CN108329921A - A kind of preparation method of modified attapulgite and its application in soil remediation - Google Patents
A kind of preparation method of modified attapulgite and its application in soil remediation Download PDFInfo
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- CN108329921A CN108329921A CN201711449344.0A CN201711449344A CN108329921A CN 108329921 A CN108329921 A CN 108329921A CN 201711449344 A CN201711449344 A CN 201711449344A CN 108329921 A CN108329921 A CN 108329921A
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- modified attapulgite
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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
Abstract
The invention belongs to technical field of soil remediation, a kind of preparation method more particularly to modified attapulgite and its application in soil remediation, the present invention prepares modified attapulgite by composite magnetic nano-particle and nano calcium oxide, it can be used for chlorobenzene and the dual contaminated soil reparation of metal cadmium ion, soil pH conditions are not strict with, it is applied widely；The removal efficiency of the method that modified attapulgite prepared by the present invention repairs chlorobenzene and the dual contaminated soil of metal cadmium ion, chlorobenzene and metal cadmium ion is high, has good repairing effect；The preparation method of modified attapulgite of the present invention, magnetic nano-particle load factor is high, not easily to fall off, after modified attapulgite is used for soil remediation, can be separated and recovered by magnetic field, cost-effective.
Description
Technical field
The invention belongs to technical field of soil remediation, and in particular to a kind of preparation method of modified attapulgite and its be repaiied in soil
Application in multiple.
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 cost is higher；Chinese patent CN201510170522 discloses a kind of utilization modified attapulgite disposition dangerous contamination
The method of organo-chlorine pesticide POPs in the leachate of place, this method can only be used to organochlorine in the leachate of removal dangerous contamination place
Pesticide；Chinese patent CN2015104209684 discloses a kind of soil remediation medicament, is made of pulvis and liquid agent；The powder
The portland cement that agent is 20%~63% by weight percent, 20%~63% quick lime, 10%~18% clay mineral
Matter, 2%~5% Fe-base compound and 5%~10% sulfur-based compound composition；And the liquid agent is then by weight percent
For 5%~20% sustained release sulfate, 3%~10% phosphorio compound and 70%~92% water composition；The soil remediation
Medicament has the advantages that the soil pH value scope of application is wide, but only can be with the heavy metal pollution in rehabilitating soil.
Invention content
The present invention solves the above-mentioned technical problems in the prior art, provide a kind of modified attapulgite preparation method and its
Application in soil remediation.
To solve the above problems, technical scheme is as follows：
A kind of preparation method of modified attapulgite, includes the following steps,
S1, recessed native raw material is taken, is ground, the recessed soil particle after grinding is between 400-600 mesh；
Hydrogen peroxide solution is added in S2, the recessed soil particle obtained by step 1, ultrasonic disperse is uniform, and concentrated ammonia liquor is added, and adjusts pH
For 10-11, it is warming up to 60-70 DEG C, is reacted 2-4 hours；
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, high-temperature calcination obtains blocks of solid；
S4, the blocks of solid is soaked into solution, the solution is that mass fraction is 0.5-1.5% calcium chloride and matter
The aqueous povidone solution that score is 4-8% is measured, is warming up to 80-90 DEG C, under ultrasound condition, weak aqua ammonia is added, continues
Ultrasound removes solvent, takes solid, dries, and crushes, and modified attapulgite is made.
Preferably, in the step 2, the mass ratio of recessed soil particle and hydrogen peroxide is 1:2-3.
Preferably, in the step 2, the mass fraction of the hydrogen peroxide solution is 28-32%.
Preferably, the mass ratio of the SG-Si602 being added in the step 3 and the recessed soil particle being added in step 2 is 1:
45-63。
Preferably, the mass ratio of the magnetic nano-particle and the recessed soil particle being added in step 2 that are added in the step 3 is
1:12-16。
Preferably, the magnetic nano-particle is magnetic ferroferric oxide nano-particles or magnetic nickel nano particle.
Preferably, in step 4, the modified attapulgite particle after crushing is 40-60 mesh.
