CN111111605B - Magnetic nano adsorbent for removing heavy metal chromium and preparation method and application thereof - Google Patents
Magnetic nano adsorbent for removing heavy metal chromium and preparation method and application thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
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Abstract
The invention discloses a magnetic nano adsorbent for removing heavy metal chromium, which is a nano material of sulfur-doped iron lanthanum bimetallic oxide, and a preparation method thereof, wherein the preparation method comprises the following steps: 1) Dissolving an iron ion compound and a ferrous ion compound by deionized water, and adding an alkaline reagent to obtain a turbid solution; 2) Adding LaCl into the turbid solution 3 ·6H 2 O and H 2 NCSNH 2 And adding hydrazine hydrate after stirring at a controlled temperature, filtering and drying to obtain the sulfur-doped iron lanthanum bimetal oxide nano material, wherein the material has high efficiency of adsorbing heavy metal chromium, no secondary pollution, strong repeatability and stability, and the adsorbent is convenient to recover.
Description
Technical Field
The invention relates to the field of heavy metal treatment, in particular to a magnetic nano adsorbent for removing heavy metal chromium and a preparation method and application thereof.
Background
Because the tobacco planting soil in tobacco areas in China has heavy metal pollution in different degrees. Among them, chromium metal has a great toxic effect on tobacco. When the chromium content in the soil reaches a certain value, the growth and development of the tobacco plants are completely inhibited. In addition, heavy metals accumulated in the tobacco may enter a human body along with smoke when the cigarette is combusted, so that certain influence is caused on human health. Therefore, the research on the prevention and control of the heavy metal in the tobacco is an important content for the quality safety control of the tobacco.
In recent years, metal oxide materials have been widely used for adsorbing water and heavy metals in soil. However, in the adsorption process, metal ions with a certain concentration are transferred from the surface of the material to the reaction system, and the metal ions in the solution cause secondary pollution to the environment. In addition, these materials are not easily recycled after use and are difficult to reuse, thereby limiting their development and use. Based on this, the stability and repeatability of the material have become important indexes for measuring the quality of the material.
Disclosure of Invention
In order to solve the problems, the invention provides the magnetic nano adsorbent for removing the heavy metal chromium and the preparation method and application thereof, the efficiency of adsorbing the heavy metal chromium is high, secondary pollution is avoided, the repeatability and the stability are strong, and the adsorbent is convenient to recover.
The technical scheme of the invention is to provide a magnetic nano adsorbent for removing heavy metal chromium, wherein the adsorbent is a nano material of sulfur-doped iron lanthanum bimetallic oxide.
Further, a preparation method of the magnetic nano adsorbent for removing heavy metal chromium is provided, and comprises the following steps:
1) Dissolving an iron ion compound and a ferrous ion compound by deionized water, and adding an alkaline reagent to obtain a turbid solution;
2) Adding LaCl into the turbid solution 3 ·6H 2 O and H 2 NCSNH 2 And adding hydrazine hydrate after stirring at a controlled temperature, filtering and drying to obtain the sulfur-doped iron lanthanum bimetal oxide nano material.
Preferably, the iron ion compound comprises FeCl 3 ·6H 2 O, the ferrous ion compound comprises FeSO 4 ·7H 2 O。
Preferably, in the step 1), the alkaline reagent comprises ammonia water, and the pH of the turbid liquid is 9-10.
Preferably, the reaction temperature of the step 2) is 80-100 ℃, preferably, the reaction temperature is 90 ℃, and the stirring time is 60min.
Preferably, the hydrazine hydrate is reacted with the LaCl 3 ·6H 2 The molar ratio of O is 1.
Preferably, the FeCl 3 ·6H 2 O and FeSO 4 ·7H 2 The molar ratio of O is 2.
Preferably, feCl 3 ·6H 2 O and LaCl 3 ·6H 2 The molar ratio of O is 1 3 ·6H 2 O and LaCl 3 ·6H 2 The molar ratio of O is 2.
Preferably, the FeCl 3 ·6H 2 O and H 2 NCSNH 2 1-3, preferably the molar ratio of FeCl 3 ·6H 2 O and H 2 NCSNH 2 1 is 1.
Further, the application of the magnetic nano adsorbent for removing the heavy metal chromium is also provided, and the magnetic nano adsorbent is characterized in that after the adsorbent is thrown into tobacco planting soil or water to adsorb the heavy metal chromium, the adsorbent is recovered by a magnet.
