CN108329920B - Regeneration method of magnetic soil remediation agent - Google Patents
Regeneration method of magnetic soil remediation agent Download PDFInfo
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- CN108329920B CN108329920B CN201711449323.9A CN201711449323A CN108329920B CN 108329920 B CN108329920 B CN 108329920B CN 201711449323 A CN201711449323 A CN 201711449323A CN 108329920 B CN108329920 B CN 108329920B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/40—Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
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Abstract
The invention belongs to the technical field of soil remediation, and particularly relates to a regeneration method of a magnetic soil remediation agent, wherein the magnetic soil remediation agent is a compound loaded with magnetic nanoparticles and nano calcium oxide by taking attapulgite as a carrier, a mixed solution containing 6-10% of dihydric phosphate by mass and 0.15-0.45% of microcystin by mass is added, the mixed solution is heated to 60-80 ℃, ultrasonic treatment is carried out for 2-4 hours, solid substances are taken, the solid substances are subjected to washing by pure water, then the solid substances are subjected to high-temperature calcination for 50-80 minutes at the temperature of 420 ℃ and 380 ℃, and then the regeneration is completed after cooling; when the regenerated magnetic soil remediation agent is applied to remediation of chlorobenzene and metal cadmium ion double-polluted soil again, the removal efficiency of chlorobenzene and metal cadmium ions is high, the remediation effect is good, the magnetic soil remediation agent can be separated and recovered through a magnetic field and can be repeatedly used, and the cost is greatly saved.
Description
Technical Field
The invention belongs to the technical field of soil remediation, and particularly relates to a regeneration method of a magnetic soil remediation agent.
Background
Soil is originally a natural accommodation place and a purification treatment place of various wastes, soil accepts pollutants, does not indicate that the soil is polluted, and indicates that the soil is polluted only when various pollutants accommodated in the soil are excessive and influence and exceed the self-purification capacity of the soil, so that the soil has harmful influence on hygiene and epidemiology. Causes of soil pollution, such as industrial sludge, garbage agriculture, sewage irrigation, pollutant sedimentation in the atmosphere, and the use of heavy metal-containing mineral fertilizers and pesticides in large quantities.
Soil remediation usually depends on a soil remediation agent, and the existing soil remediation agent usually has a single function, so that the soil remediation method is complex, difficult to recover and regenerate and high in cost.
Disclosure of Invention
The invention solves the technical problems in the prior art and provides a regeneration method of a magnetic soil remediation agent.
In order to solve the problems, the technical scheme of the invention is as follows:
a regeneration method of a magnetic soil repairing agent, wherein the magnetic soil repairing agent is a compound which takes attapulgite as a carrier and is loaded with magnetic nano particles and nano calcium oxide, the regeneration comprises the following steps,
s1, removing the surface soil by using the magnetic soil remediation agent used for soil remediation;
s2, adding a mixed solution into the treated magnetic soil remediation agent, wherein the mixed solution contains 6-10% of dihydric phosphate and 0.15-0.45% of microcystin (4 beta-acetoxyl-pseudo guaiane-11 (13) -alkene-12, 8 alpha-lactone) by mass percent, heating to 60-80 ℃, and performing ultrasonic treatment for 2-4 hours to obtain a solid substance;
s3, washing the solid substance with pure water, calcining at 380-420 ℃ for 50-80 minutes, and cooling to finish regeneration.
Preferably, the magnetic nanoparticles are magnetic ferroferric oxide nanoparticles or magnetic nickel nanoparticles.
Preferably, the method for removing the surface soil in the step 1 is to add pure water into the magnetic soil remediation agent and perform ultrasonic treatment for 1-2 hours.
Preferably, the step of adding pure water and sonicating for 1-2 hours is repeated 2-5 times.
Preferably, the dihydrogen phosphate is potassium dihydrogen phosphate or sodium dihydrogen phosphate.
Preferably, the volume ratio of the magnetic soil remediation agent to the mixed solution in the step 2 is 1: 2.5-3.5.
