CN112934165A - Porous iron-manganese composite material for efficiently fixing and removing antimony pollution and preparation method and application thereof - Google Patents
Porous iron-manganese composite material for efficiently fixing and removing antimony pollution and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of adsorption materials, and discloses a porous iron-manganese composite material for efficiently fixing and removing antimony pollution, and a preparation method and application thereof. The method comprises the following steps: respectively preparing permanganate solution, manganese salt solution and iron salt solution from permanganate, manganese salt and iron salt; dropwise adding the permanganate solution into the manganese salt solution, and stirring to obtain a suspension; adding the ferric salt solution into the suspension, and stirring to obtain a mixed solution; and adjusting the pH value of the mixed solution to 6.5-8.5, performing aging treatment, centrifuging to obtain a precipitate, washing, drying, grinding and sieving to obtain the porous iron-manganese composite material for efficiently removing antimony pollution by fixation. The material has the characteristics of porosity, high specific surface area and stable adsorption; can be used for treating the pollution of trivalent antimony and pentavalent antimony, and has high removal rate and high adsorption capacity. The method is simple, the reaction condition is mild, and the energy consumption is low.
Description
Technical Field
The invention belongs to the technical field of adsorption materials, and particularly relates to a porous iron-manganese composite material for efficiently fixing and removing antimony pollution, and a preparation method and application thereof.
Background
Natural antimony exists mainly in the form of ore, with the main valences being sb (iii) and sb (v). The worldwide storage of antimony is 4-5 million tons, while the storage of antimony in China is the first place in the world. As a world producing antimony, the yield of China is about 79.6 percent of the total world. In recent years, the unreasonable exploitation of antimony ores and the irregular use of antimony-containing products have led to a dramatic rise in the content of antimony in soils, water and the atmosphere in china. Wherein the content of antimony in the environment of areas rich in antimony ores such as Hunan, Guizhou and Guangxi far exceeds the background value. The concentration of Sb in mine drainage and flotation industrial wastewater in China is as high as 30 mg.L-1. The investigation found that the concentration of Sb in the adjacent rivers of the delafossite and the delafossite in the great Bao mountain is as high as 900 and 52.7 mug/L.
Antimony is receiving increasing attention for its toxicity and biological effects. As the antimony can inhibit the growth of microorganisms and influence the activity of soil enzymes, the exceeding of the antimony content in the soil has great influence on the growth and the quality of crops, and has potential harm to human health. Antimony-containing dust exposed to the air can cause respiratory diseases in workers. Antimony poisoning can cause headache, dizziness, abdominal pain, constipation, and poor appetite. The united states environmental protection agency and the european union have listed antimony as a priority contaminant. The world health organization stipulates that the sanitary standard of antimony in drinking water is 20 ug/L. And the limit value of the concentration of antimony in the 'quality standard of surface water environment' (GB 3838-2002) in China is 0.005 mg/L.
How to develop a material capable of efficiently fixing trivalent antimony and pentavalent antimony has become one of the key points of research. Although there is a method for preparing a manganese-iron composite oxide and removing antimony in situ (CN201910961787.0), the manganese-iron composite reported in the literature has no porous structure, and the specific surface area of the adsorbing material is an important characteristic affecting the adsorption performance, so there is room for further improving the removal performance of pentavalent antimony. And the document does not discuss the removal effect of the iron-manganese composite material on the trivalent antimony. Antimony trioxide is more hazardous to ecosystem and needs more attention.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a porous iron-manganese composite material for efficiently removing antimony pollution by fixation and a preparation method and application thereof.
The invention aims to provide a preparation method of a porous iron-manganese composite material polluted by antimony. The prepared porous iron-manganese composite material can be used for treating trivalent antimony and pentavalent antimony pollution, and has the advantages of high removal rate and high adsorption quantity.
One of the purposes of the invention is to provide the porous iron-manganese composite material prepared by the preparation method. The porous iron-manganese composite material has the characteristics of abundant pore structures, high specific surface area and stability.
The invention also aims to provide application of the porous iron-manganese composite material. The porous iron-manganese composite material is used for treating the problem of antimony pollution (trivalent antimony and pentavalent antimony) in the environment.
The purpose of the invention is realized by at least one of the following technical solutions.
The porous iron-manganese composite material for efficiently fixing and removing antimony pollution is a porous iron-manganese composite material.
