CN115504513B - Preparation method and application of porous calcium iron@magnesium iron composite spinel with heterojunction structure - Google Patents
Preparation method and application of porous calcium iron@magnesium iron composite spinel with heterojunction structure Download PDFInfo
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- CN115504513B CN115504513B CN202211285016.2A CN202211285016A CN115504513B CN 115504513 B CN115504513 B CN 115504513B CN 202211285016 A CN202211285016 A CN 202211285016A CN 115504513 B CN115504513 B CN 115504513B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
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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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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Abstract
The invention discloses a preparation method and application of porous calcium iron@magnesium iron composite spinel with a heterojunction structure. The method comprises the steps of mixing and reacting a dispersion liquid of calcium salt and ferric salt with a magnesium hydroxide dispersion liquid, roasting a product, adding the product into an ammonium chloride solution, stirring and reacting, and centrifugally drying to obtain the porous calcium iron@magnesium iron composite spinel with the heterojunction structure. The raw materials used in the method can completely enter the product, a large amount of salt-containing wastewater can not be generated, and no by-product is generated. The composite spinel material prepared by the invention has strong magnetism and is favorable for recycling; the material also has a large specific surface area and rich pore structures, and active sites are fully exposed, so that the adsorption quantity and adsorption efficiency are improved; therefore, the material has good application prospect in the aspect of pollutant removal.
Description
Technical Field
The invention belongs to the technical field of inorganic material synthesis and heavy metal ion removal, and particularly relates to synthesis of porous calcium iron@magnesium iron composite spinel with a heterojunction structure and application of porous calcium iron@magnesium iron composite spinel to removal of heavy metal arsenic and cadmium in soil.
Background
Land is the basis for everything to survive, however soil pollution is increasingly serious, wherein soil heavy metal pollution becomes a global problem affecting human health. Over five million areas of the world exist, and soil covering 2000 hectares of land is contaminated with different heavy metals, and the management of heavy metal pollution of soil is urgent. Soil heavy metal pollution is a ubiquitous environmental problem in China, and the pollution of heavy metal to farmland soil can seriously affect food quality and safety, so that risks are formed to human health through a food chain.
Arsenic (As) compounds have been recognized by the international cancer research institute As a first class of carcinogens, have high fluidity in soil, and diffuse into groundwater by means of migration and permeation, etc., and are extremely harmful to the human body, whether ingested orally, skin contacted, or inhaled through the respiratory tract. And heavy metal cadmium (Cd) also has high toxicity, bioaccumulation and concealment, and the continuous existence of the cadmium in the soil can cause the crops to be damaged, thereby endangering the health of human bodies. Therefore, the development of a soil heavy metal restoration agent with high adsorption efficiency, high selectivity, environmental protection and low cost is urgently needed to remove heavy metal arsenic and cadmium pollution in soil.
The existing materials for repairing heavy metal pollution have many characteristics such as dihydroxyl metal hydroxides (LDHs), such as alkalinity, interlayer anion exchange property, memory effect and the like, so that the materials have obvious advantages in the aspect of heavy metal removal. However, the material can only reduce the bioavailability of heavy metals in an in-situ mineralization mode, but the heavy metal elements are still remained in the soil, and the possibility of secondary pollution still exists when the external conditions change.
The magnetic material has excellent performance in terms of solid-liquid separation, such as the characteristic surface effect and magnetic response characteristic of the magnetic nano material, so that the magnetic material can be efficiently recovered when being used as a heavy metal ion adsorbent, and is simple in desorption in use, thereby avoiding secondary pollution. There are many studies on using magnetic materials for restoring heavy metals in soil or water and utilizing the magnetism thereof to perform rapid separation by adopting physical modes such as magnets, such as carbon-based magnetic composite materials, mesoporous silicon magnetic composite materials, metal and oxide magnetic composite materials, metal organic frameworks and other magnetic composite materials. However, the materials have some common problems at present: the conventional magnetic material has small specific surface area, small adsorption capacity and low efficiency, while some organic composite magnetic materials have high specific surface area and high adsorption capacity, but have high price, the preparation process is complex, and some polluted organic raw materials are used, so that the use of the materials is severely limited.