Preferably, the magnetic soil remediation agent is prepared by the following method:
s1, grinding the attapulgite raw material, wherein the ground attapulgite particles are 500 meshes;
s2, adding a hydrogen peroxide solution with the mass fraction of 28-32% into the attapulgite particles obtained in the step 1, ultrasonically dispersing the mixture uniformly, adding strong ammonia water, adjusting the pH to 10-11, heating to 60-70 ℃, and reacting for 2-4 hours; the mass ratio of the attapulgite particles to the hydrogen peroxide is 1: 2;
s3, keeping the temperature at 60-70 ℃, adding SG-Si602(N- (beta-aminoethyl) -aminopropyl methyl dimethoxy silane) into the system obtained in the step 2 under high-speed stirring, adding magnetic nanoparticles, adjusting the pH value to 4-5 with acetic acid, continuously stirring for 2-4 hours, and calcining at 220-240 ℃ for 7-8 hours to obtain a blocky solid; the mass ratio of SG-Si602 to attapulgite particles is 1: 54; the mass ratio of the magnetic nano particles to the attapulgite particles is 1: 14;
s4, soaking the blocky solid into a solution, wherein the solution is a polyvinylpyrrolidone aqueous solution with the mass fraction of 1% and the mass fraction of 6%, heating to 80-90 ℃, and carrying out ultrasonic treatment, wherein the ultrasonic reaction conditions are as follows: the power is 400-600W, the frequency is 36KHz, the time is 30-60 minutes, 1 percent of diluted ammonia water by mass percent is added, the ultrasonic treatment is continued, the solvent is removed, the solid is taken out, dried and crushed, and the magnetic soil repairing agent with 40-60 meshes is prepared.
Compared with the prior art, the invention has the advantages that,
the invention provides a regeneration method of a magnetic soil remediation agent, which can regenerate the magnetic soil remediation agent for soil remediation without reducing the performance of the magnetic soil remediation agent.
Detailed Description
Example 1:
preparation of magnetic soil repairing agent
S1, grinding the attapulgite raw material, wherein the ground attapulgite particles are 500 meshes;
s2, adding a hydrogen peroxide solution with the mass fraction of 28-32% into the attapulgite particles obtained in the step 1, ultrasonically dispersing the mixture uniformly, adding strong ammonia water, adjusting the pH to 10-11, heating to 60-70 ℃, and reacting for 2-4 hours; the mass ratio of the attapulgite particles to the hydrogen peroxide is 1: 2;
s3, keeping the temperature at 60-70 ℃, adding SG-Si602 into the system obtained in the step 2 under high-speed stirring, adding magnetic nickel nano-particles, adjusting the pH value to 4-5 by acetic acid, continuously stirring for 2-4 hours, and calcining at the high temperature of 240 ℃ for 7-8 hours at 220 ℃ to obtain a blocky solid; the mass ratio of SG-Si602 to attapulgite particles is 1: 54; the mass ratio of the magnetic nickel nano particles to the attapulgite particles is 1: 14;
s4, soaking the blocky solid into a solution, wherein the solution is a polyvinylpyrrolidone aqueous solution with the mass fraction of 1% and the mass fraction of 6%, heating to 80-90 ℃, and carrying out ultrasonic treatment, wherein the ultrasonic reaction conditions are as follows: the power is 400-600W, the frequency is 36KHz, the time is 30-60 minutes, 1 percent of diluted ammonia water by mass percent is added, the ultrasonic treatment is continued, the solvent is removed, the solid is taken out, dried and crushed, and the magnetic soil repairing agent with 40-60 meshes is prepared.
Example 2:
the magnetic soil remediation agent prepared in the example 1 is used for remediation of soil polluted by both chlorobenzene and metal cadmium ions, and comprises the following specific steps:
the method comprises the steps of selecting soil with chlorobenzene concentration of 100mg/kg and metal cadmium ion concentration of 100mg/kg, uniformly mixing the magnetic soil remediation agent prepared in example 1 with polluted soil according to a mass ratio of 1:5, uniformly spraying a mixed phosphate aqueous solution of potassium dihydrogen phosphate with a mass fraction of 4-6% and dipotassium hydrogen phosphate with a mass fraction of 2-3% under a stirring condition, keeping the soil moist, heating for 24-48 hours at 40-50 ℃, drying and crushing to 65-75 meshes, and separating the magnetic soil remediation agent from the soil in a magnetic field with a magnetic field strength of 40000-50000V/m under the stirring condition; and detecting the removal rate of cadmium and chlorobenzene in the soil and the recovery rate of the modified attapulgite.
TABLE 1 test of removal of cadmium, chlorobenzene and recovery of modified attapulgite
| Removal rate of cadmium% | Removal rate of chlorobenzene% | Recovery rate of modified attapulgite |
| 99.8 | 99.7 | 99.2 |
Example 3:
regeneration of magnetic soil remediation agents
S1, adding pure water into the magnetic soil remediation agent separated after the soil remediation is carried out in the embodiment 2, and carrying out ultrasonic treatment for 1-2 hours to remove surface soil; the steps of adding pure water and carrying out ultrasonic treatment for 1 to 2 hours can be repeated for 2 to 5 times according to the condition of soil attached to the surface of the magnetic soil remediation agent.
