CN111186933A - Chemical method for quickly forming sea urchin-shaped schneiderian minerals from acid mine wastewater - Google Patents
Chemical method for quickly forming sea urchin-shaped schneiderian minerals from acid mine wastewater Download PDFInfo
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Abstract
The invention discloses a chemical method for quickly forming sea urchin-shaped schwertmannite from acid mine wastewater. The invention adopts a chemical method to circularly react and regulate the formation of sea urchin-shaped Schlemn minerals: firstly filtering to remove suspended particles in the acid mine wastewater, then adding a certain amount of zero-valent iron powder for proper stirring, after recovering zero-valent iron by a magnet, adding a certain amount of hydrogen peroxide into the filtrate at a certain speed range for stirring reaction, precipitating reddish brown solid particles at the bottom, simply filtering, repeating the steps, precipitating iron ions in the acid mine wastewater to the maximum extent, washing and drying the recovered reddish brown solid, and obtaining the environment functional material with a typical sea urchin-shaped structure, namely Shi mineral. The method for recovering the valuable iron ions from the acid mine wastewater is an efficient strategy for recycling the valuable metal ions in the acid mine wastewater and reducing the wastewater pollution.
Description
Technical Field
The invention belongs to the field of environmental engineering, and relates to a chemical method for quickly forming sea urchin-shaped schlerzilian minerals from acid mine wastewater.
Background
In the process of mining mineral resources such as natural pyrite and the like, sulfide minerals contained in the mineral resources are oxidized under the action of air, water and microorganisms to generate a large amount of acidic drainage, and the mineral resources are one of the most serious environmental pollutions faced by mining industry. If the acidic mine wastewater is discharged into rivers, lakes and other water bodies, the water quality of the water bodies is acidified, the growth environment of bacteria and microorganisms is damaged, and the self-purification function of the water bodies is reduced. If discharged into the soil, the acid and a large amount of heavy metal ions can acidify and poison the soil, resulting in withering and death of vegetation. Heavy metal ions also enter the soil and can be absorbed by plants and harm human health through the food chain. A large amount of metal ions in the acid mine wastewater are abundant in iron ions, and the content of the metal ions is as high as 500-4500 mg/L. The acidic mine wastewater is directly treated, and the metal ions reduce the treatment efficiency on one hand and cause the waste of valuable metal resources on the other hand.
The method for recovering metal ions from acid mine wastewater and simultaneously obtaining environment functional materials is an effective strategy for repairing mine wastewater and realizing resource utilization. Chinese patent 201610030955.0 discloses a method for recovering iron in acid mine wastewater in the form of nano zero-valent iron, which discusses adopting liquid phase reductionThe specific implementation mode of the method is that excessive sodium borohydride is utilized to reduce iron into zero-valent iron under the protection of nitrogen, and the recovered nano zero-valent iron is an environmental functional material and can be applied to removing hexavalent chromium in water; chinese patent 201510920933.7 discloses a process for recovering valuable metals from mine wastewater by sulfate-reducing bacteria, which reduces sulfate in acidic mine wastewater to H2S, the method for forming metal sulfide by selectively precipitating different metals can effectively precipitate Cu in the acid mine wastewater in the form of sulfide2+，Zn2+，Fe2+And Fe3+Ions. Chinese invention patent 201910083782.2 discloses a process for preparing schlerian mineral from acid mine wastewater based on zero-valent iron reduction coupling microbial mineralization, which precipitates most of iron ions in the acid mine wastewater to generate schlerian mineral under the action of microorganisms, wherein the schlerian mineral is applied to the environment and can be used as an inorganic pigment, an efficient arsenic adsorbent, a Fenton-like catalyst and the like, and is a potential environment functional material.