The preparation method of the porous iron-manganese composite material for efficiently and fixedly removing antimony pollution, provided by the invention, comprises the following steps of:
(1) respectively preparing soluble permanganate, soluble manganese salt and soluble iron salt into a permanganate solution, a manganese salt solution and an iron salt solution;
(2) slowly dripping the permanganate solution obtained in the step (1) into a manganese salt solution, and stirring to obtain a suspension;
(3) slowly adding an iron salt solution into the suspension liquid obtained in the step (2), and stirring to obtain a mixed liquid;
(4) and (4) adjusting the pH value of the mixed solution obtained in the step (3) to 6.5-8.5, then carrying out aging treatment, centrifuging to obtain a precipitate, washing, drying, grinding and sieving to obtain the porous iron-manganese composite material for efficiently removing antimony pollution by fixation.
Further, the permanganate in the step (1) is more than one of potassium permanganate and sodium permanganate; the manganese salt is more than one of manganese chloride, manganese nitrate and manganese sulfate; the ferric salt is more than one of ferric nitrate, ferric sulfate and ferric chloride; the molar ratio of the permanganate to the manganese salt to the iron salt is (1.5-9): (1-6): (2.5-15).
Preferably, the permanganate salt in the step (1) is potassium permanganate; the manganese salt is manganese chloride; the soluble ferric salt is ferric chloride.
Preferably, the molar ratio of the permanganate salt to the manganese salt to the iron salt is (3-6): (2-4): (5-10).
Further, the concentration of the permanganate solution in the step (1) is 0.015-0.090 mol/L; the concentration of the manganese salt solution is 0.010mol/L-0.060 mol/L; the concentration of the ferric salt solution is 0.025mol/L-0.150 mol/L.
Preferably, the solvents of the permanganate solution, the manganese salt solution and the iron salt solution in step (1) are all deionized water.
Further, the dropping rate of the permanganate solution dropped into the manganese salt solution in the step (2) is 0.1-5 mL/min; the stirring treatment time is 1-3 h.
Further, the speed of adding the iron salt solution into the suspension in the step (3) is 5-10ml/min, and the stirring treatment time is 1-3 h.
Further, the time of the aging treatment in the step (4) is 6-18 h.
Further, the centrifugation speed in the step (4) is 2000-6000rpm, and the centrifugation time is 10-20 min; the drying temperature is 40-80 ℃, and the drying time is 18-36 h; the size of the sieving mesh is 100-500 meshes.
Preferably, in the step (4), the mixed solution is adjusted to 6.5 to 8.5 by using ammonia water.
More preferably, in the step (4), the mixed solution is adjusted to 7.0 to 8.0 with ammonia water.
Preferably, the washing in step (4) is performed by washing the precipitate with deionized water, and the number of washing is 3-5.
The invention provides a porous iron-manganese composite material prepared by the preparation method and used for efficiently fixing and removing antimony pollution.
The porous iron-manganese composite material for efficiently fixing and removing antimony pollution provided by the invention can be applied to the aspect of treating heavy metal antimony pollution.
The porous iron-manganese composite material for efficiently removing antimony pollution is prepared based on the strong oxidizing property of manganese oxide, the strong affinity of iron oxide to antimony and the high fixing property of high-surface-area material to antimony due to the high adsorbability of the material to pollutants, and can be used for treating the problem of antimony pollution in the environment.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the preparation process is simple, the reaction condition is mild, the energy consumption is low, the yield is high, and the application prospect is wide;
(2) in the preparation method provided by the invention, elements in the used iron-manganese oxide are natural composition components, and the preparation method has the characteristics of low price, wide sources, no environmental pollution and the like; the selected reagent has low price and no toxicity.
(3) The porous iron-manganese composite material for efficiently and fixedly removing antimony pollution provided by the invention has developed pores and larger specific surface area, and is beneficial to removing pollutants;
(4) the porous iron-manganese composite material for efficiently and fixedly removing antimony pollution has excellent adsorbability for removing Sb (III) or Sb (V), and has the characteristics of high adsorption rate and large adsorption quantity.
