CN114524441A - Treatment method of serpentine and asbestos tailings - Google Patents
Treatment method of serpentine and asbestos tailings Download PDFInfo
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- CN114524441A CN114524441A CN202210086501.0A CN202210086501A CN114524441A CN 114524441 A CN114524441 A CN 114524441A CN 202210086501 A CN202210086501 A CN 202210086501A CN 114524441 A CN114524441 A CN 114524441A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention belongs to the technical field of hydrometallurgy, and particularly relates to a serpentine treatment method. Furthermore, the invention relates to a method for recovering serpentine from serpentine containing materials such as asbestos tailings using said treatment method. The method can realize effective separation of silicon and magnesium in the serpentine and can convert magnesium and silicon elements into products with economic value. In addition, the method has the advantages of short flow, low cost and high efficiency, and is beneficial to industrial use.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a serpentine and a method for treating serpentine-containing materials such as asbestos tailings.
Background
The asbestos tailings are mineral residues generated in asbestos beneficiation, and mainly comprise serpentine and a small amount of magnetite. The amount of asbestos tailings stored in China reaches billions of tons, and the accumulation of a large amount of tailings pollutes the environment and occupies a large amount of land on one hand, and causes resource waste on the other hand. The problem of recycling asbestos tailings is solved, and the method is an urgent and serious task. The main mineral component of the tailings, namely serpentine, is analyzed, and the molecular formula of the serpentine can be obtained: mg (magnesium)6[Si4O10](OH)8. As can be seen from the molecular formula, although the tailings are waste, the tailings have high contents of two high-value elements of magnesium and silicon, and have great economic development potential. The reasonable technological process of comprehensive utilization of asbestos tailing is designed to produce high value-added product containing Si and Mg, and has important significance in treating pollution of asbestos tailing and creating new economic value.
As a result, much work has been done by many researchers and researchers. Hanqing and the like (sodium silicate is prepared by using asbestos tailings and the performance research thereof [ J ]. Shandong chemical industry, 2021,50(9):3.) select sodium hydroxide as an active agent, mix with pretreated and ground asbestos tailings, and then heat at 600 ℃ to obtain an active roasting product of sodium silicate-containing water glass. It can be known from the analysis part of the paper that the method may have problems of poor product purity and excessively wide particle size distribution in industrial mass production, and furthermore, the paper does not propose a scheme for development and utilization of magnesium element. The method comprises the steps of developing sulfuric acid leaching liquor of asbestos tailings by using the Huzhuyen and the like (extracting magnesium from serpentine acid leaching filtrate to prepare acicular nano magnesium hydroxide [ J ]. nonmetal ore 2005,28(1):3.), refining the acid leaching liquor to remove impurity elements in the acid leaching liquor to obtain purified magnesium sulfate, then adopting a constant-temperature water bath magnesium sulfate solution, and then dropwise adding ammonia water to generate nano magnesium hydroxide to obtain magnesium hydroxide fibers with the average particle size of 15 nm. The key point of the method is to slowly drop ammonia water and control the crystal grains of the magnesium hydroxide not to grow rapidly. Although the method can be realized in a laboratory, the method has low efficiency in industrial production and is not suitable for large-scale production and preparation. Yangjiru (the research on the preparation of magnesium chloride hexahydrate and light magnesium oxide from serpentine [ D ]. the university of compost industry, 2008.) selects hydrochloric acid to leach serpentine to obtain magnesium sulfate hexahydrate, and uses the magnesium sulfate hexahydrate as a raw material to prepare light magnesium oxide. The paper focuses on the process parameters for preparing light magnesium oxide. Although the method has certain feasibility, the process flow is long, the acid leaching residue containing silicon is not effectively utilized, the overall cost is high, and the economic efficiency is not obvious.
Disclosure of Invention
The first purpose of the invention is to provide a serpentine treatment method, which aims to realize the separation of magnesium and silicon and obtain high-value silicon products and magnesium products.
The second purpose of the invention is to provide a method for treating serpentine-containing materials such as asbestos tailings.
Serpentine has the formula Mg6[Si4O10](OH)8In order to solve the technical problem, the invention provides the following technical scheme:
a method for treating serpentine comprises freezing and activating serpentine under negative pressure, performing alkaline leaching, and performing solid-liquid separation to obtain silicon leachate and magnesium oxide.