Preferably, in step 4, the mass fraction of the weak aqua ammonia is 1-2%.
Preferably, in step 4, the condition of ultrasonic reaction is：Power 400-600W, frequency 30-42KHz, time 30-
60 minutes.
The above-mentioned recessed soil of improvement can be used for chlorobenzene and the dual contaminated soil reparation of heavy metal ion.
Improve that recessed soil can be used for chlorobenzene and the method for the dual contaminated soil reparation of metal cadmium ion is：
By modified attapulgite and contaminated soil according to 1:The mass ratio of 4-6 after mixing, under stirring condition, uniformly sprays
Phosphate aqueous solution is spilt, after being heated 24-48 hours under the conditions of 40-50 DEG C, dries pulverizing detaches modified attapulgite and soil in magnetic field
Earth.
Preferably, the soil particle of crushing is 65-75 mesh.
Preferably, magnetic field intensity is 40000~50000V/m.
Preferably, the phosphate is the mixed aqueous solution of potassium dihydrogen phosphate, dipotassium hydrogen phosphate, the potassium dihydrogen phosphate
Mass fraction is 4-6%, and the mass fraction of the dipotassium hydrogen phosphate is 2-3%.
Compared with the existing technology, advantages of the present invention is as follows,
The present invention is prepared for a kind of modified attapulgite, can be used for chlorobenzene and the dual contaminated soil reparation of metal cadmium ion, right
Soil pH conditions are not strict with, applied widely；
The method that modified attapulgite prepared by the present invention repairs chlorobenzene and the dual contaminated soil of metal cadmium ion, chlorobenzene and gold
The removal efficiency for belonging to cadmium ion is high, has good repairing effect；
The preparation method of modified attapulgite of the present invention, magnetic nano-particle load factor is high, not easily to fall off, and modified attapulgite is for soil
After earth is repaired, it can be separated and recovered by magnetic field, it is cost-effective.
Specific implementation mode
Embodiment 1：
A kind of preparation method of modified attapulgite, includes the following steps,
S1, recessed native raw material is taken, is ground, the recessed soil particle after grinding is 400 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 ferriferrous oxide nano-particle, and vinegar acid for adjusting pH be 4-5, continue stirring 2-4 hours after, 220-240 DEG C of high-temperature calcination 7-8
Hour, obtain blocks of solid；The mass ratio of SG-Si602 and recessed soil particle is 1:45；Magnetic ferroferric oxide nano-particles with it is recessed
The mass ratio of soil particle is 1:12；
S4, the blocks of solid is soaked into solution, the solution is that mass fraction is 0.5% calcium chloride and quality point
Number is 4% 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, is removed molten
Agent takes solid, dries, and crushes, the modified attapulgite of 40-60 mesh is made；
Embodiment 2：
A kind of preparation method of modified attapulgite, includes the following steps,
S1, recessed native raw material is taken, is ground, the recessed soil particle after grinding is 600 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 1:3；
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 1:63；The mass ratio of magnetic nickel nano particle and recessed soil particle
It is 1:16；
S4, the blocks of solid is soaked into solution, the solution is that mass fraction is 1.5% calcium chloride and quality point
Number is 8% 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 2% weak aqua ammonia, continues ultrasound, is removed molten
Agent takes solid, dries, and crushes, the modified attapulgite of 40-60 mesh is made.
Embodiment 3：
A kind of preparation method of modified attapulgite, includes the following steps,
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 ferriferrous oxide nano-particle, and vinegar acid for adjusting pH be 4-5, continue stirring 2-4 hours after, 220-240 DEG C of high-temperature calcination 7-8
Hour, obtain blocks of solid；The mass ratio of SG-Si602 and recessed soil particle is 1:54；Magnetic ferroferric oxide nano-particles with it is recessed
The mass ratio of 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 modified attapulgite of 40-60 mesh is made；
Embodiment 4：
With embodiments 3, the mass ratio of SG-Si602 and recessed soil particle in 2 are changed the step, modified attapulgite is prepared,
A groups：The mass ratio of SG-Si602 and recessed soil particle is 1:36；
B groups：The mass ratio of SG-Si602 and recessed soil particle is 1:70.