In the scheme, metal ions form metal oxide by a coprecipitation method under an alkaline condition, and the obtained metal oxide can be directly used after being dried without further calcination, so that the reaction time and the cost are greatly saved. In addition, the metal oxide formed by the process has higher specific surface area, which is caused by introducing sulfur element into the material. The sulfur element replaces the lattice position of partial oxygen element to reduce the vacancy of the material, so that the metal element is combined more tightly, the material is more stable and the repeatability is good. The high valence state iron in the scheme is very stable, has strong binding capacity with sulfur oxide and stable bonding, so that the S-LaFeO has strong stability, and prevents the phenomenon that metal ions migrate from the surface of the material to an adsorption system in the process of adsorbing heavy metals. On the other hand, iron is less harmful to the environment than copper. The invention has the beneficial effects that:
1. the rare earth element lanthanum oxide in the material improves the adsorption efficiency of the chromium metal;
2. the sulfur is doped in the material, so that all metal elements are combined more tightly, and the stability of the metal oxide is effectively improved.
3. Hydrazine hydrate is used as an alkaline reducing agent to reduce part of high-valence metals in the reaction process, and the material is rich in a large amount of low-valence metals, thereby being beneficial to the adsorption of chromium metal.
4. The high-valence iron is very stable, has strong binding capacity with sulfur oxide and stable bonding, so that the S-LaFeO has strong stability, the phenomenon that metal ions migrate from the surface of the material to an adsorption system in the process of adsorbing heavy metals is prevented, the metal ions are not lost, and the material repeatability is stronger.
5. The obtained sulfur-doped metal oxide contains a certain amount of ferroferric oxide, has strong magnetism, is convenient to recover and has high recovery rate.
Drawings
FIG. 1 is a scanning electron microscope photograph of the S-LaFeO nano-material prepared by the invention;
FIG. 2 is a transmission electron microscope photograph of the S-LaFeO nano-material prepared by the invention;
FIG. 3 shows FeCl 3 ·6H 2 O and LaCl 3 ·6H 2 A test result chart of the influence of the molar ratio of O on the adsorbability of the material;
FIG. 4 shows hydrazine hydrate and LaCl 3 ·6H 2 The influence of the molar ratio of O on the adsorbability of the material is shown in a test result graph;
FIG. 5 is a diagram showing the test results of different concentrations of metallic chromium in the adsorbed soil for S-LaFeO nano-material;
FIG. 6 is a comparison graph of adsorption effects of different adsorption materials on heavy metal chromium with the same concentration in soil;
FIG. 7 is a graph comparing the mobility results of metal ions transferred from the surface to the reaction system for different adsorption materials;
FIG. 8 is a diagram showing the adsorption effect of the S-LaFeO nanomaterial on hexavalent chromium in soil after being recycled for multiple uses;
FIG. 9 is a test chart of adsorption results of S-LaFeO nano-materials on heavy metal chromium with different concentrations in water;
FIG. 10 is a graph showing the adsorption effect of different adsorption materials on hexavalent chromium in water after being recycled for multiple uses.
Detailed Description
In order to more clearly illustrate the embodiments of the present invention and the technical solutions in the prior art, the following description will be made with reference to the accompanying drawings.
It is obvious that the drawings in the following description are only some examples of the invention, and it is obvious to a person skilled in the art that other drawings and other embodiments can be obtained from these drawings without inventive effort, and the invention is not limited to this example.
In the scheme, the preparation method of the magnetic nano adsorbent for removing heavy metal chromium comprises the following specific operation steps:
FeCl is added 3 ·6H 2 O and FeSO 4 ·7H 2 O is dissolved in deionized water, wherein FeCl 3 ·6H 2 O and FeSO 4 ·7H 2 And the molar ratio of O is 2. Adding LaCl after the solution is turbid 3 ·6H 2 O and H 2 NCSNH 2 So that FeCl is brought into contact 3 ·6H 2 O and LaCl 3 ·6H 2 1-4 molar ratio of O 3 ·6H 2 O and H 2 NCSNH 2 1-3, at a temperature of 80-100 ℃, continuously stirring for 60min, and finally adding hydrazine hydrate, hydrazine hydrate and LaCl 3 ·6H 2 And (3) the molar ratio of O is 1.