The research of the invention finds that the serpentine is subjected to freezing activation under negative pressure, the microstructure and the phase of the modifier can be obviously activated, the subsequent alkaline leaching treatment effect can be effectively improved, the alkaline leaching selectivity of silicon and magnesium is obviously improved, and a high-quality silicon product and a high-activity nano magnesium oxide product can be obtained.
In the invention, the freezing activation treatment under the negative pressure is further combined with alkaline leaching, so that the high-selectivity separation of silicon and magnesium in serpentine can be realized, the alkaline leaching rate of silicon can be improved, and high-quality magnesium oxide can be obtained. The research also finds that the control of the temperature and the negative pressure in the freezing and activating stage is beneficial to further and synergistically improving the subsequent alkaline leaching separation selectivity of silicon and magnesium and is beneficial to constructing the active structure of the prepared magnesium oxide.
Preferably, the temperature of freezing activation is less than or equal to-100 ℃; more preferably from-130 ℃ to-100 ℃.
Preferably, the pressure of the freezing activation process is less than or equal to 1 Pa; preferably 0.1 to 0.8 Pa.
Preferably, the freeze activation stage is operated continuously by evacuating air from the system at an evacuation rate of 20 to 100L/s.
In the present invention, the time of freeze activation can be adjusted as necessary, for example, the time of freeze activation is 2 to 5 hours.
The alkali liquor in the alkaline leaching stage is an aqueous solution of alkali metal hydroxide; for example, at least one of sodium hydroxide and potassium hydroxide.
Preferably, the concentration of the alkali liquor is 20-40%;
preferably, the liquid-solid ratio in the alkaline leaching stage is 10-20: 1;
preferably, the temperature of the alkaline leaching stage is 100-;
preferably, the alkaline leaching time is 1-3 h.
In the present invention, after the alkaline leaching treatment, solid-liquid separation can be performed based on a conventional method. For example, the solid-liquid separation method is centrifugation.
In the invention, metasilicate leachate can be obtained through solid-liquid separation treatment; magnesium oxide with properties can also be obtained.
Preferably, the magnesium oxide is nano-active magnesium oxide; the preferred specific surface area is greater than or equal to 100m 2/g.
The invention also provides a method for treating the serpentine-containing material, and the serpentine in the serpentine-containing material is recovered by adopting the method for treating the serpentine.
In the invention, the serpentine-containing material can be serpentine-containing minerals, solid wastes and the like.
The invention relates to a specific scheme, in particular to a treatment method of asbestos tailings containing serpentine.
In the invention, the content of the components of the asbestos tailings is not particularly required, for example, the content of magnetite in the asbestos tailings can be 2-10 wt%; in addition, less than 5 wt.% of other types of minerals (such as magnesite) are allowed to be present, the balance being serpentine.
In the present invention, the demagnetization process can be performed based on the existing means, for example, the demagnetization process comprises the following steps:
ball-milling asbestos tailings, screening to obtain fine tailing powder, and treating the fine tailing powder in a dry-method electromagnetic powder iron remover with magnetic induction intensity of 10000-20000 gausses; and recovering to obtain the demagnetizing material.
The invention discloses a preferable treatment method of asbestos tailings, which comprises the following specific operation steps:
(1) placing asbestos tailings (tailings for short) into a three-dimensional vibration ball mill for ball milling at the rotation speed of 200-500r/min for 1-5h, then sieving with a 200-500-mesh sieve, and taking out the sieved fine tailings powder.
(2) And (3) putting the fine tailing powder into a dry-method electromagnetic powder iron remover for treatment, wherein the magnetic induction intensity of the iron remover is 10000-20000 gausses. And repeatedly carrying out multiple times of treatment to obtain demagnetized tailing powder.
(3) Putting the demagnetized tailing powder into negative pressure refrigeration equipment, wherein the temperature of a cold trap is as follows: the negative pressure is less than or equal to 1Pa at the temperature of less than or equal to-100 ℃, and the air extraction rate is 20-100L/s.
(4) Adding the frozen and activated tailing powder into a sodium hydroxide solution for alkaline leaching, wherein the concentration of sodium hydroxide is 20-40%, the liquid-solid ratio is 10-20:1, the temperature is 100-. And after the alkaline leaching is finished, performing solid-liquid separation by centrifugation to obtain a solution of sodium metasilicate, and washing the obtained solid with deionized water to obtain the nano active magnesium oxide.
According to the preferred embodiment of the invention, the silicon oxide in the tailings can be simply converted into the sodium metasilicate solution. The magnesium oxide is converted into nano magnesium oxide particles with high activity and large specific surface area along with the removal of the silicon oxide.