In view of the wide application of the Schneider minerals in the environmental field, the method for recovering iron from the acid mine wastewater in the form of the Schneider minerals has certain economic and environmental benefits. The schneiderian mineral is a reddish brown iron oxysulfate mineral, widely exists in acid mine wastewater, and has a typical sea urchin-shaped structure. Can be prepared from acid mine wastewater by a chemical method and a biological method, and compared with the biological method, the chemical method has the advantages of rapid reaction, environment-friendly reagents, easy regulation and control of conditions and the like, but has the defects that the generated Schleman mineral is easy to agglomerate, the microstructure of the Schleman mineral is an oval sphere particle aggregate and does not have the traditional burr-shaped structural characteristics, and therefore, the specific surface area (4-10 m) of the Schleman mineral synthesized by the chemical method is large2Per gram) is much smaller than that of (60-100 m) prepared by biological method2/g) resulting in a great reduction in the adsorption capacity for heavy metals (e.g., As, Cr, Se, etc.) and heterogeneous fenton catalytic activity. The purity, particle size, specific surface area and active site number of the functional material are direct factors for determining the adsorption and catalytic capacity of the material, so that the conditions for preparing the Schneider minerals by a chemical method are optimized and quickly selectedThe method for obtaining the Schwerner minerals with high purity and large specific surface area from the acid mine wastewater is an efficient strategy for reducing the pollution of the acid mine wastewater and recycling valuable metal ions, and has very important practical significance for the remediation of the acid mine wastewater and the treatment of environmental pollution.
Disclosure of Invention
The invention aims to provide a method for rapidly and efficiently recovering iron ions from acid mine wastewater by a chemical method to obtain sea urchin-shaped Schlemm minerals, so that valuable metals in the mine wastewater are effectively recycled, and the discharge of pollutants and the harm of heavy metals to the ecological environment are reduced.
The purpose of the invention can be realized by the following technical scheme:
the invention discloses a chemical method for quickly forming sea urchin-shaped schwertmannite from acid mine wastewater, which is characterized by comprising the following steps of:
(1) filtering to remove suspended particles in the acid mine wastewater, and determining the concentration of iron ions in the solution;
(2) adding zero-valent iron powder into the filtered acidic wastewater, properly stirring for a period of time, and recovering the residual zero-valent iron by using a magnet; the mass of the added zero-valent iron is 0.4-0.8 time of the iron ion amount measured in the step (1); the stirring speed is 100-400rpm, and the stirring time is 30-90 min;
(3) then, adding a certain amount of hydrogen peroxide into the filtered solution at a certain speed, and continuously stirring for a period of time; wherein the molar concentration of the hydrogen peroxide is 0.7-1.2 times of the amount of iron ions in the acid mine wastewater in the step (1); the dropwise adding mode is that the materials are added in 3-6 equal parts at intervals of 0.5-1 h, the stirring speed is 200-400rpm, and the stirring time is 3-7 h;
(4) filtering and recovering the reddish brown solid, washing with deionized water and drying;
(5) repeating the steps (1) - (4) for a plurality of times, reducing the dosage of zero-valent iron and hydrogen peroxide in each treatment process, and recovering all solid materials after a plurality of reactions.
In the method, the mass of the zero-valent iron added in the step (2) is preferably 0.4-0.6 times of the mass of the iron ions measured in the step (1); the stirring speed is 100-200rpm, and the stirring time is 60-90 min; the residual zero-valent iron recovered by the magnet can be continuously used in the subsequent steps after being simply cleaned and dried.
In the step (3), the molar concentration of the hydrogen peroxide is preferably 1.0-1.2 times of the iron ion amount determined in the step (1); the dropping mode is that the materials are added in 5-6 equal parts at intervals of 1h, the stirring speed is 300-400rpm, and the stirring time is 4-7 h;
in the step (4), the drying temperature is 40-80 ℃, and the drying time is 12-24 h; the obtained reddish brown solid material is schneiderian mineral;
in the step (5), the repetition times are 3-8 times, and the addition amount of the zero-valent iron and the hydrogen peroxide in each time is reduced by 20-40% in the previous batch.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention can obtain schneiderian minerals with sea urchin-shaped structures by controlling the adding rate and proportion of hydrogen peroxide in the chemical mineralization process, and the specific surface area of the schneiderian minerals is 4-10m2Increased/g to 150-2G, more active sites are exposed.
