DEG C of high-temperature calcination 7-8 hours obtains To blocks of solid;The mass ratio of SG-Si602 and recessed soil particle is 1:54;The mass ratio of magnetic nickel nano particle and recessed soil particle It is 1:14;
S4, the blocks of solid is soaked into solution, the solution is that mass fraction is 1% calcium chloride and mass fraction For 6% aqueous povidone solution, it is warming up to 80-90 DEG C, carries out ultrasound, the condition of ultrasonic reaction is:Power 400- 600W, frequency 36KHz, time are 30-60 minutes, and addition mass fraction is 1% weak aqua ammonia, continues ultrasound, removes solvent, takes Solid is dried, and crushes, the magnetic soil renovation agent of 40-60 mesh is made.
Embodiment 2:
Magnetic soil renovation agent prepared by embodiment 1 is used for chlorobenzene and the dual contaminated soil reparation of metal cadmium ion, The specific steps are:
A concentration of 100mg/kg of chlorobenzene in the soil of selection, a concentration of 100mg/kg of metal cadmium ion, by embodiment 1 The magnetic soil renovation agent of preparation is with contaminated soil according to 1:5 mass ratio after mixing, under stirring condition, uniformly sprays The mixed phosphate saline solution for the dipotassium hydrogen phosphate that potassium dihydrogen phosphate, mass fraction that mass fraction is 4-6% are 2-3% is spilt, Ground moistening is kept, after being heated 24-48 hours under the conditions of 40-50 DEG C, dries pulverizing is 65-75 mesh, and stirring condition is in magnetic field Separation magnetic soil renovation agent and soil in the magnetic field that intensity is 40000~50000V/m;Detect the removal of cadmium, chlorobenzene in soil The rate of recovery of rate and modified attapulgite.
The rate of recovery of 1 cadmium of table, the removal rate of chlorobenzene and modified attapulgite is tested
The removal rate % of cadmium The removal rate % of chlorobenzene The rate of recovery % of modified attapulgite
99.8 99.7 99.2
Embodiment 3:
The regeneration of magnetic soil renovation agent
Pure water is added in S1, the magnetic soil renovation agent by embodiment 2 for being isolated after soil remediation, ultrasonic 1-2 is small When, remove surface soil;Also the soil regime that can be adhered to according to magnetic soil renovation agent surface, will be added pure water, ultrasonic 1-2 is small When the step of repeat 2-5 times.
S2, it is added mixed solution into the magnetic soil renovation agent handled well, magnetic soil renovation agent and mixed solution Volume ratio is 1:2.5-3.5, in the mixed solution containing mass fraction be 10% sodium dihydrogen phosphate and mass fraction be 0.45% little Hua gold is picked one's ears plain (4 β-acetoxyl groups-puppet guainane -11 (13)-alkene -12,8 α-lactone), is heated to 80 DEG C, Ultrasound takes solid matter after 4 hours;
S3, after the solid matter is eluted with pure water, then high-temperature calcination 50 minutes under the conditions of 420 DEG C are cooling, that is, complete Regeneration.
Embodiment 4:
The regeneration of magnetic soil renovation agent
Pure water is added in S1, the magnetic soil renovation agent by embodiment 2 for being isolated after soil remediation, ultrasonic 1-2 is small When, remove surface soil;Also the soil regime that can be adhered to according to magnetic soil renovation agent surface, will be added pure water, ultrasonic 1-2 is small When the step of repeat 2-5 times.
S2, it is added mixed solution into the magnetic soil renovation agent handled well, magnetic soil renovation agent and mixed solution Volume ratio is 1:2.5-3.5, in the mixed solution containing mass fraction be 6% potassium dihydrogen phosphate and mass fraction be 0.15% little Hua gold is picked one's ears plain (4 β-acetoxyl groups-puppet guainane -11 (13)-alkene -12,8 α-lactone), is heated to 60 DEG C, Ultrasound takes solid matter after 2 hours;
S3, after the solid matter is eluted with pure water, then high-temperature calcination 80 minutes under the conditions of 380 DEG C are cooling, that is, complete Regeneration.
Embodiment 5:
The regeneration of magnetic soil renovation agent
Pure water is added in S1, the magnetic soil renovation agent by embodiment 2 for being isolated after soil remediation, ultrasonic 1-2 is small When, remove surface soil;Also the soil regime that can be adhered to according to magnetic soil renovation agent surface, will be added pure water, ultrasonic 1-2 is small When the step of repeat 2-5 times.
S2, it is added mixed solution into the magnetic soil renovation agent handled well, magnetic soil renovation agent and mixed solution Volume ratio is 1:2.5-3.5, in the mixed solution containing mass fraction be 8% potassium dihydrogen phosphate and mass fraction be 0.3% little Hua gold is picked one's ears plain (4 β-acetoxyl groups-puppet guainane -11 (13)-alkene -12,8 α-lactone), is heated to 70 DEG C, Ultrasound takes solid matter after 3 hours;
S3, after the solid matter is eluted with pure water, then high-temperature calcination 60 minutes under the conditions of 400 DEG C are cooling, that is, complete Regeneration.
Embodiment 6:
The regeneration of magnetic soil renovation agent, with embodiment 5, the difference is that, dihydric phosphate uses phosphoric acid in step 2 Ammonium dihydrogen replaces potassium dihydrogen phosphate.