Example 1
FeCl 3 ·6H 2 O and FeSO 4 ·7H 2 Dissolving O in deionized water, slowly adding ammonia water under stirring, and continuously stirring for 30 min. After the solution is turbid, addingLaCl 3 ·6H 2 O，FeCl 3 ·6H 2 O and LaCl 3 ·6H 2 Molar ratio of O 2 NCSNH 2 Continuously stirring for 60min at a certain temperature, finally adding hydrazine hydrate, fully reacting, filtering and drying.
Fig. 1 is a scanning electron microscope photograph of the sulfur-doped iron lanthanum bimetallic oxide prepared by the method. As can be seen from fig. 1, the surface of the sulfur-doped iron lanthanum bimetallic oxide obtained in the present embodiment is uneven, has a micro void structure, has a large specific surface area, and can increase the adsorption amount of heavy metal chromium.
Fig. 2 is a transmission electron microscope photograph of the sulfur-doped iron lanthanum bimetallic oxide prepared by the method. As can be seen from fig. 2, the sulfur-doped iron lanthanum bimetallic oxide obtained in this embodiment has uniform particles, a diameter of about 5nm to 8nm, and a more stable material structure.
In the experimental test, feCl is selected 3 ·6H 2 O and LaCl 3 ·6H 2 When the molar ratio of O is 1 3 ·6H 2 O and LaCl 3 ·6H 2 The increase in the molar ratio of O increases first and then decreases as shown in fig. 3. By comparison, feCl 3 ·6H 2 O and LaCl 3 ·6H 2 When the molar ratio of O is 2.
Example 2
FeCl is added 3 ·6H 2 O and FeSO 4 ·7H 2 Dissolving O in deionized water, slowly adding ammonia water under stirring, and continuously stirring for 30 min. Adding LaCl after the solution is turbid 3 ·6H 2 O，FeCl 3 ·6H 2 O and LaCl 3 ·6H 2 The molar ratio of O is 2 2 NCSNH 2 Continuously stirring for 60min at a certain temperature, finally adding hydrazine hydrate, fully reacting, filtering and drying. In experimental tests, the adsorptivity of the material increased first and then decreased with increasing number of moles of hydrazine hydrate, as shown in fig. 4. By comparison, the molar ratio of hydrazine hydrate to lacl3.6h2o is 1:1, the material has the best adsorption performance.
Example 3
The nano-sized sulfur-doped iron lanthanum bimetallic oxide with magnetism prepared according to the method of example 2 was subjected to adsorption test.
By adopting a pot experiment, reagents with different concentrations of chromium metal are prepared according to 20kg of soil in each pot, and the concentrations are respectively 50 mg/kg, 100 mg/kg, 200 mg/kg, 300 mg/kg and 500 mg/kg. Within 1 week after the tobacco seedlings are transplanted and survive, the adsorbent S-LaFeO prepared by the scheme is treated, sequentially poured into pots one by one, and sprayed with distilled water in contrast. Each concentration was treated for 5 tubs separately. Topping buds, cultivating in a standardized way, harvesting the buds after ripening, and baking in a three-stage way. The tobacco leaf samples are taken to analyze the heavy metal residual quantity of the tobacco leaves, and the adsorption removal rate is calculated, and the results are shown in figure 5, and the adsorbent in the soil with different concentrations of metal chromium has obvious adsorption.
Example 4
Taking the concentration of hexavalent chromium in the soil as 100 mg/kg, and mixing the magnetic nano-scale sulfur-doped iron lanthanum bimetallic oxide adsorbent S-LaFeO prepared by the method in the embodiment 2 with different nano-metal oxides LaFeO, S-LaO, S-FeO and Fe 3 O 4 、La 2 O 3 S-LaCuO and S-CuFeO are used for carrying out adsorption comparison experiments;
the LaFeO, S-LaO, S-FeO and Fe 3 O 4 、La 2 O 3 The preparation processes of the materials such as S-LaCuO, S-CuFeO and the like are the same as those of S-LaFeO, and are prepared according to the synthesis steps of the scheme, and the difference is that the used raw materials are different, for example, the synthesis steps of LaFeO are as follows: feCl 3 ·6H 2 O and FeSO 4 ·7H 2 O is dissolved in deionized water, wherein FeCl 3 ·6H 2 O and FeSO 4 ·7H 2 And the molar ratio of O is 2. Adding LaCl after the solution is turbid 3 ·6H 2 O, making FeCl 3 ·6H 2 O and LaCl 3 ·6H 2 The molar ratio of O is 1-4 3 ·6H 2 And the molar ratio of O is 1. The method comprises the following specific steps: by adopting a pot experiment, preparing a concentration reagent of 100 mg/kg of metallic chromium according to 20kg of soil per pot, and sequentially pouring 20mg/kg of S-LaFeO, S-LaO, S-FeO and Fe in each pot within 1 week after the tobacco seedlings are transplanted and survive 3 O 4 、La 2 O 3 S-LaCuO and S-CuFeO metal oxides, each concentration of which is treated for 5 basins respectively. Topping buds, cultivating in standardization, harvesting after maturation, and baking in three stages. The tobacco leaf samples are taken to analyze the residual quantity of heavy metals in the tobacco leaves, and the adsorption removal rate is calculated, and the result is shown in fig. 6, which shows that compared with other nano metal oxides, the nano sulfur-doped iron lanthanum bimetallic oxide adsorbent S-LaFeO prepared by the scheme has the highest removal rate of heavy metal chromium.
