CN112479218A - Recycling and harmless treatment method for tailings - Google Patents
Recycling and harmless treatment method for tailings Download PDFInfo
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- CN112479218A CN112479218A CN202011431485.1A CN202011431485A CN112479218A CN 112479218 A CN112479218 A CN 112479218A CN 202011431485 A CN202011431485 A CN 202011431485A CN 112479218 A CN112479218 A CN 112479218A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
- C04B28/26—Silicates of the alkali metals
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/02—Selection of the hardening environment
- C04B40/0263—Hardening promoted by a rise in temperature
- C04B40/0268—Heating up to sintering temperatures
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00767—Uses not provided for elsewhere in C04B2111/00 for waste stabilisation purposes
- C04B2111/00784—Uses not provided for elsewhere in C04B2111/00 for waste stabilisation purposes for disposal only
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a recycling and harmless treatment method of tailings, which comprises the steps of placing the tailings, sodium-containing alkaline compounds and water media in a sealed reaction kettle for hydrothermal reaction, carrying out solid-liquid separation on hydrothermal reaction products, concentrating obtained liquid phase to obtain sodium silicate products, and carrying out high-temperature treatment on obtained solid phase to realize heavy metal stabilization.
Description
Technical Field
The invention relates to a tailing disposal method, in particular to a method for recycling silicate resources in heavy metal-containing siliceous tailings and harmlessly treating heavy metals, and belongs to the technical field of comprehensive utilization of mining and metallurgy solid waste resources and environmental remediation.
Background
In China, a plurality of mine enterprises exist, and more than half of tailings are silica-alumina tailings. Most of the silico-aluminous tailings are stored in a tailing pond for a long time due to limited secondary resource utilization ways, and have fine granularity, complex components and more or less heavy metal elements, so that the secondary resource utilization ways have great threats to the surrounding ecological environment, and the secondary resource utilization ways are always the key points of government and various enterprises. Therefore, the method has great practical significance in resource utilization and harmless disposal of the tailings.
Sodium silicate is used as one of basic raw materials for industrial production, the production raw materials mainly comprise sodium salt and quartz, and the principle of the production is that sodium silicate is generated by the reaction of element sodium and silicon oxide under the high-temperature condition. However, if the silica-alumina tailings contain a large amount of silicon oxides, if quartz can be replaced by the silica-alumina tailings to produce sodium silicate, the raw material sources can be expanded to a certain extent, and the silica-alumina tailings are recycled to achieve effective treatment of recycling and reduction of the tailings, but the tailings have complex components and contain heavy metals, so that no good related method for preparing the sodium silicate by replacing industrial sodium salts, quartz and the like with the tailings is found at present, and therefore, the development of a method for preparing the sodium silicate by using the tailings has important significance for improving the mine environment and recycling the tailings resources.
Disclosure of Invention
Based on the defects of limited raw materials for synthesizing sodium silicate and limited consumption ways of the alumino-silicate tailings in the prior art, the invention aims to provide the method for preparing the high-purity sodium silicate by using the alumino-silicate tailings containing heavy metals as the raw materials and realizing the stabilization treatment of the heavy metals.
In order to realize the technical purpose, the invention provides a recycling and harmless treatment method of tailings, which comprises the steps of placing the tailings, a sodium-containing alkaline compound and a water medium into a sealed reaction kettle for hydrothermal reaction, carrying out solid-liquid separation on a hydrothermal reaction product, concentrating an obtained liquid phase to obtain a sodium silicate product, and carrying out high-temperature treatment on an obtained solid phase to realize heavy metal stabilization.
According to the invention, the tailing raw material is subjected to hydrothermal reaction under an alkaline condition, silicon element in the tailing is converted into sodium silicate, the temperature condition of generating the sodium silicate by a high-temperature solid phase can be effectively reduced under the high-pressure condition of the hydrothermal reaction, the reaction selectivity is higher, the sodium silicate enters the reaction solution with higher selectivity, so that the raw material for producing the sodium silicate is expanded, and the slag phase obtained by the hydrothermal reaction mainly comprises heavy metal enriched slag and a certain amount of components such as sodium silicate and sodium aluminate, can be effectively solidified and stabilized under the high-temperature condition, and is subjected to stabilization treatment on non-silicon aluminum elements in the tailing, so that the harmless and recycling properties of the tailing are effectively realized.
In the prior art, generally, the tailings need higher temperature (more than 400 ℃) in the normal-pressure high-temperature activation process, but the technical scheme of the invention utilizes the high-temperature high-pressure process of the hydrothermal reaction, so that the reaction activation energy can be effectively reduced, the low-temperature activation of the tailings can be realized, and the activation reaction of the tailings can be realized at the temperature of 100-250 ℃.
As a preferred embodiment, the tailings are siliceous tailings, wherein the silicon content is not less than 30%, and the silicon content is measured by silicon dioxide.
As a preferable scheme, the tailings are subjected to grinding pretreatment, and the particle size of the tailings is smaller than 400 meshes.