Embodiment 7:
The regeneration of magnetic soil renovation agent, with embodiment 5, the difference is that, change the step the dense of potassium dihydrogen phosphate in 2 Degree:
A groups:Potassium dihydrogen phosphate mass fraction is 0%;
B groups:Potassium dihydrogen phosphate mass fraction is 4%;
C groups:Potassium dihydrogen phosphate mass fraction is 14%.
Embodiment 8:
The regeneration of magnetic soil renovation agent, with embodiment 5, the difference is that, change the step 3 calcination condition:
A groups:High-temperature calcination 60 minutes under the conditions of 320 DEG C;
B groups:High-temperature calcination 60 minutes under the conditions of 520 DEG C.
Embodiment 9:
Magnetic soil renovation agent after regeneration is used for chlorobenzene and the dual contaminated soil reparation of metal cadmium ion
By the regenerated magnetic soil renovation agents of embodiment 3-8, chlorobenzene concentration is repaired using the soil remediation step of embodiment 2 For 100mg/kg, the contaminated soil of a concentration of 100mg/kg of metal cadmium ion, after the completion of reparation, cadmium in soil, chlorobenzene The rate of recovery of removal rate and modified attapulgite is as follows
The rate of recovery of 2 cadmium of table, the residual quantity of chlorobenzene and modified attapulgite is tested
According to the result of table 2 it is found that the magnetic soil renovation agent after regeneration still has excellent repair ability and very high The rate of recovery, in regenerative process, the selection of dihydric phosphate has an impact regeneration effect, is better than using ammonium using the effect of sylvite Salt;The temperature of calcining also influences the repairing performance of the magnetic soil renovation agent after regeneration, and calcination temperature is too low, regenerates magnetic soil Renovation agent reduces the removal rate of chlorobenzene, and calcination temperature is excessively high, and regeneration magnetic soil renovation agent reduces the removal rate of cadmium ion.
It should be noted that above-described embodiment is only presently preferred embodiments of the present invention, there is no for the purpose of limiting the invention Protection domain, the equivalent replacement or replacement made on the basis of the above all belong to the scope of protection of the present invention.

Claims (7)

1. a kind of regeneration method of magnetic soil renovation agent, which is characterized in that wherein magnetic soil renovation agent is using recessed soil as load Body has loaded the compound of magnetic nano-particle, nano calcium oxide, and regeneration includes the following steps,
S1, surface soil will be removed for the magnetic soil renovation agent after soil remediation;
S2, mixed solution is added into the magnetic soil renovation agent handled well, it is 6- that mass fraction is contained in the mixed solution The little Hua gold earpick element that 10% dihydric phosphate and mass fraction is 0.15-0.45%, is heated to 60-80 DEG C, ultrasonic 2-4 After hour, solid matter is taken;
S3, after the solid matter is eluted with pure water, it is cooling then high-temperature calcination 50-80 minutes under the conditions of 380-420 DEG C, i.e., Complete regeneration.
2. the regeneration method of magnetic soil renovation agent as described in claim 1, which is characterized in that the magnetic nano-particle is Magnetic ferroferric oxide nano-particles or magnetic nickel nano particle.
3. the regeneration method of magnetic soil renovation agent as described in claim 1, which is characterized in that remove surface described in step 1 The method of soil is that pure water is added in magnetropism soil-repairing agent, 1-2 hours ultrasonic.
4. the regeneration method of magnetic soil renovation agent as claimed in claim 3, which is characterized in that pure water is added, ultrasonic 1-2 is small When the step of repeat 2-5 times.
5. the regeneration method of magnetic soil renovation agent as described in claim 1, which is characterized in that the dihydric phosphate is phosphorus Acid dihydride potassium or sodium dihydrogen phosphate.
6. the regeneration method of magnetic soil renovation agent as described in claim 1, which is characterized in that magnetic soil described in step 2 The volume ratio of renovation agent and mixed solution is 1:2.5-3.5.
7. the regeneration method of magnetic soil renovation agent as described in claim 1, which is characterized in that the magnetic soil renovation agent It is made by the following method:
S1, recessed native raw material is taken, is ground, the recessed soil particle after grinding is 500 mesh;
The hydrogen peroxide solution that mass fraction is 28-32% is added in S2, the recessed soil particle obtained by step 1, ultrasonic disperse is uniform, adds Enter concentrated ammonia liquor, adjusting pH is 10-11, is warming up to 60-70 DEG C, is reacted 2-4 hours;The mass ratio of recessed soil particle and hydrogen peroxide is 1: 2;
S3, it keeps temperature to be 60-70 DEG C, under high-speed stirred, SG-Si602 is added in step 2 gained system, magnetism is added and receives Rice corpuscles, and vinegar acid for adjusting pH is 4-5, after continuing stirring 2-4 hours, 220-240 DEG C of high-temperature calcination 7-8 hours obtains bulk Solid;The mass ratio of SG-Si602 and recessed soil particle is 1:54;The mass ratio of magnetic nano-particle and recessed soil particle is 1:14;
S4, the blocks of solid is soaked into solution, the solution is that mass fraction is that 1% calcium chloride is with mass fraction 6% aqueous povidone solution is warming up to 80-90 DEG C, carries out ultrasound, and the condition of ultrasonic reaction is:Power 400- 600W, frequency 36KHz, time are 30-60 minutes, and addition mass fraction is 1% weak aqua ammonia, continues ultrasound, removes solvent, takes Solid is dried, and crushes, the magnetic soil renovation agent of 40-60 mesh is made.
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