2. The Schwerner mineral obtained by the invention and the mineral synthesized by the traditional chemical method have higher adsorption capacity to heavy metals (such As As, Cr, Se and the like), and have higher degradation rate to organic matters when being used As a Fenton-like catalyst.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
FIG. 2 is a scanning electron micrograph of a Schneider mineral obtained in example 1.
FIG. 3 is a scanning electron micrograph of a Schneider mineral obtained in example 2.
FIG. 4 is a scanning electron micrograph of a Schneider mineral obtained in example 3.
Fig. 5 is a scanning electron microscope picture of schneiderian mineral obtained in comparative example 1.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The technical scheme of the invention is further specifically described by embodiments and comparative examples in combination with the accompanying drawings.
Example 1
A chemical method for quickly forming sea urchin-shaped schneiderian minerals from acid mine wastewater comprises the following specific steps:
(1) the method comprises the steps of adopting actual acidic mine wastewater of abandoned copper ores of Jiangxi Tourling, removing suspended particles through simple filtration, and determining Fe contained in the actual acidic mine wastewater3+Is 1235 mg/L.
(2) Adding 494mg/L of zero-valent iron powder which is mixed with Fe in acid mine wastewater into the filtered solution3+The mass ratio was 0.4, and the mixture was stirred at 100rpm for 90min, and unreacted zero-valent iron was recovered with a magnet.
(3) Adding 26.5mM hydrogen peroxide into the filtrate after reaction, wherein the hydrogen peroxide is mixed with Fe in the mine wastewater3+The mixture was added at 6 portions at a molar ratio of 1.2, 4.4mM at 1 hour intervals, and stirred at 400rpm for 7 hours.
(4) The solid obtained by suction filtration was dried in a vacuum oven at 40 ℃.
(5) Repeating the steps (1) - (4) for a plurality of times, reducing the dosage of zero-valent iron and hydrogen peroxide in each treatment process, and recovering all solid materials after a plurality of reactions.
Repeating the steps (1) to (4) for 8 times, gradually reducing the dosage of the zero-valent iron and the hydrogen peroxide by 40% each time, and drying for 24 hours in a vacuum drying oven after multiple reactions. Finally, the iron concentration in the original acid mine wastewater is reduced to 170mg/L, the sulfate radical concentration is reduced to 5005mg/L from 8011mg/L, and the yield of the obtained Schneider minerals is 11.9 g/L.
Example 2
A chemical method for rapidly recovering sea urchin-shaped Schlemn minerals from acid mine wastewater comprises the following specific steps:
(1) the method comprises the steps of adopting actual acidic mine wastewater of abandoned copper ores of Jiangxi Tourling, removing suspended particles through simple filtration, and determining Fe contained in the actual acidic mine wastewater3+Is 1235 mg/L.
(2) Adding 988mg/L of zero-valent iron powder into the filtered solution, wherein the mass of the zero-valent iron powder is equal to that of Fe in the acid mine wastewater3+The mass ratio was 0.8, and the mixture was stirred at 400rpm for 30min, and unreacted zero-valent iron was recovered with a magnet.
(3) Adding 15.4mM hydrogen peroxide into the filtrate after reaction, wherein the hydrogen peroxide is mixed with Fe in the mine wastewater3+The mixture was added at a molar ratio of 0.7 in 3 portions, 5.1mM was added every 1 hour, and the mixture was stirred at 200rpm for 3 hours.
(4) The solid obtained by suction filtration is placed in a vacuum drying oven to be dried at the temperature of 80 ℃.
(5) Repeating the steps for 3 times, gradually reducing the adding amount of zero-valent iron and hydrogen peroxide by 20% each time, and drying in a vacuum drying oven for 12h after multiple reactions. Finally, the iron concentration in the original acid mine wastewater is reduced to 230mg/L, the sulfate radical concentration is reduced to 5802mg/L from 8011mg/L, and the yield of the obtained Schneider minerals is 8.2 g/L.
Example 3
A chemical method for rapidly recovering sea urchin-shaped Schlemn minerals from acid mine wastewater comprises the following specific steps:
(1) the method comprises the steps of adopting actual acidic mine wastewater of abandoned copper ores of Jiangxi Tourling, removing suspended particles through simple filtration, and determining Fe contained in the actual acidic mine wastewater3+Is 1235 mg/L.