Example 5
Taking the concentration of hexavalent chromium in the soil as 100 mg/kg, and mixing the magnetic nano-scale S-doped Fe-La bimetallic oxide adsorbent S-LaFeO prepared by the method in the embodiment 2 with different nano-metal oxides LaFeO, S-LaO, S-FeO and Fe 3 O 4 、La 2 O 3 S-LaCuO and S-CuFeO are used for metal ion migration experiments to verify the stability of the material, and the ratio of metal ions transferred from the surface of the material to a reaction system is used as a judgment principle;
the LaFeO, S-LaO, S-FeO and Fe 3 O 4 、La 2 O 3 The preparation processes of the materials such as S-LaCuO, S-CuFeO and the like are the same as those of S-LaFeO, and the materials are prepared by laboratory synthesis.
The method comprises the following specific steps: adopting pot experiment, preparing 100 mg/kg chromium metal concentration reagent according to 20kg soil per pot, processing, sequentially pouring equal amount of S-LaFeO, S-LaO, S-FeO and Fe within 1 week after the tobacco seedling is transplanted and survived 3 O 4 、La 2 O 3 S-LaCuO and S-CuFeO metal oxides, each concentration of which is treated for 5 basins respectively. 100g of the soil treated with the heavy metal chromium is respectively taken, diluted by 10 times by deionized water, and the concentration of the corresponding metal ions in different metal oxides transferred into the soil is measured, and the result is shown in figure 7, which illustrates the methodThe nano-scale sulfur-doped iron lanthanum bimetallic oxide adsorbent S-LaFeO prepared by the scheme has small mobility and high stability, and is not easy to cause secondary pollution.
The S-LaCuO material can separate out a large amount of copper ions in the process of adsorbing heavy metals, thereby causing secondary pollution to the environment. The main reason why the copper element is separated out is that the low-valence copper element originally contained in the material is unstable and is easily oxidized in the use process, and the binding energy between high-valence copper ions and sulfur oxide is weakened, so that the bonding is easily broken, and the stability of the material is finally influenced. Therefore, iron is used to replace copper, and the high valence state iron in the new material is more stable than the high valence state copper.
Example 6
The nano-scale sulfur-doped iron lanthanum bimetallic oxide adsorbent S-LaFeO material obtained in the embodiment 2 is subjected to a recycling test, potted soil which has adsorbed heavy metal chromium is scattered and refined, the nano material in the scheme is recovered by using a magnet, the recovery rate is 63%, the recovered S-LaFeO nano material is subjected to alkali desorption of heavy metal chromium, the heavy metal chromium is reused after filtration and drying, an adsorption experiment is carried out on 100 mg/kg heavy metal chromium in the soil according to the proportion of the weight of the soil and the weight of the adsorbent used in the embodiment 3 (20 kg soil corresponds to 20mg/kg adsorbent), the heavy metal chromium is repeatedly recovered according to the steps, the removal rate of the material on 100 mg/kg heavy metal chromium in the soil after multiple times of recovery is measured, and the result is shown in FIG. 8, and the material still has a very high adsorption removal rate when being used for the fifth time. This shows that the material has good stability, the recovery and the cyclic utilization of the material are high, and the use cost is greatly reduced.