Has the advantages that:
1. the serpentine is innovatively subjected to negative pressure freezing activation, and is further matched with an alkaline leaching treatment process, so that the silicon and magnesium in the serpentine can be conveniently and efficiently separated, the leaching rate of silicon is improved, and the nanoscale magnesium oxide with high specific surface area can be obtained.
2. In the invention, the serpentine treatment process is adopted, so that the high-efficiency treatment of serpentine-containing materials such as asbestos tailings can be effectively realized.
The process can convert the magnesium oxide into a nano sheet-like shape, and the nano magnesium oxide has large specific surface area and strong activity and can be used in high-added-value fields such as antibacterial agents, adsorbents and the like. In addition, metasilicates obtained by alkaline leaching, such as sodium metasilicate, can be used in the fields of washing aids and the like. In a word, the patent adopts a scheme of comprehensively utilizing asbestos tailings, converts silicon and magnesium elements in the asbestos tailings into products with economic values, has short preparation flow, high efficiency and low cost, and is suitable for large-scale industrial application.
Detailed Description
The present invention will be described in detail with reference to examples, but the present invention is not limited thereto.
The tailings used in the examples and the comparative examples are all asbestos tailings in Xinjiang, and the main mineral components and compositions are as follows: 92.3% serpentine, 5.8% magnetite and small amounts of magnesite and other minerals.
In the following cases, the solutions in the alkaline leaching process are all aqueous solutions of alkali, and the liquid-solid ratio in the alkaline leaching stage is the liquid volume (mL) and the solid weight ratio (g).
Example 1
(1) Placing asbestos tailings (tailings for short) into a three-dimensional vibration ball mill for ball milling at a rotating speed of 250r/min for 2 hours, then sieving through a 250-mesh sieve, and taking out fine tailings powder below the sieve.
(2) And (3) putting the fine tailing powder into a dry-method electromagnetic powder iron remover for treatment, wherein the magnetic induction intensity of the iron remover is 15000 gauss. And repeating the treatment for 3 times to obtain demagnetized tailing powder.
(3) And (4) putting the demagnetized tailing powder into negative pressure refrigeration equipment, wherein the temperature of a cold trap is-100 ℃, the negative pressure reaches 0.8Pa, and the air extraction rate is 80L/s. And obtaining the freeze activated tailing powder after treatment.
(4) And adding the frozen and activated tailing powder into a sodium hydroxide solution for alkaline leaching, wherein the mass fraction of sodium hydroxide is 35%, the liquid-solid ratio is 18:1, the temperature is 120 ℃, and the time is 2.5 hours. And after the alkaline leaching is finished, performing solid-liquid separation by adopting centrifugation to obtain a solution of sodium metasilicate, and washing the obtained solid for 3 times by using deionized water to obtain the nano active magnesium oxide.
(5) And testing the quality of silicon in the sodium metasilicate and the quality of silicon in the frozen and activated tailing powder, and taking the ratio of the two qualities as the leaching rate of the silicon. In addition, the specific surface area of the obtained magnesium oxide was tested to characterize its activity.
Example 2
(1) Placing asbestos tailings (tailings for short) into a three-dimensional vibration ball mill for ball milling at the rotating speed of 350r/min for 1.5h, then sieving by a 300-mesh sieve, and taking out the sieved fine tailings powder.
(2) And (3) putting the fine tailings powder into a dry-method electromagnetic powder iron remover for treatment, wherein the magnetic induction intensity of the iron remover is 17000 Gauss. And repeating the treatment for 3 times to obtain the demagnetized tailing powder.
(3) And (3) putting the demagnetized tailing powder into negative pressure refrigeration equipment, wherein the temperature of a cold trap is-110 ℃, the negative pressure reaches 0.5Pa, and the air extraction rate is 60L/s. And obtaining the freeze activated tailing powder after treatment.
(4) Adding the frozen and activated tailing powder into a sodium hydroxide solution for alkaline leaching, wherein the mass fraction of sodium hydroxide is 30%, the liquid-solid ratio is 15:1, the temperature is 160 ℃, and the time is 2 hours. And after the alkaline leaching is finished, performing solid-liquid separation by adopting centrifugation to obtain a solution of sodium metasilicate, and washing the obtained solid for 3 times by using deionized water to obtain the nano active magnesium oxide.
(5) And testing the quality of silicon in the sodium metasilicate and the quality of the silicon in the frozen and activated tailing powder, and taking the ratio of the two qualities as the leaching rate of the silicon. In addition, the specific surface area of the obtained magnesium oxide was tested to characterize its activity.