Drawings
FIGS. 1a and 1b are SEM and EDS diagrams of a porous FeMn composite for efficient fixed removal of antimony contamination prepared in example 1, respectively;
FIG. 2 is a BET plot of the porous FeMn composite prepared in example 1;
FIG. 3 is an SEM image of the porous FeMn composite material prepared in example 2 and used for efficient fixed removal of antimony contamination;
FIG. 4 is an SEM image of the porous FeMn composite material prepared in example 3 and used for efficient fixed removal of antimony contamination;
FIGS. 5a and 5b are graphs showing the results of time versus the fixation of antimony by the porous FeMn composite for efficient fixation of antimony contamination in example 4;
FIGS. 6a and 6b are graphs showing the results of the initial concentration on the fixation of antimony by the porous FeMn composite for efficient fixation of antimony contamination in example 5.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but the practice and protection of the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
A preparation method of a porous iron-manganese composite material for efficiently fixing and removing antimony pollution comprises the following steps:
(1) respectively and accurately weighing 0.045mol of potassium permanganate, 0.030mol of manganese chloride and 0.075mol of ferric chloride, respectively adding the potassium permanganate, the 0.030mol of manganese chloride and the 0.075mol of ferric chloride into 1000mL of deionized water, and uniformly dissolving to obtain a potassium permanganate solution with a concentration of 0.045mol/L, a manganese chloride solution with a concentration of 0.030mol/L and a ferric chloride solution with a concentration of 0.075 mol/L;
(2) dripping the potassium permanganate solution into the manganese chloride solution at the dripping speed of 1mL/min, and then stirring for 2h to obtain a suspension;
(3) adding the ferric chloride solution into the suspension obtained in the step (2) at a dropping speed of 7.5mL/min, and stirring for 2h to obtain a mixed solution;
(4) and (3) adjusting the pH value of the mixed solution obtained in the step (3) to 7.5 by using ammonia water, aging for 12h, centrifuging at 4000rpm for 15min, removing supernatant, washing with deionized water for several times, drying at the temperature of 60 ℃ for 24h, grinding and sieving with a 200-mesh sieve to obtain the porous iron-manganese composite material for efficiently and fixedly removing antimony pollution.
The prepared porous iron-manganese composite material has the appearance and the specific surface area which are represented as shown in a figure 1a, a figure 1b and a figure 2. Wherein FIG. 1a is an SEM image, FIG. 1b is an EDS image, and FIG. 2 is a BET image. As can be seen from fig. 1a, 1b and 2, the obtained iron-manganese composite material has a rich pore structure, and nanoparticles are uniformly distributed on the stacked sheets, so that the specific surface area of the iron-manganese composite material is large, which is beneficial to removing pollutants.
Example 2
A preparation method of a porous iron-manganese composite material for efficiently fixing and removing antimony pollution comprises the following steps:
(1) respectively and accurately weighing 0.015mol of potassium permanganate, 0.010mol of manganese chloride and 0.025mol of ferric chloride, respectively adding the potassium permanganate, the 0.010mol of manganese chloride and the 0.025mol of ferric chloride into 1000mL of deionized water, and uniformly dissolving to obtain a potassium permanganate solution with the concentration of 0.015mol/L, a manganese chloride solution with the concentration of 0.010mol/L and a ferric chloride solution with the concentration of 0.025 mol/L;
(2) dripping the potassium permanganate solution into the manganese chloride solution at the dripping speed of 0.1mL/min, and then stirring for 1h to obtain a suspension;
(3) adding the ferric chloride solution into the suspension obtained in the step (2) at a dropping speed of 5.0mL/min, and stirring for 1h to obtain a mixed solution;
(4) and (3) adjusting the pH value of the mixed solution obtained in the step (3) to 7.0 by using ammonia water, aging for 6h, centrifuging at 2000rpm for 10min, removing supernatant, washing with deionized water for several times, drying at 40 ℃ for 18h, grinding and sieving with a 100-mesh sieve to obtain the porous iron-manganese composite material for efficiently and fixedly removing antimony pollution.
The morphology of the prepared porous iron-manganese composite material is shown in figure 3. As can be seen from fig. 3, the obtained fe-mn composite material also has a rich pore structure, and nanoparticles are uniformly distributed on the stacked sheets.
Example 3
A preparation method of a porous iron-manganese composite material for efficiently fixing and removing antimony pollution comprises the following steps:
(1) respectively and accurately weighing 0.090mol of potassium permanganate, 0.060mol of manganese chloride and 0.150mol of ferric chloride, respectively adding the potassium permanganate, the 0.060mol of manganese chloride and the 0.150mol of ferric chloride into 1000mL of deionized water, and dissolving the potassium permanganate, the manganese chloride and the ferric chloride uniformly to obtain a potassium permanganate solution with a concentration of 0.090mol/L, a manganese chloride solution with a concentration of 0.060mol/L and a ferric chloride solution with a concentration of 0.150 mol/L;
(2) dripping the potassium permanganate solution into the manganese chloride solution at a dripping speed of 5mL/min, and then stirring for 3h to obtain a suspension;
(3) adding the ferric chloride solution into the suspension obtained in the step (2) at a dropping speed of 10mL/min, and stirring for 3 hours to obtain a mixed solution;
(4) and (3) adjusting the pH value of the mixed solution obtained in the step (3) to 8.0 by using ammonia water, aging for 18h, centrifuging at 6000rpm for 20min, removing supernatant, washing with deionized water for several times, drying at the temperature of 80 ℃ for 36h, grinding and sieving with a 500-mesh sieve to obtain the porous iron-manganese composite material for efficiently and fixedly removing antimony pollution.