Embodiment 5：
With embodiment 3, the concentration of calcium chloride and aqueous povidone solution in 4 is changed the step, modified attapulgite is prepared,
A groups：The mass fraction of calcium chloride water is 2.5%, and the mass fraction of aqueous povidone solution is
12%；
B groups：The mass fraction of calcium chloride water is 0.25%, and the mass fraction of aqueous povidone solution is
1%.
Embodiment 6：
With embodiment 3, SG-Si602 in step 3 is replaced using vinyltrimethoxysilane, standby modified attapulgite.
Embodiment 7：
It improves recessed soil and 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
1-6 modified attapulgites are with contaminated soil according to 1:The mass ratio of 4-6 after mixing, under stirring condition, uniformly sprays quality
The mixed phosphate saline solution for the dipotassium hydrogen phosphate that potassium dihydrogen phosphate that score is 4-6%, mass fraction are 2-3% keeps soil
Earth moistens, and after heat 24-48 hours under the conditions of 40-50 DEG C, dries pulverizing is 65-75 mesh, in magnetic field intensity under stirring condition
Recessed soil and soil are improved to be isolated in the magnetic field of 40000~50000V/m；The removal rate of cadmium, chlorobenzene in soil is detected, and
The rate of recovery of modified attapulgite.
As shown in Table 1, SG-Si602 influences the load factor of magnetic nano-particle with the mass ratio of recessed soil particle, to influence
The rate of recovery of modified attapulgite；The load that the concentration of calcium chloride and aqueous povidone solution influences magnetic nano-particle is strong
Degree, concentration is low, and possible magnetic nano-particle is easy to fall off, to affect the rate of recovery of modified attapulgite, excessive concentration, recessed soil surface
The calcium oxide of covering is excessive, can also reduce the rate of recovery of modified attapulgite.
The rate of recovery of 1 cadmium of table, the removal rate of chlorobenzene and modified attapulgite is tested
| Modified attapulgite group | The removal rate % of cadmium | The removal rate % of chlorobenzene | The rate of recovery % of modified attapulgite |
| Embodiment 1 | 99.4 | 98.6 | 99.1 |
| Embodiment 2 | 99.5 | 99.2 | 99.4 |
| Embodiment 3 | 99.8 | 99.7 | 99.2 |
| Embodiment 4-A groups | 87.1 | 84.2 | 21.2 |
| Embodiment 4-B groups | 74.6 | 65.2 | 18.5 |
| Embodiment 5-A groups | 89.2 | 87.1 | 38.7 |
| Embodiment 5-B groups | 81.4 | 83.2 | 26.9 |
| Embodiment 6 | 31.6 | 29.8 | 47.5 |
Embodiment 8：
It improves recessed soil and 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 3
Modified attapulgite is with contaminated soil according to 1:The mass ratio of 4-6 after mixing, under stirring condition, uniformly sprays phosphoric acid brine
Solution keeps ground moistening, and after heat 24-48 hours under the conditions of 40-50 DEG C, dries pulverizing is 65-75 mesh, under stirring condition
It is isolated in the magnetic field that magnetic field intensity is 40000~50000V/m and improves recessed soil and soil；Cadmium, chlorobenzene are gone in detection soil
Except rate and the rate of recovery of modified attapulgite.
A groups, phosphate aqueous solution are：The phosphoric acid that ammonium dihydrogen phosphate that mass fraction is 4-6%, mass fraction are 2-3%
The mixed aqueous solution of hydrogen diammonium；
B groups, phosphate aqueous solution are：The phosphoric acid that sodium dihydrogen phosphate that mass fraction is 4-6%, mass fraction are 2-3%
The mixed aqueous solution of disodium hydrogen；
The rate of recovery of 2 cadmium of table, the removal rate of chlorobenzene and modified attapulgite is tested
| Group | The removal rate % of cadmium | The removal rate % of chlorobenzene | The rate of recovery % of modified attapulgite |
| A groups | 83.2 | 82.7 | 99.1 |
| B groups | 85.8 | 84.6 | 99.3 |
According to the Comparative result of Tables 1 and 2 it is found that in repair process, phosphatic selection has an impact repairing effect,
It is better than the effect using ammonium salt, sodium salt using the effect of sylvite.