Disclosure of Invention
The invention provides a green, simple and efficient method for preparing porous calcium iron@magnesium iron composite spinel with a heterojunction structure and application of the porous calcium iron@magnesium iron composite spinel in removing heavy metals such as arsenic and cadmium in soil. Compared with other conventional methods, the raw materials used in the method can completely enter the product, so that a large amount of salt-containing wastewater can not be generated, and no by-product is generated. In the chemical reaction of the preparation process, magnesium hydroxide is used as a magnesium source and provides an alkaline environment; the organic calcium provides a calcium source, and meanwhile, the organic functional group realizes a pore-forming function, so that the specific surface area is increased; the introduction of the iron source not only provides the necessary constituent elements of the magnetic material, but also utilizes the specific action of the iron source and arsenic to realize the selective adsorption of the arsenic. The composite material prepared by the invention has strong magnetism and is favorable for recycling; the active sites are fully exposed, so that the adsorption quantity is improved, and the adsorption efficiency is improved; therefore, the material has good application prospect in the aspect of pollutant removal. In addition, the raw materials used in the invention are all biological friendly materials, wherein calcium, magnesium and iron are all nutrient elements necessary for plants and human bodies, so that the environment is not damaged, and secondary pollution is not generated.
The preparation method of the porous calcium iron@magnesium iron composite spinel with the heterojunction structure comprises the following steps: mixing the dispersion liquid of calcium salt and ferric salt with the magnesium hydroxide dispersion liquid, stirring and reacting for 3-6 hours at 80-140 ℃, centrifugally washing and drying the product, roasting for 3-6 hours at 600-800 ℃, naturally cooling, adding into an ammonium chloride solution, stirring for 4-8 hours at 50-90 ℃, centrifuging, and drying to obtain the porous calcium iron@magnesium iron composite spinel with the heterojunction structure.
The concentration of the magnesium hydroxide dispersion liquid is 0.2-1.5mol/L.
The calcium salt is one or more of calcium alginate, calcium oxalate and calcium citrate; the ferric salt is one or two of ferric nitrate and ferric chloride.
The concentration of the calcium salt in the dispersion liquid of the calcium salt and the ferric salt is 0.1-1.5mol/L, and the concentration of the ferric salt is 0.1-1.5mol/L.
The mass ratio of magnesium element, calcium element and iron element after the dispersion liquid is mixed is 1-3:1:1.
The roasted product is added into an ammonium chloride solution, and the addition amount is 1-10% of the mass of the ammonium chloride solution.
The mass fraction of ammonium chloride in the ammonium chloride solution is 20-30%.
The application of the prepared porous calcium iron@magnesium iron composite spinel with the heterojunction structure in removing heavy metals in soil.
The invention has the beneficial effects that:
(1) The raw materials required for preparation have wide sources, good biocompatibility and no secondary pollution; the preparation method is simple, has high efficiency, can be generated in a large scale, does not generate byproduct salt in the reaction process, and reduces the wastewater treatment cost.
(2) The prepared material has high magnetic saturation strength (up to 74 emu/g), and is favorable for the rapid separation of magnetic materials; (3) The prepared material has large specific surface area (up to 327m 2 And/g) and abundant pore structures, which is beneficial to the adsorption of heavy metal arsenic and cadmium.
Drawings
Fig. 1 is an XRD pattern of porous calcium iron @ magnesium iron composite spinel of the heterojunction structure of example 1.
Fig. 2 is a hysteresis loop diagram of porous calcium iron @ magnesium iron composite spinel of the heterojunction structure of example 1.
Fig. 3 is a pore size distribution plot of porous calcium iron @ magnesium iron composite spinel of the heterojunction structure of example 1.
Fig. 4 is an XRD pattern of porous calcium iron @ magnesium iron composite spinel of heterojunction structure in application example 2.
Fig. 5 is a scanning electron microscope image of a porous calcium iron @ magnesium iron composite spinel of the heterojunction structure in application example 2.
Fig. 6 is a transmission electron microscope image of porous calcium iron @ magnesium iron composite spinel of the heterojunction structure in application example 3.
Fig. 7 is a BET plot of porous calcium iron @ magnesium iron composite spinel of heterojunction structure in application example 3.
Detailed Description
The invention will be further illustrated by the following specific examples in order to provide a better understanding of the manner in which the invention operates, but the scope of the invention is not limited thereto.
Example 1:
(1) 2.33g (0.04 mol, mg (OH)) of magnesium hydroxide was weighed out 2 ) Dispersing in 100ml deionized water to obtain suspension A; 11.68g (0.02 mol, C) of calcium alginate are weighed 18 H 24 O 19 Ca) and 8.08g (0.02 mol, fe (NO) 3 ) 3 ·9H 2 O) was dispersed in 100ml of deionized water to obtain a mixed solution B. Mixing the suspension APouring into a reactor with the rotating speed of 3000rpm, rapidly stirring for 5min, rapidly adding the suspension B, reacting at 85 ℃ for 4 hours, centrifuging, collecting solid, and drying in a 50 ℃ oven for 12 hours to obtain a substance C;
(2) Placing the substance C in a muffle furnace at 600 ℃ for roasting for 4 hours, and naturally cooling to obtain a substance D;
(3) And weighing 5g D substances, adding the substances into 100ml of ammonium chloride solution with the mass fraction of 20%, mechanically stirring at 60 ℃ for 6 hours, centrifuging, and drying to obtain the porous calcium iron@magnesium iron composite spinel with the heterojunction structure.