S2, adding a mixed solution into the treated magnetic soil remediation agent, wherein the volume ratio of the magnetic soil remediation agent to the mixed solution is 1:2.5-3.5, the mixed solution contains 10% of sodium dihydrogen phosphate and 0.45% of microcystin (4 beta-acetoxy-pseudo guaiane-11 (13) -alkene-12, 8 alpha-lactone), heating to 80 ℃, and performing ultrasonic treatment for 4 hours to obtain a solid substance;
and S3, washing the solid substance with pure water, calcining at the high temperature of 420 ℃ for 50 minutes, and cooling to finish regeneration.
Example 4:
regeneration of magnetic soil remediation agents
S1, adding pure water into the magnetic soil remediation agent separated after the soil remediation is carried out in the embodiment 2, and carrying out ultrasonic treatment for 1-2 hours to remove surface soil; the steps of adding pure water and carrying out ultrasonic treatment for 1 to 2 hours can be repeated for 2 to 5 times according to the condition of soil attached to the surface of the magnetic soil remediation agent.
S2, adding a mixed solution into the treated magnetic soil remediation agent, wherein the volume ratio of the magnetic soil remediation agent to the mixed solution is 1:2.5-3.5, the mixed solution contains 6% by mass of potassium dihydrogen phosphate and 0.15% by mass of microcystin (4 beta-acetoxyl-pseudo guaiane-11 (13) -alkene-12, 8 alpha-lactone), heating to 60 ℃, and performing ultrasonic treatment for 2 hours to obtain a solid substance;
and S3, washing the solid substance with pure water, calcining at 380 ℃ for 80 minutes, and cooling to finish regeneration.
Example 5:
regeneration of magnetic soil remediation agents
S1, adding pure water into the magnetic soil remediation agent separated after the soil remediation is carried out in the embodiment 2, and carrying out ultrasonic treatment for 1-2 hours to remove surface soil; the steps of adding pure water and carrying out ultrasonic treatment for 1 to 2 hours can be repeated for 2 to 5 times according to the condition of soil attached to the surface of the magnetic soil remediation agent.
S2, adding a mixed solution into the treated magnetic soil remediation agent, wherein the volume ratio of the magnetic soil remediation agent to the mixed solution is 1:2.5-3.5, the mixed solution contains 8% by mass of potassium dihydrogen phosphate and 0.3% by mass of microcystin (4 beta-acetoxyl-pseudo guaiane-11 (13) -alkene-12, 8 alpha-lactone), heating to 70 ℃, and performing ultrasonic treatment for 3 hours to obtain a solid substance;
and S3, washing the solid substance with pure water, calcining at the high temperature of 400 ℃ for 60 minutes, and cooling to finish regeneration.
Example 6:
the regeneration of the magnetic soil remediation agent is the same as example 5, except that ammonium dihydrogen phosphate is used as the dihydrogen phosphate in the step 2 instead of potassium dihydrogen phosphate.
Example 7:
regeneration of magnetic soil remediation agent, same as example 5, except that the concentration of potassium dihydrogen phosphate in step 2 was changed:
group A: the mass fraction of the potassium dihydrogen phosphate is 0 percent;
group B: the mass fraction of the potassium dihydrogen phosphate is 4 percent;
group C: the mass fraction of the potassium dihydrogen phosphate is 14 percent.
Example 8:
regeneration of magnetic soil remediation agent, as in example 5, except that the calcination conditions in step 3 were changed:
group A: calcining at 320 ℃ for 60 minutes;
group B: calcining at 520 ℃ for 60 minutes.
Example 9:
the regenerated magnetic soil remediation agent is used for soil remediation of chlorobenzene and metal cadmium ion double pollution
The magnetic soil remediation agent regenerated in the examples 3 to 8 is used for remediating the polluted soil with the chlorobenzene concentration of 100mg/kg and the metal cadmium ion concentration of 100mg/kg by the soil remediation step of the example 2, and after the remediation is finished, the removal rate of cadmium and chlorobenzene in the soil and the recovery rate of the modified attapulgite are as follows
TABLE 2 residual amounts of cadmium, chlorobenzene and recovery tests of modified attapulgite
According to the results in the table 2, the regenerated magnetic soil repairing agent still has excellent repairing capability and high recovery rate, the selection of the dihydric phosphate influences the regeneration effect in the regeneration process, and the effect of using potassium salt is better than that of using ammonium salt; the calcination temperature also influences the repair performance of the regenerated magnetic soil repair agent, the removal rate of the regenerated magnetic soil repair agent to chlorobenzene is reduced due to too low calcination temperature, the removal rate of the regenerated magnetic soil repair agent to cadmium ions is reduced due to too high calcination temperature.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and all equivalent substitutions or substitutions made on the above-mentioned embodiments are included in the scope of the present invention.