(2) Adding 741mg/L of zero-valent iron powder which is mixed with Fe in the acid mine wastewater into the filtered solution3+The mass ratio was 0.6, and the mixture was stirred at 200rpm for 60min, and unreacted zero-valent iron was recovered with a magnet.
(3) Adding 23.1mM hydrogen peroxide into the filtrate after reaction, wherein the hydrogen peroxide is mixed with Fe in the mine wastewater3+The mixture was added at 5 portions at a molar ratio of 1.05, 4.6mM at 1 hour intervals, and stirred at 300rpm for 4 hours.
(4) The solid obtained by suction filtration is placed in a vacuum drying oven to be dried at 60 ℃.
(5) Repeating the step 3 times, gradually reducing the dosage of zero-valent iron and hydrogen peroxide by 15% each time, and drying in a vacuum drying oven for 18h after multiple reactions. Finally, the iron concentration in the original acid mine wastewater is reduced to 190mg/L, the sulfate radical concentration is reduced from 8011mg/L to 5442mg/L, and the yield of the obtained Schneider minerals is 10.2 g/L.
Comparative example 1
The traditional chemical mineralization method for forming the schlerian minerals from the acid mine wastewater comprises the following steps:
(1) the method comprises the steps of adopting actual acidic mine wastewater of abandoned copper ores of Jiangxi Tourling, removing suspended particles through simple filtration, and determining Fe contained in the actual acidic mine wastewater3+Is 1235 mg/L;
(2) adding 988mg/L of zero-valent iron powder into the filtered acidic wastewater, stirring for 4 hours at the stirring speed of 100rpm, and recovering unreacted zero-valent iron by using a magnet;
(3) then, 26.5mM hydrogen peroxide was directly added to the filtered solution, and the mixture was stirred at 400rpm for 12 hours.
(4) Filtering and recovering a reddish brown solid, cleaning with deionized water, and drying in a vacuum drying oven at 40 ℃;
(5) repeating the steps (1) - (4) for 8 times to recover all solid materials.
Finally, the iron concentration in the original acid mine wastewater is reduced to 250mg/L, the sulfate radical concentration is reduced to 6105mg/L from 8011mg/L, and the yield of the obtained Schneider minerals is 7.5 g/L.
Comparison of basic Properties of the Schneider minerals prepared in comparative example 1 and examples 1 to 3
1Adsorption conditions: the pH value is 7.0, and the addition amount of the Schwerer mineral is 0.25 g/L.
2Fenton-like experimental conditions: the concentration of phenol is 50mg/L, the concentration of hydrogen peroxide is 300mg/L, and the addition amount of Schneider minerals is 1 g/L.
Claims (6)
1. A chemical method for quickly forming sea urchin-shaped schneiderian minerals from acid mine wastewater is characterized by comprising the following steps of:
(1) filtering to remove suspended particles in the acid mine wastewater;
(2) adding zero-valent iron powder into the filtered acidic wastewater, properly stirring for a period of time, and recovering the residual zero-valent iron by using a magnet; the mass of the added zero-valent iron is 0.4-0.8 time of the iron ion amount measured in the step (1); the stirring speed is 100-400rpm, and the stirring time is 30-90 min;
(3) then, adding a certain amount of hydrogen peroxide into the filtered solution at a certain speed, and continuously stirring for a period of time; wherein the molar concentration of the hydrogen peroxide is 0.7-1.2 times of the amount of iron ions in the acid mine wastewater in the step (1); the dropwise adding mode is that the materials are added in 3-6 equal parts at intervals of 0.5-1 h, the stirring speed is 200-400rpm, and the stirring time is 3-7 h;
(4) filtering and recovering the reddish brown solid, washing with deionized water and drying;
(5) repeating the steps (1) - (4) for a plurality of times, reducing the dosage of zero-valent iron and hydrogen peroxide in each treatment process, and recovering all solid materials after a plurality of reactions.