Fig. 1 is an XRD pattern of porous calcium iron @ magnesium iron composite spinel of heterojunction structure prepared in example 1. As can be seen from fig. 1, each diffraction peak in the XRD diffraction pattern of the porous calcium iron@magnesium iron composite spinel with the heterojunction structure prepared in example 1 can correspond to the standard patterns of the calcium iron spinel and the magnesium iron spinel, which indicates that the method provided by the invention can synthesize the pure porous calcium iron@magnesium iron composite spinel with the heterojunction structure.
Fig. 2 is a hysteresis loop diagram of porous calcium iron @ magnesium iron composite spinel of heterojunction structure prepared in example 1. As can be seen from fig. 2, the porous calcium iron@magnesium iron composite spinel of the heterojunction structure prepared in example 1 shows excellent magnetic properties, reaching 75.1emu/g.
FIG. 3 is a pore size distribution plot of porous Ca-Fe @ Mg-Fe composite spinel of heterojunction structure prepared in example 1. As can be seen from fig. 3, the porous calcium iron@magnesium iron composite spinel with the heterojunction structure prepared in example 1 has a rich pore structure, and the pore size distribution is 10-20 nm.
Example 2:
(1) 3.50g (0.06 mol, mg (OH)) of magnesium hydroxide was weighed out 2 ) Dispersing in 100ml deionized water to obtain suspension A; 4.98g (0.01 mol, C) of calcium citrate are weighed 12 H 10 Ca 3 O 14 ) And ferric nitrate 12.12g (0.03 mol, feCl) 3 ·9H 2 O) was dispersed in 100ml of deionized water to obtain a mixed solution B. Pouring the suspension A into a reactor with the rotating speed of 3000rpm, rapidly stirring for 5min, and rapidly stirring the suspension BAdding, reacting for 4 hours at 85 ℃, centrifugally collecting solids, and drying in a 50 ℃ oven for 12 hours to obtain a substance C;
(2) Placing the substance C in a muffle furnace at 600 ℃ for roasting for 4 hours, and naturally cooling to obtain a substance D;
(3) 3g D substances are weighed and added into 100ml of ammonium chloride solution with the mass fraction of 25%, the mixture is mechanically stirred for 4 hours at the temperature of 80 ℃ and then centrifugally separated, and the porous calcium iron@magnesium iron composite spinel is obtained after drying.
Fig. 4 is an XRD pattern of porous calcium iron @ magnesium iron composite spinel of heterojunction structure prepared in example 2. As can be seen from fig. 4, each diffraction peak in the XRD diffraction pattern of the porous calcium iron@magnesium iron composite spinel with the heterojunction structure prepared in example 2 can correspond to the standard patterns of the calcium iron spinel and the magnesium iron spinel, which indicates that the method provided by the invention can synthesize pure calcium iron@magnesium iron composite spinel with the heterojunction structure.
Fig. 5 is a scanning electron microscope image of the porous calcium iron @ magnesium iron composite spinel of the heterojunction structure prepared in example 2. As can be seen from fig. 5, the porous calcium iron@magnesium iron composite spinel of the heterojunction structure prepared in example 2 exhibits a two-dimensional platelet structure with a particle size of about 50nm.
Example 3:
(1) 3.50g (0.06 mol, mg (OH)) of magnesium hydroxide was weighed out 2 ) Dispersing in 100ml deionized water to obtain suspension A; 2.56g (0.02 mol, caC2O 4) of calcium oxalate and 10.82g (0.04 mol, feCl) of ferric chloride were weighed out 3 ·6H 2 O) was dispersed in 100ml of deionized water to obtain a mixed solution B. Pouring the suspension A into a reactor with the rotating speed of 3000rpm, rapidly stirring for 5min, rapidly adding the suspension B, reacting at 60 ℃ for 4 hours, centrifugally collecting solids, and drying in a 50 ℃ oven for 12 hours to obtain a substance C;
(2) Placing the substance C in a muffle furnace at 600 ℃ for roasting for 4 hours, and naturally cooling to obtain a substance D;
(3) 3g D substances are weighed and added into 100ml of ammonium chloride solution with the mass fraction of 30%, the mixture is mechanically stirred for 6 hours at the temperature of 80 ℃ and then centrifugally separated, and the porous calcium iron@magnesium iron composite spinel is obtained after drying.