As a preferred embodiment, the sodium-containing basic compound is sodium hydroxide and/or sodium carbonate. The sodium-containing alkaline compound is mainly used for the conversion of silicon to form water-soluble silicate.
Preferably, the mass ratio of the tailings, the sodium-containing alkaline compound and the water is 1: 0.6-4: 5-50. The mass ratio of the tailings to the sodium-containing alkaline compound is preferably 1: 1-3. If the proportion of the sodium-containing alkaline compound is too low, the extraction efficiency of silicon is reduced, and if the proportion of the sodium-containing alkaline compound is too high, the purity of the extracted silicon is affected, and the high-purity sodium silicate product is not obtained.
As a preferred embodiment, the hydrothermal reaction conditions are: reacting for 1-6 hours at the temperature of 100-250 ℃. The hydrothermal reaction process can improve the efficiency of the hydrothermal reaction by increasing stirring. The conversion and extraction efficiency of silicon can be improved under the preferred hydrothermal reaction conditions. The preferable hydrothermal reaction temperature is 150-230 ℃. If the hydrothermal reaction temperature is low, the conversion of silicon is low, and if the reaction temperature is too high, the purity of the obtained product is insufficient and a large amount of impurities are contained.
As a preferable scheme, the high-temperature treatment temperature is 600-1000 ℃ and the time is 1-4 hours. Under the high temperature condition, the heavy metal and impurity components in the tailings can be stabilized by utilizing the gelling effect of the sodium silicate and the sodium aluminate, and the environmental pollution caused by leaching under the natural condition is prevented. The optimal high-temperature treatment temperature is 600-700 ℃, a glass phase is difficult to form at a low temperature, effective fixation of heavy metals cannot be realized, and the fixation effect of the heavy metals at a high temperature is not remarkably improved, so that the energy consumption is overlarge.
As a preferable scheme, when the hydrothermal reaction product is subjected to solid-liquid separation, a method combining filtration and centrifugal separation is adopted.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
1) the method for producing the sodium silicate takes the silica-alumina tailings as the raw material, and can convert siliceous components in the tailings into the sodium silicate through lower temperature, thereby effectively realizing the feasibility of preparing the sodium silicate by using the industrial tailings, effectively enlarging the range of the raw materials for producing the sodium silicate and having obvious advantages compared with the prior production technology.
2) The residue left after the production of the sodium silicate, which contains a certain amount of components of the sodium silicate and the sodium aluminate, can effectively solidify and stabilize the heavy metal components in the tailings at high temperature, so the production has little pollution to the environment.
Detailed Description
The following specific examples are intended to further illustrate the present disclosure, but not to limit the scope of the claims.
Example 1
In this embodiment, the tailings of mineral separation in a tin ore field of a municipality of Guangxi province are collected as raw materials, and the chemical compositions of the tailings of mineral separation are shown in table 1:
TABLE 1 tailings chemistry and content of mineral processing
| Chemical composition | SiO2 | Al2O3 | FeO | CaO | MgO | As2O3 | PbO | Others |
| Content/wt. -%) | 65.12 | 4.57 | 10.03 | 5.65 | 3.21 | 1.04 | 0.25 | 10.13 |
And grinding the tailings in the table 1, and collecting the tailings with the granularity of less than 200 meshes. According to the grinding tailings: sodium hydroxide: distilled water 1: 1.5: 30 mass ratio in a 1L reaction kettle, and heating for 4 hours at a constant temperature under the condition of stirring at 180 ℃; after the reaction is finished, filtering the reaction solution through a mesoporous filter cloth, centrifuging the reaction solution through a centrifuge, collecting supernatant, and collecting filter residues and centrifugal residues; concentrating the supernatant to obtain solid sodium silicate product, and treating the filter residue and the centrifugal slag at 600 deg.C in air atmosphere to obtain block-shaped stabilizer to stabilize heavy metal.
The detection proves that the yield of the obtained solid sodium silicate product reaches 65.3 percent, and the quality of the product meets the first-class standard of industrial solid sodium silicate in the table 2 of Industrial sodium silicate (GB/T4209-2008). The leaching concentration of heavy metals As and Pb in the filter residue and the centrifugal residue after the high-temperature treatment at 600 ℃ meets the II-class limit value of the underground water environment quality standard (GB/T14848-93).
Example 2
In this embodiment, the tailings of mineral separation in a tin ore field of a municipality of Guangxi province are collected as raw materials, and the chemical compositions of the tailings of mineral separation are shown in table 1:
TABLE 1 tailings chemistry and content of mineral processing
| Chemical composition | SiO2 | Al2O3 | FeO | CaO | MgO | As2O3 | PbO | Others |
| Content/wt. -%) | 65.12 | 4.57 | 10.03 | 5.65 | 3.21 | 1.04 | 0.25 | 10.13 |
And grinding the tailings in the table 1, and collecting the tailings with the granularity of less than 200 meshes. According to the grinding tailings: sodium hydroxide: distilled water 1: 2: 20 is evenly mixed in a 1L reaction kettle in a mass ratio, and is heated for 2 hours at a constant temperature under the stirring condition of 230 ℃; after the reaction is finished, filtering the reaction solution through a mesoporous filter cloth, centrifuging the reaction solution through a centrifuge, collecting supernatant, and collecting filter residues and centrifugal residues; concentrating the supernatant to obtain solid sodium silicate product, and treating the filter residue and the centrifugal slag at 700 deg.C in air atmosphere to obtain block-shaped stabilizer to stabilize heavy metal.
