CN114524458B - Preparation and application of heavy metal contaminated soil conditioner - Google Patents
Preparation and application of heavy metal contaminated soil conditioner Download PDFInfo
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- CN114524458B CN114524458B CN202210183903.2A CN202210183903A CN114524458B CN 114524458 B CN114524458 B CN 114524458B CN 202210183903 A CN202210183903 A CN 202210183903A CN 114524458 B CN114524458 B CN 114524458B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/02—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The invention provides a heavy metal contaminated soil conditioner prepared from CuWO 4 ‑CoFe 2 O 4 Is compounded, and is hydrothermally prepared into porous spherical CuWO 4 The physical adsorption of heavy metal ions is greatly facilitated due to the high specific surface area and the rich and developed pore structure, and the nanometer CoFe is prepared by combining the microwave hydrothermal reaction and polyvinylpyrrolidone as a crystal control agent 2 O 4 Uniformly combined with CuWO 4 The two synergistically enhance the degradation performance of heavy metals in the soil.
Description
Technical Field
The invention belongs to the field of environmental protection, and particularly relates to a soil conditioner and a preparation method thereof.
Background
With the rapid development of economy, soil pollution is becoming more serious, and polluted soil treatment is also one of the important works of current environmental treatment. Among numerous soil pollutants, heavy metal ion pollution is one of the main pollution sources, is difficult to be decomposed by microorganisms and is easy to be accumulated in the bodies of animals and plants, and the social development and the body health of human bodies are seriously influenced.
Currently, numerous researchers have explored solutions to heavy metal contamination of soil. CN113101959A discloses a graphite-like carbon nitride composite material for soil remediation and a preparation method and application thereof. The composite material comprises the following raw materials: titanium dioxide material, graphene material and g-C 3 N 4 A material; the g to C 3 N 4 The material is a sheet material; the titanium dioxide material is titanium dioxide nanoparticles; the g-C is distributed on the surface of the graphene material 3 N 4 A material; and titanium dioxide materials are distributed on the surface of the graphene material. The composite material utilizes a graphene material and g-C 3 N 4 The large specific surface area of the material realizes the adsorption of large organic particles; graphene materials, g-C 3 N 4 The material and the titanium dioxide material form a heterojunction, so that the degradation of organic pollutants in soil is realized, and the degradation rate of the pollutants in the soil can reach more than 90% after illumination for 4 hours. CN108456530A discloses a magnetic carboxylated hollow microsphere soil remediation agent and a preparation method thereof, wherein the preparation method comprises the following steps: preparation of monodisperse SiO by improved process 2 Microsphere hydrothermal synthesis of Fe 3 O 4 Synthesis of Fe by dialysis method using @ C hollow microsphere 3 O 4 @C-COOHHollow microspheres. CN112480930A discloses a preparation method of a magnetic soil heavy metal restoration agent, the prepared heavy metal restoration agent and application thereof. The invention provides a method for preparing a magnetic soil heavy metal restoration agent by using silicon-containing tailing leaching residues, which is magnetic Fe modified by tetraethoxysilane 3 O 4 And as a magnetic core, the silicon-containing tailing leaching residue is subjected to hydrothermal activation to be used as a silicon source and an alkali source for synthesizing a repairing agent shell, and then a hydrothermal method is utilized to synthesize the magnetic soil repairing agent with a core-shell structure.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of the soil conditioner, which has the advantages of simple preparation process, low cost, environmental protection and convenience for industrial production; has better degradation effect on the soil polluted by heavy metals.
A heavy metal contaminated soil conditioner is prepared by the following steps:
(1) Dissolving (0.08-0.1) mol of soluble copper salt, (0.08-0.1) mol of soluble tungsten source, and (0.03-0.08) mol of sodium tartrate, and (0.16-0.2) mol of urea in deionized water, stirring for a certain time, mixing uniformly, transferring into a hydrothermal reaction kettle, and carrying out hydrothermal reaction at 180-200 ℃ for 12-24h to obtain porous spherical CuWO 4 ；
(2) Mixing porous spherical CuWO 4 Dissolving in deionized water, adding 0.01-0.02 mol of soluble cobalt salt, 0.02-0.04 mol of ferric salt and 15-20 mg of polyvinylpyrrolidone, transferring the mixed solution into a high-pressure reaction kettle, and carrying out microwave hydrothermal reaction to obtain CuWO 4 -CoFe 2 O 4 Composite material of nano CoFe 2 O 4 Growing on porous spherical CuWO 4 In the pores of (a).
Preferably, the soluble copper salt and the soluble tungsten source are respectively copper nitrate, copper sulfate, sodium tungstate and tungsten nitrate.
Preferably, the soluble cobalt salt and the iron salt are cobalt nitrate, cobalt sulfate, ferric nitrate and ferric sulfate respectively.
Preferably, the temperature of the microwave hydrothermal reaction is 150-180 ℃, the reaction time is 10-20h, and the microwave power is 100-300w.
The beneficial effect of this application:
porous spherical CuWO with particle size of 4-7 microns and prepared by the application 4 The physical adsorption of heavy metal ions is greatly facilitated due to the high specific surface area and the rich and developed pore structure, and the nanometer CoFe is prepared by combining the microwave hydrothermal reaction and polyvinylpyrrolidone as a crystal control agent 2 O 4 Uniformly combined with CuWO 4 The two synergistically enhance the degradation performance of heavy metals in the soil.