Example 7
The magnetic nano-scale sulfur-doped iron lanthanum bimetallic oxide adsorbent S-LaFeO prepared by the method in the embodiment 2 is applied to adsorbing heavy metal chromium in water, and the method comprises the following specific steps: preparing metal chromium mother liquor with different concentrations, namely 50 mg/L, 100 mg/L, 200 mg/L, 300 mg/L and 500 mg/L, and respectively adding 0.1 g/L of adsorbent: S-LaFeO, S-LaO, S-FeO, fe 3 O 4 、La 2 O 3 S-LaCuO, S-CuFeO, filtering and dryingAnd (4) taking the treated water solution sample to analyze the residual quantity of the heavy metal, reusing each recovered and dried adsorbing material, and calculating the adsorption removal rate after repeated use.
The results are shown in fig. 9, which illustrates that the nano-scale sulfur-doped iron lanthanum bimetallic oxide adsorbent S-LaFeO prepared by the scheme has good adsorption effect on heavy metal chromium in water.
As shown in FIG. 10, the adsorbent S-LaFeO prepared by the scheme has higher recovery rate compared with other adsorbing materials, and the adsorption performance is more stable after the adsorbent S-LaFeO is used for multiple times.
Specific embodiments of the present invention have been described above in detail.
It should be understood that numerous modifications and variations can be devised by those skilled in the art in light of the above teachings. Therefore, any technical solutions that can be obtained by a person skilled in the art through logical analysis, reasoning or limited experiments based on the present inventive concept should be within the scope of protection defined by the claims.
Claims (9)
1. The magnetic nano adsorbent for removing heavy metal chromium is characterized in that the adsorbent is a nano material of sulfur-doped iron lanthanum bimetallic oxide; the preparation method of the magnetic nano adsorbent for removing the heavy metal chromium comprises the following steps:
1) Dissolving an iron ion compound and a ferrous ion compound by deionized water, and adding an alkaline reagent to obtain a turbid solution;
2) Adding LaCl into the turbid solution 3 ·6H 2 O and H 2 NCSNH 2 And adding hydrazine hydrate after stirring at a controlled temperature, filtering and drying to obtain the sulfur-doped iron lanthanum bimetal oxide nano material.
2. The magnetic nano-adsorbent for removing heavy metal chromium according to claim 1, wherein the iron ion compound comprises FeCl 3 ·6H 2 O, the ferrous ion compound comprises FeSO 4 ·7H 2 O。
3. The magnetic nano-adsorbent for removing heavy metal chromium according to claim 1, wherein in the step 1), the alkaline reagent comprises ammonia water, and the pH of the turbid liquid is 9-10.
4. The magnetic nano-adsorbent for removing heavy metal chromium according to claim 1, wherein the reaction temperature of the step 2) is 80-100 ℃.
5. The magnetic nano-adsorbent for removing heavy metal chromium according to claim 1, wherein the hydrazine hydrate and the LaCl are 3 ·6H 2 The molar ratio of O is 1.
6. The magnetic nano-adsorbent for removing heavy metal chromium according to claim 2, wherein the FeCl is 3 ·6H 2 O and FeSO 4 ·7H 2 The molar ratio of O is 2.
7. The magnetic nano-adsorbent for removing heavy metal chromium according to claim 2, wherein the FeCl is 3 ·6H 2 O and LaCl 3 ·6H 2 The molar ratio of O is 1.
8. The magnetic nano-adsorbent for removing heavy metal chromium according to claim 2, wherein the FeCl is 3 ·6H 2 O and H 2 NCSNH 2 1 to 3 in a molar ratio of 1.
9. The application of the magnetic nano-adsorbent for removing the heavy metal chromium according to claim 1, wherein after the adsorbent is thrown into tobacco planting soil or water to adsorb the heavy metal chromium, the adsorbent is recovered by a magnet.
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| CN107913662A (en) * | 2017-11-27 | 2018-04-17 | 中国科学院城市环境研究所 | A kind of novel Armco magnetic iron/lanthanum is compound except arsenic adsorbent material and preparation method thereof |
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| CN107913662A (en) * | 2017-11-27 | 2018-04-17 | 中国科学院城市环境研究所 | A kind of novel Armco magnetic iron/lanthanum is compound except arsenic adsorbent material and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| A label-free nano-probe for sequential and quantitative determination of Cr(VI) and ascorbic acid in real samples based on S and N dual-doped carbon dots;Shengmei Song等;《Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy》;20190221;第215卷;全文 * |
| Efficient removal of As(III) from aqueous solution by S-doped copperlanthanum bimetallic oxides: Simultaneous oxidation and adsorption;Yuxin Li等;《Chemical Engineering Journal》;20191023;第384卷;第123274页 * |
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