The detection shows that the yield of the obtained solid sodium silicate product is 56.5 percent, and the quality of the product meets the first-class standard of industrial solid sodium silicate in the table 2 of Industrial sodium silicate (GB/T4209-2008). The leaching concentration of heavy metals As and Pb in the filter residue and the centrifugal residue after high-temperature treatment at 700 ℃ meets the II-class limit value of the underground water environment quality standard (GB/T14848-93).
The foregoing embodiments and description have been presented only to illustrate the principles and preferred embodiments of the invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention as hereinafter claimed.
Claims (7)
1. A method for recycling and harmlessly treating tailings is characterized by comprising the following steps: placing the tailings, sodium-containing alkaline compounds and water media in a sealed reaction kettle for hydrothermal reaction, carrying out solid-liquid separation on a hydrothermal reaction product, concentrating an obtained liquid phase to obtain a sodium silicate product, and carrying out high-temperature treatment on the obtained solid phase to realize heavy metal stabilization.
2. The method for recycling and harmlessly treating tailings according to claim 1, wherein the method comprises the following steps: the tailings are siliceous tailings, wherein the silicon content is not less than 30 percent, and the silicon content is measured by silicon dioxide.
3. The method for recycling and harmlessly treating tailings according to claim 1 or 2, wherein the method comprises the following steps: and the tailings are subjected to grinding pretreatment, and the granularity of the tailings is smaller than 400 meshes.
4. The method for recycling and harmlessly treating tailings according to claim 1, wherein the method comprises the following steps: the sodium-containing alkaline compound is sodium hydroxide and/or sodium carbonate.
5. The method for recycling and harmlessly treating tailings according to claim 1, 2 or 4, wherein the method comprises the following steps: the mass ratio of the tailings, the sodium-containing alkaline compound and the water is 1: 0.6-4: 5-50.
6. The method for recycling and harmlessly treating tailings according to claim 1, wherein the method comprises the following steps: the hydrothermal reaction conditions are as follows: reacting for 1-6 hours at the temperature of 100-250 ℃.
7. The method for recycling and harmlessly treating tailings according to claim 1, wherein the method comprises the following steps: the high-temperature treatment is carried out at the temperature of 600-1000 ℃ for 1-4 hours.
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| CN202011431485.1A CN112479218A (en) | 2020-12-10 | 2020-12-10 | Recycling and harmless treatment method for tailings |
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| CN202011431485.1A CN112479218A (en) | 2020-12-10 | 2020-12-10 | Recycling and harmless treatment method for tailings |
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| CN112479218A true CN112479218A (en) | 2021-03-12 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116283436A (en) * | 2023-01-31 | 2023-06-23 | 中国地质科学院 | Method for preparing silicon-calcium-potassium-magnesium fertilizer from tailings, silicon-calcium-potassium-magnesium fertilizer and its application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104229896A (en) * | 2014-09-15 | 2014-12-24 | 中国科学院过程工程研究所 | Alkaline leaching silicon removal method of manganese ore |
| CN110272054A (en) * | 2019-08-08 | 2019-09-24 | 龙岩高岭土股份有限公司 | A method of sodium metasilicate is extracted from Kaolin Tailings with low temperature middle-pressure process |
| CN111530895A (en) * | 2020-05-19 | 2020-08-14 | 宁夏大学 | Method for high-stability solidification of arsenic slag and tailing slag |
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2020
- 2020-12-10 CN CN202011431485.1A patent/CN112479218A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104229896A (en) * | 2014-09-15 | 2014-12-24 | 中国科学院过程工程研究所 | Alkaline leaching silicon removal method of manganese ore |
| CN110272054A (en) * | 2019-08-08 | 2019-09-24 | 龙岩高岭土股份有限公司 | A method of sodium metasilicate is extracted from Kaolin Tailings with low temperature middle-pressure process |
| CN111530895A (en) * | 2020-05-19 | 2020-08-14 | 宁夏大学 | Method for high-stability solidification of arsenic slag and tailing slag |
Non-Patent Citations (1)
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| 佚名: ""以尾矿合成偏硅酸钠及其脱色的实验研究"", 《豆丁网》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116283436A (en) * | 2023-01-31 | 2023-06-23 | 中国地质科学院 | Method for preparing silicon-calcium-potassium-magnesium fertilizer from tailings, silicon-calcium-potassium-magnesium fertilizer and its application |
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