Claims (5)
1. A regeneration method of a magnetic soil repairing agent is characterized in that the magnetic soil repairing agent is a compound which takes attapulgite as a carrier and is loaded with magnetic nano particles and nano calcium oxide, the regeneration comprises the following steps,
s1, removing the surface soil by using the magnetic soil remediation agent used for soil remediation;
s2, adding a mixed solution into the treated magnetic soil remediation agent, wherein the mixed solution contains 6-10% of dihydric phosphate and 0.15-0.45% of microcystin by mass, heating to 60-80 ℃, and performing ultrasonic treatment for 2-4 hours to obtain a solid substance; the volume ratio of the magnetic soil repairing agent to the mixed solution is 1:2.5-3.5
S3, washing the solid substance with pure water, calcining the solid substance at 380-420 ℃ for 50-80 minutes, and cooling to finish regeneration;
the magnetic soil remediation agent is prepared by the following method:
A. grinding attapulgite raw materials, wherein the ground attapulgite particles are 500 meshes;
B. adding a hydrogen peroxide solution with the mass fraction of 28-32% into the attapulgite particles obtained in the step 1, ultrasonically dispersing uniformly, adding strong ammonia water, adjusting the pH to 10-11, heating to 60-70 ℃, and reacting for 2-4 hours; the mass ratio of the attapulgite particles to the hydrogen peroxide is 1: 2;
C. keeping the temperature at 60-70 ℃, adding SG-Si602 into the system obtained in the step 2 under high-speed stirring, adding magnetic nanoparticles, adjusting the pH value to 4-5 by acetic acid, continuously stirring for 2-4 hours, and calcining at the high temperature of 240 ℃ for 7-8 hours to obtain a blocky solid; the mass ratio of SG-Si602 to attapulgite particles is 1: 54; the mass ratio of the magnetic nano particles to the attapulgite particles is 1: 14;
D. soaking the blocky solid into a solution, wherein the solution is a polyvinylpyrrolidone aqueous solution with the mass fraction of 1% and the mass fraction of 6%, heating to 80-90 ℃, and carrying out ultrasonic treatment, wherein the ultrasonic reaction conditions are as follows: the power is 400-600W, the frequency is 36KHz, the time is 30-60 minutes, 1 percent of diluted ammonia water by mass percent is added, the ultrasonic treatment is continued, the solvent is removed, the solid is taken out, dried and crushed, and the magnetic soil repairing agent with 40-60 meshes is prepared.
2. The method of claim 1, wherein said magnetic nanoparticles are magnetic ferroferric oxide nanoparticles or magnetic nickel nanoparticles.
3. The method of claim 1 wherein said step 1 of removing surface soil comprises adding purified water to said magnetic soil remediation agent and subjecting said mixture to ultrasound for 1 to 2 hours.
4. The method of claim 3 wherein the steps of adding purified water and sonicating for 1-2 hours are repeated 2-5 times.
5. The method of regenerating a magnetic soil remediation agent of claim 1 wherein the monobasic phosphate salt is potassium or sodium monobasic phosphate.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105405567A (en) * | 2015-12-07 | 2016-03-16 | 上海交通大学 | Magnetic remediation material for organic matter pollution in soil or water, and preparation method as well as application thereof |
| CN106268812A (en) * | 2016-08-25 | 2017-01-04 | 扬州大学 | A kind of nano-magnetic ecological restoration material on the ferroso-ferric oxide load attapulgite removing removal organic polluter and preparation method thereof |
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| CN104787833B (en) * | 2015-04-10 | 2017-02-22 | 环境保护部南京环境科学研究所 | Method for disposing organochlorine pesticide POPs of lixivium in dangerous and polluted sites by utilizing modified attapulgite clay. |
| CN105126743A (en) * | 2015-08-20 | 2015-12-09 | 南京航空航天大学 | Preparation and recovery methods for magnetic clay adsorption material |
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| CN105405567A (en) * | 2015-12-07 | 2016-03-16 | 上海交通大学 | Magnetic remediation material for organic matter pollution in soil or water, and preparation method as well as application thereof |
| CN106268812A (en) * | 2016-08-25 | 2017-01-04 | 扬州大学 | A kind of nano-magnetic ecological restoration material on the ferroso-ferric oxide load attapulgite removing removal organic polluter and preparation method thereof |
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| 小花金挖耳中1个新的化合物;高雪等;《中草药》;20150304;第46卷(第1期);第19-21页 * |
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