CN111057869A - Leaching process of magnesium ions in serpentine - Google Patents
Leaching process of magnesium ions in serpentine Download PDFInfo
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- CN111057869A CN111057869A CN201911069802.7A CN201911069802A CN111057869A CN 111057869 A CN111057869 A CN 111057869A CN 201911069802 A CN201911069802 A CN 201911069802A CN 111057869 A CN111057869 A CN 111057869A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
- C22B26/22—Obtaining magnesium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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Abstract
A leaching process of magnesium ions in serpentine comprises the following steps: mixing serpentine and a leaching agent, carrying out normal-pressure water bath reaction at the stirring speed of 200-600 r/min, adding fluorite mineral powder serving as a leaching aid while stirring for 1-3 min, continuously reacting and leaching for 1-4 h, and filtering to obtain a magnesium ion leaching solution. The leaching aid adopted in the process is relatively small in dosage, cheap and easily available, safe and non-toxic, does not cause environmental pollution, and provides a more appropriate leaching aid for improving the efficiency of acid leaching of serpentine. In addition, the invention can realize the efficient acid leaching of serpentine under normal pressure, improves the pH value of the leaching solution, reduces the corrosion to leaching equipment, and has relatively simple and easily controlled operation and easy realization of industrialization.
Description
Technical Field
The invention relates to the field of hydrometallurgy, in particular to a leaching process of magnesium ions in serpentine.
Background
In the prior serpentine development and utilization process, due to the problems of ore properties, mining process, dressing and smelting technology and the like, a large amount of serpentine tailings are generated, and account for about one third to two thirds of the mining amount. The discharge and accumulation of a large amount of serpentine tailings not only occupy the land, but also cause serious environmental pollution and natural ecological damage, and influence the normal production order. In addition, the serpentine tailings contain about 40% of magnesium element and a small amount of other metal elements, and valuable metal elements are not recycled, so that the metal mineral resources are greatly wasted, and huge loss is brought to national economy. Therefore, the comprehensive utilization problem of the tailings containing the serpentine is effectively solved, the development of ecological environment is facilitated, the crisis that magnesium resources are reduced day by day can be relieved, the economic value of the ore is increased, the economic income of enterprises is improved, and the unification of resources, economy and environment is realized. Meanwhile, the comprehensive utilization process of the serpentine tailings is optimized, the valuable components in the serpentine tailings are efficiently, environmentally and economically extracted, and the method has important practical significance for improving the comprehensive utilization level of mineral resources.
At present, the common methods for extracting valuable components from serpentine mainly comprise physical beneficiation, biological beneficiation and chemical beneficiation, wherein the chemical beneficiation method (leaching and roasting) is a main method for extracting the valuable components from the serpentine.
Disclosure of Invention
The technical task of the invention is to provide a high-efficiency and economic leaching process of magnesium ions in serpentine aiming at the problems of low efficiency, large energy consumption in the process and serious equipment corrosion in the serpentine,
the technical scheme adopted by the invention for solving the technical problems is as follows: a leaching process of magnesium ions in serpentine comprises the following steps: mixing serpentine and a leaching agent, carrying out normal-pressure water bath reaction at the stirring speed of 200-600 r/min, adding fluorite mineral powder serving as a leaching aid while stirring for 1-3 min, continuously reacting and leaching for 1-4 h, and filtering to obtain a magnesium ion leaching solution.
Preferably, the liquid-solid mass ratio of the serpentine to the leaching agent is 3: 1-6: 1.
Preferably, the leaching agent is a sulfuric acid aqueous solution, wherein the use amount of sulfuric acid is 1.1-1.4 times of the theoretical value.
Preferably, the adding amount of the fluorite mineral powder is 1-7% of the mass of the serpentine.
Further preferably, the adding amount of the fluorite mineral powder is 5% of the mass of the serpentine.
Preferably, the temperature of the water bath reaction is 70-90 ℃.
Preferably, the particle size of the serpentine and fluorite mineral powder is-0.074 mm.
Further preferably, the liquid-solid ratio is 4: 1, and the use amount of the sulfuric acid is 1.1 times of the theoretical value; the water bath temperature is 90 ℃, and the leaching time is 2 h.
Compared with the traditional leaching process, the method has the advantages that:
1. the process can effectively dissolve the magnesium element in the serpentine ore at normal pressure and low temperature, and improves the leaching efficiency. Meanwhile, compared with the traditional method for acid leaching of serpentine, the addition of the leaching aid (fluorite mineral powder) can reduce the acid consumption, improve the pH value of the leaching solution, reduce the corrosion degree of leaching equipment and prolong the service life of the equipment;
2. the auxiliary leaching agent adopted in the invention is relatively small in usage amount of fluorite mineral powder, cheap and easily available, safe and nontoxic, and can not cause environmental pollution;
3. the process realizes the comprehensive recycling of the serpentine tailings, can efficiently extract valuable metal elements, reduces the economic cost and the environmental cost, and realizes the unification of economic, resource and environmental benefits to the utmost extent, thereby having important significance for realizing the efficient comprehensive utilization of serpentine resources.