Fig. 6 is a transmission electron microscopy image of porous calcium iron @ magnesium iron composite spinel of heterojunction structure prepared in example 3. As can be seen from fig. 6, the porous calcium iron@magnesium iron composite spinel with the heterojunction structure prepared in example 3 exhibits random nano-particles with a particle size of about 3-5 nm.
Fig. 7 is a graph of nitrogen adsorption and desorption of porous calcium iron @ magnesium iron composite spinel of heterojunction structure prepared in example 3. As can be seen from FIG. 7, the porous calcium-iron@magnesium-iron composite spinel of the heterojunction structure prepared in example 3 has a specific surface area as high as 327m 2 /g。
Application example 1:
the porous calcium iron@magnesium iron composite spinel with the heterojunction structure is used for removing arsenic and cadmium in soil:
400mg kg of As (III) containing -1 、Cd(Ⅱ)4mg kg -1 Is a soil of the plant. Two soil portions of 20g were weighed, the first soil sample was not added with any passivating agent, and the other soil sample was added with 0.5% (0.1 g) of the porous calcium iron@magnesium iron composite spinel of the heterojunction structure prepared in example 1 relative to the soil mass. Respectively adding 20mL of deionized water into the two samples, carrying out ultrasonic treatment until the soil and the mineralizer are completely dispersed, respectively placing the two samples on a magnetic stirrer at the stirring speed of 400rpm, placing the soil samples in an oven at 45 ℃ for 12h after stirring for 4 days to dry the water, and fully grinding the soil samples by using a mortar. Porous calcium iron @ magnesium iron composite spinel in soil is separated from the soil using strong magnets. And after digestion of the residual soil sample, detecting the As (III) content and the Cd (II) content in the sample by using ICP-MS. The result shows that compared with the soil without the porous calcium iron@magnesium iron composite spinel, the contents of As and Cd in the soil with the porous calcium iron@magnesium iron composite spinel are respectively reduced by 35.3% and 28.5%, and the prepared porous calcium iron@magnesium iron composite spinel can effectively reduce heavy metal arsenic and cadmium in the soil, so that the restoration effect is achieved.
Claims (8)
1. The preparation method of the porous calcium iron@magnesium iron composite spinel with the heterojunction structure is characterized by comprising the following specific steps of: mixing the dispersion liquid of calcium salt and ferric salt with the magnesium hydroxide dispersion liquid, stirring and reacting for 3-6 hours at 80-140 ℃, centrifugally washing and drying the product, roasting for 3-6 hours at 600-800 ℃, naturally cooling, adding into an ammonium chloride solution, stirring for 4-8 hours at 50-90 ℃, centrifuging, and drying to obtain the porous calcium iron@magnesium iron composite spinel with the heterojunction structure.
2. The method according to claim 1, wherein the concentration of the magnesium hydroxide dispersion is 0.2 to 1.5mol/L.
3. The preparation method according to claim 1, wherein the calcium salt is one or more of calcium alginate, calcium oxalate and calcium citrate; the ferric salt is one or two of ferric nitrate and ferric chloride.
4. The method according to claim 1, wherein the concentration of the calcium salt in the dispersion of the calcium salt and the iron salt is 0.1 to 1.5mol/L and the concentration of the iron salt is 0.1 to 1.5mol/L.
5. The method according to claim 1, wherein the amount ratio of magnesium element, calcium element, iron element substances after mixing the dispersion is 1-3:1:1.
6. The preparation method according to claim 1, wherein the calcined product is added to the ammonium chloride solution in an amount of 1-10% by mass of the ammonium chloride solution.
7. The preparation method according to claim 1, wherein the mass fraction of ammonium chloride in the ammonium chloride solution is 20-30%.
8. Use of porous calcium iron @ magnesium iron composite spinel of a heterojunction structure prepared by the method according to any one of claims 1-7 in removing heavy metals in soil.
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| CN1646436A (en) * | 2002-04-03 | 2005-07-27 | 圣戈本陶瓷及塑料股份有限公司 | Spinel substrate and heteroepitaxial growth of III-V materials thereon |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1646436A (en) * | 2002-04-03 | 2005-07-27 | 圣戈本陶瓷及塑料股份有限公司 | Spinel substrate and heteroepitaxial growth of III-V materials thereon |
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