Example 3
(1) Placing asbestos tailings (tailings for short) into a three-dimensional vibration ball mill for ball milling at a rotating speed of 400r/min for 1.5h, then sieving with a 400-mesh sieve, and taking out sieved tailing fine powder.
(2) And (3) putting the fine tailing powder into a dry-method electromagnetic powder iron remover for treatment, wherein the magnetic induction intensity of the iron remover is 19000 gauss. And repeating the treatment for 3 times to obtain demagnetized tailing powder.
(3) And (4) putting the demagnetized tailing powder into negative pressure refrigeration equipment, wherein the temperature of a cold trap is-130 ℃, the negative pressure reaches 0.1Pa, and the air extraction rate is 40L/s. And obtaining the freeze activated tailing powder after treatment.
(4) Adding the frozen and activated tailing powder into a sodium hydroxide solution for alkaline leaching, wherein the mass fraction of sodium hydroxide is 20%, the liquid-solid ratio is 12:1, the temperature is 180 ℃, and the time is 1.5 h. And after the alkaline leaching is finished, performing solid-liquid separation by adopting centrifugation to obtain a solution of sodium metasilicate, and washing the obtained solid for 3 times by using deionized water to obtain the nano active magnesium oxide.
(5) And testing the quality of silicon in the sodium metasilicate and the quality of silicon in the frozen and activated tailing powder, and taking the ratio of the two qualities as the leaching rate of the silicon. In addition, the specific surface area of the obtained magnesium oxide was tested to characterize its activity.
Comparative example 1
The only difference compared to example 1 is that the treatment step of negative pressure freeze activation was not performed, and the alkaline leaching under the conditions described above was performed directly.
Comparative example 2
The only difference compared to example 1 is that the freezing process was carried out at atmospheric pressure.
Table 1: test results of examples and comparative examples
| Material | Leaching rate of silicon% | Specific surface area of magnesium oxide m2/g |
| Example 1 | 92.3 | 154 |
| Example 2 | 93.1 | 158 |
| Example 3 | 93.5 | 169 |
| Comparative example 1 | 33.7 | 25 |
| Comparative example 2 | 38.2 | 29 |
In conclusion, the material constructed by the method has higher silicon leaching rate, and the obtained magnesium oxide has larger specific surface area and activity.
Claims (10)
1. A serpentine treatment method is characterized in that serpentine is subjected to freezing activation under negative pressure, then alkaline leaching treatment is carried out, and solid-liquid separation is carried out to obtain silicon leachate and magnesium oxide.
2. The method of claim 1, wherein the temperature of freeze activation is ≦ -100 ℃; more preferably from-130 ℃ to-100 ℃.
3. The method of claim 1, wherein the pressure of the freeze activation process is 1Pa or less; preferably 0.1 to 0.8 Pa.
4. A serpentine treatment process according to claim 1, wherein the freeze activation stage is operated to continuously evacuate air from the system at a rate of 20 to 100L/s.
5. The method of claim 1, wherein the freeze activation time is 2 to 5 hours.
6. The method for treating serpentine according to claim 1, wherein the alkali in the alkaline leaching stage is an aqueous solution of an alkali metal hydroxide;
preferably, the concentration of the alkali liquor is 20-40%;
preferably, the liquid-solid ratio in the alkaline leaching stage is 10-20: 1;
preferably, the temperature of the alkaline leaching stage is 100-;
preferably, the alkaline leaching time is 1-3 h.
7. A method of treating serpentine according to any one of claims 1 to 6, wherein the solid-liquid separation is centrifugation;
preferably, the magnesium oxide is nano-active magnesium oxide; the preferred specific surface area is greater than or equal to 100m 2/g.
8. A method for treating a serpentine-containing material, characterized in that serpentine is recovered by the method according to any one of claims 1 to 7.
9. The treatment method according to claim 8, wherein the asbestos tailings are subjected to demagnetization treatment, and then the demagnetization material is treated by the treatment method according to any one of claims 1 to 7 to obtain leachate enriched with silicon and magnesium slag.
10. The process of claim 9, wherein the demagnetizing step comprises:
ball-milling asbestos tailings, screening to obtain fine tailing powder, and treating the fine tailing powder in a dry-method electromagnetic powder iron remover with magnetic induction intensity of 10000-20000 gausses; and recovering to obtain the demagnetizing material.
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