Drawings
Fig. 1 is an SEM image of the material of example 1.
Detailed Description
Example 1
(1) Dissolving 0.1mol of copper nitrate, 0.1mol of sodium tungstate, 0.07mol of sodium tartrate and 0.2mol of urea in deionized water, stirring for a certain time, uniformly mixing, transferring the mixture into a hydrothermal reaction kettle, and carrying out hydrothermal reaction at 180 ℃ for 12 hours to obtain porous spherical CuWO 4 ；
(2) Mixing porous spherical CuWO 4 Dissolving the mixture in 100ml of deionized water, then adding 0.01mol of cobalt nitrate, 0.02mol of ferric nitrate and 18mg of polyvinylpyrrolidone, transferring the mixed solution into a high-pressure reaction kettle, carrying out microwave hydrothermal reaction at the reaction temperature of 160 ℃, the reaction time of 12h and the reaction power of 150w to obtain CuWO 4 -CoFe 2 O 4 Composite material of nano CoFe 2 O 4 Growing on porous spherical CuWO 4 In the pores of (a).
Comparative example 1
Dissolving 0.1mol of copper nitrate, 0.1mol of sodium tungstate, 0.07mol of sodium tartrate and 0.2mol of urea in deionized water, stirring for a certain time, uniformly mixing, transferring the mixture into a hydrothermal reaction kettle, and carrying out hydrothermal reaction at 180 ℃ for 12 hours to obtain porous spherical CuWO 4 。
Comparative example 2
0.01mol of cobalt nitrate, 0.02mol of ferric nitrate and 18mg of polyvinylpyrrolidone are added into 100ml of deionized water, and the mixed solution is transferred toCarrying out microwave hydrothermal reaction in a high-pressure reaction kettle at the temperature of 160 ℃, the reaction time of 12h and the reaction power of 150w to obtain CoFe 2 O 4 。
And (3) testing the soil heavy metal removal rate:
and (3) taking 5kg of clean soil sample, uniformly adding a lead nitrate solution into the soil system, adding chromium nitrate and lead nitrate to adjust the concentration of the lead nitrate solution in the soil to be 500mg/kg, turning the soil every 3 days, and testing the removal rate of chromium ions and lead ions after 15 days.
| Removal rate of chromium ion | Removal rate of lead ion | |
| Example 1 | 72.1％ | 65.4％ |
| Comparative example 1 | 63.8％ | 56.8％ |
| Comparative example 2 | 32.4％ | 48.5％ |
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which may be made by those skilled in the art without departing from the spirit and scope of the present invention as defined in the appended claims.
Claims (3)
1. A heavy metal contaminated soil conditioner is prepared by the following steps:
(1) Dissolving (0.08-0.1) mol of soluble copper salt, (0.08-0.1) mol of soluble tungsten source, and (0.03-0.08) mol of sodium tartrate, and (0.16-0.2) mol of urea in deionized water, stirring for a certain time, mixing uniformly, transferring into a hydrothermal reaction kettle, and carrying out hydrothermal reaction at 180-200 ℃ for 12-24h to obtain porous spherical CuWO with the diameter of 4-7 microns 4 ；
(2) Mixing porous spherical CuWO 4 Dissolving in deionized water, adding (0.01-0.02) mol of soluble cobalt salt, (0.02-0.04) mol of soluble iron salt and (15-20) mg of polyvinylpyrrolidone, transferring the mixed solution into a high-pressure reaction kettle, carrying out microwave hydrothermal reaction at 150-180 ℃, reacting for 10-20h and with the microwave power of 100-300W to obtain CuWO 4 -CoFe 2 O 4 Composite material of nano-CoFe 2 O 4 Growing on porous spherical CuWO 4 In the pores of (a).
2. The heavy metal contaminated soil conditioner of claim 1, wherein the soluble copper salt and the soluble tungsten source are respectively copper nitrate, copper sulfate, sodium tungstate and tungsten nitrate.
3. The heavy metal contaminated soil conditioner according to claim 1, wherein the soluble cobalt salt and the iron salt are cobalt nitrate, cobalt sulfate, ferric nitrate and ferric sulfate respectively.
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| CN202210183903.2A CN114524458B (en) | 2022-02-28 | 2022-02-28 | Preparation and application of heavy metal contaminated soil conditioner |
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| CN107469769A (en) * | 2017-09-06 | 2017-12-15 | 河海大学 | A kind of preparation method and applications of magnetic adsorptive material |
| CN109926063B (en) * | 2019-04-04 | 2021-11-30 | 台州学院 | Preparation method of copper tungstate nanofiber photocatalyst |
| CN110441365B (en) * | 2019-09-16 | 2021-07-02 | 石河子大学 | Detection method of iron-based spinel for heavy metal ion electrochemical sensor |
| CN112934166A (en) * | 2021-03-16 | 2021-06-11 | 莱西市两山环境生态科技中心 | Soil remediation material |
| CN113718372B (en) * | 2021-08-26 | 2022-11-25 | 山东大学 | Low-pollution high-magnetism cobalt ferrite fiber and preparation method thereof |
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