The morphology of the prepared porous iron-manganese composite material is shown in figure 4. As can be seen from fig. 4, the obtained fe-mn composite material also has a rich pore structure, and nanoparticles are uniformly distributed on the stacked sheets.
Example 4
In order to explore the relationship between the effect and the time of the prepared porous iron-manganese composite material for efficiently fixing and removing the antimony pollution in the treatment of the wastewater containing the heavy metal antimony pollution. The following tests were carried out using the Sb (III) solution and the Sb (V) solution as simulated wastewater.
The test, comprising:
accurately weighing multiple 0.005g of porous iron-manganese composite material, respectively placing in a 50mL centrifuge tube, respectively transferring 25mL of porous iron-manganese composite material with a concentration of 20 mg.L into the centrifuge tube-1Fully mixing the Sb (III) solution or the Sb (V) solution, placing the mixed solution on a water bath oscillator at the temperature of 30 +/-1 ℃ for shaking, taking the solution to pass through a 0.45-micron filter membrane when the shaking time is 1min,2.5min,5min,8min,10min,20min,30min,60min,120min,240min and 480min, and measuring the concentration of Sb (III) or Sb (V) in the solution by an atomic absorption spectrophotometer, wherein the test results are shown in a graph 5a and a graph 5 b. FIG. 5a is a graph showing the adsorption kinetics of Sb (III) by the porous iron-manganese composite material for efficiently and fixedly removing antimony pollution, and FIG. 5b is a graph showing the adsorption kinetics of Sb (III) by the porous iron-manganese composite material for efficiently removing antimony pollutionGraph of adsorption kinetics of the porous iron-manganese composite material for fixing and removing antimony pollution on Sb (V).
As can be seen from FIGS. 5a and 5b, the porous Fe-Mn composite material for efficiently and fixedly removing antimony contamination achieves the adsorption equilibrium on Sb (III) or Sb (V) within 60 minutes and 120 minutes respectively, and then the adsorption on Sb (III) or Sb (V) is not changed greatly along with the time, which shows that the porous Fe-Mn composite material can rapidly and fixedly remove Sb (III) or Sb (V), and the equilibrium adsorption amounts are 99.5 and 62.1 mg-g respectively-1.
Example 5
In order to explore the relationship between the effect of the prepared porous iron-manganese composite material for efficiently fixing and removing the antimony pollution in the treatment of the wastewater containing heavy metal antimony pollution and the concentration of the antimony in the wastewater. The following tests were carried out using the Sb (III) solution and the Sb (V) solution as simulated wastewater.
The test, comprising:
accurately weighing 0.005g of porous Fe-Mn composite material in multiple portions, respectively placing the multiple portions into 50mL of centrifuge tubes, respectively transferring 25mL of Sb (III) solution or Sb (V) solution with different initial concentrations (the initial concentration is set to be 50mg L) into the centrifuge tubes-1，100mg L-1,150mg L-1,200mg L-1,300mg L-1,400mg L-1，500mg L-1) After fully and uniformly mixing, placing on a water bath oscillator at 30 +/-1 ℃ and shaking for 24h, taking the supernatant and filtering the supernatant through a 0.45 mu m filter membrane, and measuring the concentration of Sb (III) or Sb (V) in the solution by an atomic absorption spectrophotometer. The test results are shown in fig. 6a and 6 b. FIG. 6a is a graph showing isothermal adsorption of Sb (III) by the porous Fe-Mn composite material for efficient fixed removal of Sb pollution; FIG. 6b is a graph showing isothermal adsorption of Sb (V) by the porous iron-manganese composite material for efficiently and fixedly removing antimony pollution.
As can be seen from FIGS. 6a and 6b, the maximum adsorption amounts of Sb (III) or Sb (V) of the porous Fe-Mn composite material for efficiently fixing and removing antimony contamination are 278.3 and 185.7 mg-g-1The high adsorption efficiency of the porous ferro-manganese composite material to Sb (III) or Sb (V) is demonstrated.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of a porous iron-manganese composite material for efficiently removing antimony pollution in a fixed mode is characterized by comprising the following steps:
(1) respectively preparing permanganate solution, manganese salt solution and iron salt solution from permanganate, manganese salt and iron salt;
(2) dropwise adding the permanganate solution obtained in the step (1) into a manganese salt solution, and stirring to obtain a suspension;
(3) adding an iron salt solution into the suspension obtained in the step (2), and stirring to obtain a mixed solution;
(4) and (4) adjusting the pH value of the mixed solution obtained in the step (3) to 6.5-8.5, then carrying out aging treatment, centrifuging to obtain a precipitate, washing, drying, grinding and sieving to obtain the porous iron-manganese composite material for efficiently removing antimony pollution by fixation.