2. The chemical process according to claim 1, wherein the amount of zero-valent iron added in step (2) is 0.4 to 0.6 times the amount of iron ions measured in step (1); the stirring speed is 100-200rpm, and the stirring time is 60-90 min.
3. The chemical method as claimed in claim 1, wherein the residual zero-valent iron recovered from the magnet in the step (2) is simply washed and dried, and then is used in the subsequent step.
4. The chemical method as claimed in claim 1, wherein the molar concentration of hydrogen peroxide added in the step (3) is 1.0 to 1.2 times of the amount of iron ions measured in the step (1); the dropping method is that the materials are added in 5-6 equal parts at intervals of 1h, the stirring speed is 300-400rpm, and the stirring time is 4-7 h.
5. The chemical process according to claim 1, wherein in the step (4), the drying temperature is 40-80 ℃, and the drying time is 12-24 h; the obtained reddish brown solid material is schwertmannite.
6. The chemical method as claimed in claim 1, wherein in the step (5), the repetition frequency is 3-8 times, and the addition amount of the zero-valent iron in each time is reduced by 20-40% compared with the addition amount of the hydrogen peroxide in the previous batch.
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Cited By (7)
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| CN112279466A (en) * | 2020-10-28 | 2021-01-29 | 山西农业大学 | Method for treating acid mine wastewater by combining chemistry and microorganisms |
| CN112795604A (en) * | 2020-12-25 | 2021-05-14 | 南京农业大学 | Method for preparing sulfated polysaccharide from acidic mine wastewater |
| CN113385138A (en) * | 2021-06-21 | 2021-09-14 | 南京贝克特环保科技有限公司 | Preparation method and application of Schneider mineral |
| CN114471452A (en) * | 2022-03-04 | 2022-05-13 | 太原碧蓝水利工程设计股份有限公司 | Method for rapidly treating acidic mine water and adsorbent prepared from acidic mine water |
| CN114634257A (en) * | 2022-03-04 | 2022-06-17 | 太原碧蓝水利工程设计股份有限公司 | Method for treating acidic mine water and hydroxyl potassium ferric sulfate synthesized by acidic mine water |
| CN114790010A (en) * | 2022-04-28 | 2022-07-26 | 中国地质大学（北京） | Reduced schlerren mineral, preparation method thereof and application thereof in chromium-contaminated soil |
| CN114804216A (en) * | 2022-04-28 | 2022-07-29 | 中国地质大学（北京） | Shi mineral for removing hexavalent chromium pollution in wastewater and preparation method thereof |
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| CN112279466A (en) * | 2020-10-28 | 2021-01-29 | 山西农业大学 | Method for treating acid mine wastewater by combining chemistry and microorganisms |
| CN112795604A (en) * | 2020-12-25 | 2021-05-14 | 南京农业大学 | Method for preparing sulfated polysaccharide from acidic mine wastewater |
| CN112795604B (en) * | 2020-12-25 | 2024-04-19 | 南京农业大学 | Method for preparing sulfated polysaccharide by using acid mine wastewater |
| CN113385138A (en) * | 2021-06-21 | 2021-09-14 | 南京贝克特环保科技有限公司 | Preparation method and application of Schneider mineral |
| CN114471452A (en) * | 2022-03-04 | 2022-05-13 | 太原碧蓝水利工程设计股份有限公司 | Method for rapidly treating acidic mine water and adsorbent prepared from acidic mine water |
| CN114634257A (en) * | 2022-03-04 | 2022-06-17 | 太原碧蓝水利工程设计股份有限公司 | Method for treating acidic mine water and hydroxyl potassium ferric sulfate synthesized by acidic mine water |
| CN114471452B (en) * | 2022-03-04 | 2023-09-08 | 太原碧蓝水利工程设计股份有限公司 | Method for rapidly treating acidic mine pit water and adsorbent prepared from acidic mine pit water |
| CN114790010A (en) * | 2022-04-28 | 2022-07-26 | 中国地质大学（北京） | Reduced schlerren mineral, preparation method thereof and application thereof in chromium-contaminated soil |
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Application publication date: 20200522 |