Recessed soil is being improved in chlorobenzene and the dual contaminated soil reparative experiment of metal cadmium ion, modified attapulgite with get dirty
The mass ratio of the soil of dye is preferably 1:4-6, addition modified attapulgite mass ratio is too small, and repairing effect is bad, and it is recessed that modification is added
Native mass ratio is too big, and repairing effect, which has no, to be obviously improved, but cost increases.
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 (10)
1. a kind of preparation method of modified attapulgite, which is characterized in that include the following steps,
S1, recessed native raw material is taken, is ground, the recessed soil particle after grinding is between 400-600 mesh；
Hydrogen peroxide solution is added in S2, the recessed soil particle obtained by step 1, ultrasonic disperse is uniform, and concentrated ammonia liquor is added, and adjusts pH and is
10-11 is warming up to 60-70 DEG C, reacts 2-4 hours；
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, high-temperature calcination obtains blocks of solid；
S4, the blocks of solid is soaked into solution, the solution is that mass fraction is 0.5-1.5% calcium chloride and quality point
Number is the aqueous povidone solution of 4-8%, is warming up to 80-90 DEG C, and under ultrasound condition, weak aqua ammonia is added, continues ultrasound,
Solvent is removed, solid is taken, is dried, is crushed, modified attapulgite is made.
2. the preparation method of modified attapulgite as described in claim 1, which is characterized in that the mass ratio of recessed soil particle and hydrogen peroxide
It is 1:2-3.
3. the preparation method of modified attapulgite as described in claim 1, which is characterized in that the SG- being added in the step 3
The mass ratio for the recessed soil particle being added in Si602 and step 2 is 1:45-63.
4. the preparation method of modified attapulgite as described in claim 1, which is characterized in that the magnetism being added in the step 3 is received
The mass ratio for the recessed soil particle being added in rice corpuscles and step 2 is 1:12-16.
5. the preparation method of modified attapulgite as described in claim 1, which is characterized in that the magnetic nano-particle is magnetism four
Fe 3 O nano-particle or magnetic nickel nano particle.
6. the preparation method of modified attapulgite as described in claim 1, which is characterized in that in step 4, the modified attapulgite after crushing
Particle is 40-60 mesh.
7. the preparation method of modified attapulgite as described in claim 1, which is characterized in that in step 4, the quality of the weak aqua ammonia
Score is 1-2%.
8. the preparation method of modified attapulgite as described in claim 1, which is characterized in that in step 4, the condition of ultrasonic reaction
For：Power 400-600W, frequency 30-42KHz, time are 30-60 minutes.
9. as claim 1-8 any one of them modified attapulgites are used for chlorobenzene and the dual contaminated soil reparation of metal cadmium ion
Method, which is characterized in that by modified attapulgite and contaminated soil according to 1:The mass ratio of 4-6 after mixing, stirring bar
Under part, phosphate aqueous solution is uniformly sprayed, after being heated 24-48 hours under the conditions of 40-50 DEG C, dries pulverizing detaches in magnetic field
Improve recessed soil and soil.
10. method as claimed in claim 9, which is characterized in that the phosphate be potassium dihydrogen phosphate, dipotassium hydrogen phosphate it is mixed
The mass fraction of Heshui solution, the potassium dihydrogen phosphate is 4-6%, and the mass fraction of the dipotassium hydrogen phosphate is 2-3%.
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| CN111548795A (en) * | 2020-05-09 | 2020-08-18 | 浙江正峰生态环境工程有限公司 | Phosphate modified attapulgite magnetic passivator and use method thereof |
| CN113861994A (en) * | 2021-09-30 | 2021-12-31 | 广西壮族自治区农业科学院 | Biochar soil restoration agent and preparation method thereof |
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Application publication date: 20180727 |