2. The method for preparing the porous iron-manganese composite material for efficiently and fixedly removing antimony pollution according to claim 1, wherein the permanganate in the step (1) is more than one of potassium permanganate and sodium permanganate; the manganese salt is more than one of manganese chloride, manganese nitrate and manganese sulfate; the ferric salt is more than one of ferric nitrate, ferric sulfate and ferric chloride; the molar ratio of the permanganate to the manganese salt to the iron salt is (1.5-9): (1-6): (2.5-15).
3. The preparation method of the porous iron-manganese composite material for efficiently and fixedly removing antimony pollution according to claim 2, wherein the molar ratio of the permanganate, the manganese salt and the iron salt is (3-6): (2-4): (5-10).
4. The method for preparing the porous ferro-manganese composite material for efficiently and fixedly removing the antimony pollution according to claim 1, wherein the concentration of the permanganate solution in the step (1) is 0.015-0.090 mol/L; the concentration of the manganese salt solution is 0.010mol/L-0.060 mol/L; the concentration of the ferric salt solution is 0.025mol/L-0.150 mol/L.
5. The preparation method of the porous iron-manganese composite material for efficiently and fixedly removing antimony pollution according to claim 1, wherein the dropping rate of the permanganate solution into the manganese salt solution in the step (2) is 0.1-5 mL/min; the stirring treatment time is 1-3 h.
6. The preparation method of the porous iron-manganese composite material for efficiently and fixedly removing antimony pollution according to claim 1, wherein the adding speed of the iron salt solution in the step (3) into the suspension is 5-10ml/min, and the stirring treatment time is 1-3 h.
7. The method for preparing the porous iron-manganese composite material for efficiently and fixedly removing antimony pollution according to claim 1, wherein the aging treatment time in the step (4) is 6-18 h.
8. The method as claimed in claim 1, wherein the centrifugation speed in step (4) is 2000-6000rpm, and the centrifugation time is 10-20 min; the drying temperature is 40-80 ℃, and the drying time is 18-36 h; the size of the sieving mesh is 100-500 meshes.
9. A porous iron-manganese composite material for efficient fixed removal of antimony contamination prepared by the preparation method of any one of claims 1 to 8.
10. The use of the porous ferrimanganic composite material for efficient fixed removal of antimony pollution as claimed in claim 9 in the treatment of antimony pollution containing heavy metals.
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| PCT/CN2021/127801 WO2022160836A1 (en) | 2021-01-29 | 2021-10-31 | Porous iron-manganese composite material for efficiently fixing and removing antimony pollution, preparation method therefor and use thereof |
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| CN113877522A (en) * | 2021-10-30 | 2022-01-04 | 中冶华天工程技术有限公司 | Preparation method and application of diatomite-based adsorbent loaded with iron-manganese oxide |
| CN113976074A (en) * | 2021-11-23 | 2022-01-28 | 沈阳建筑大学 | Iron-manganese mud composite gel ball adsorption antimony removal material and preparation method thereof |
| CN114272905A (en) * | 2021-12-14 | 2022-04-05 | 南昌航空大学 | Chitosan-biological iron-manganese oxide material and preparation method and application thereof |
| CN114702961A (en) * | 2022-03-17 | 2022-07-05 | 中南大学 | Amorphous ferro-manganese colloidal material and preparation method and application thereof |
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| CN116099486A (en) * | 2022-11-16 | 2023-05-12 | 北京师范大学 | Metal-based composite adsorbent for removing antimony and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113877522A (en) * | 2021-10-30 | 2022-01-04 | 中冶华天工程技术有限公司 | Preparation method and application of diatomite-based adsorbent loaded with iron-manganese oxide |
| CN113976074A (en) * | 2021-11-23 | 2022-01-28 | 沈阳建筑大学 | Iron-manganese mud composite gel ball adsorption antimony removal material and preparation method thereof |
| CN114272905A (en) * | 2021-12-14 | 2022-04-05 | 南昌航空大学 | Chitosan-biological iron-manganese oxide material and preparation method and application thereof |
| CN114702961A (en) * | 2022-03-17 | 2022-07-05 | 中南大学 | Amorphous ferro-manganese colloidal material and preparation method and application thereof |
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| WO2022160836A1 (en) | 2022-08-04 |
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