Drawings
FIG. 1 is a diagram showing the operation of acid leaching serpentine according to the embodiment of the present invention.
FIG. 2 is an X-ray diffraction analysis chart of the leaching residue of the embodiment and the comparative example.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The test methods described in the following examples of the present invention are all conventional methods unless otherwise specified; the reagents and materials, unless otherwise indicated, are commercially available;
the serpentine in the following embodiment of the invention is waste material from Xiuyan-an-Manchu Xiuyan-jade processing factory in Xiuyan Manchu of Anhui mountain city in Liaoning, the main components of the serpentine are leaf serpentine, and a small amount of Lisnake and dolomite, the granularity of the prepared sample is-0.074 mm (namely the granularity of the sample is below 0.074 mm), and the content of magnesium oxide is 43.71%.
The leaching agent in the following examples of the invention is sulfuric acid, and the theoretical amount of sulfuric acid is calculated based on the content of magnesium oxide, calcium oxide, and a small amount of iron oxide that can react with sulfuric acid in the serpentine component detection.
The fluorite ore powder adopted in the following embodiment of the invention mainly contains elements such as calcium oxide, fluorine, silicon dioxide and the like, wherein the content of calcium fluoride in the fluorite ore powder is 74%, and the granularity of the fluorite ore powder is-0.074 mm.
After leaching is finished in the following embodiments of the invention, a leaching product is filtered and leached; the filtrate product is the pregnant solution, and magnesium ions in the pregnant solution can be recovered; and (3) drying, weighing, testing grade and calculating leaching rate of the filter residue product, namely leaching residue.
The leaching rate of magnesium oxide in the following examples of the present invention means: the degree to which the magnesium to be extracted is leached, i.e. the percentage of magnesium leached.
The MgO leaching rate calculation formula is as follows:
m0-mass of leached material, in g;
R0-grade of MgO in the leached material, unit%;
m is the mass of the leaching residue, unit g;
r is the grade of MgO in the leaching residue, unit percent;
the DF-i heat collection type magnetic heating stirrer, rw20dzm.n electric stirrer, used in the following examples was purchased from prospecting mechanical plant in gillin province.
Example 1
A process for leaching magnesium ions from serpentine, as shown in figure 1, comprises the following steps:
(1) weighing 15g of serpentine ore sample to be treated under normal pressure, putting the serpentine ore sample into a beaker, adding a leaching agent according to the liquid-solid ratio of 4: 1 by mass, mixing, and pouring into a three-neck flask, wherein the addition amount of sulfuric acid serving as the leaching agent is 1.1 times of the theoretical dosage; placing the three-neck flask in a water bath kettle at 90 ℃, and continuously stirring at the rotating speed of 300 r/min;
(2) after stirring for 3min, adding fluorite mineral powder serving as an auxiliary leaching agent, wherein the adding amount of the fluorite mineral powder is 1 percent of the mass of the serpentine mineral sample; continuously stirring, filtering and leaching the ore sample after leaching for 2 hours, recovering the leaching solution, drying, weighing, preparing a sample, detecting leaching residues, and calculating the leaching rate; the leaching rate of the magnesium oxide was 88.10%.
Example 2
A leaching process of magnesium ions in serpentine comprises the following steps:
(1) the reaction conditions were the same as in the step (1) in example 1;
(2) after stirring for 3min, adding fluorite mineral powder serving as an auxiliary leaching agent, wherein the adding amount of the fluorite mineral powder is 3% of the mass of the serpentine mineral sample; continuously stirring, leaching the ore sample for 2 hours, filtering, leaching, recovering the leaching solution, drying leaching residues, weighing, preparing a sample, detecting, and calculating the leaching rate; the leaching rate of the magnesium oxide was 90.46%.
Example 3
A leaching process of magnesium ions in serpentine comprises the following steps:
(1) the reaction conditions were the same as in the step (1) in example 1;
(2) after stirring for 3min, adding fluorite mineral powder serving as an auxiliary leaching agent, wherein the adding amount of the fluorite mineral powder is 5% of the mass of the serpentine mineral sample; continuously stirring, leaching the ore sample for 2 hours, filtering, leaching, recovering the leaching solution, drying leaching residues, weighing, preparing a sample, detecting, and calculating the leaching rate; the leaching rate of the magnesium oxide is 94.88%.
Example 4
A leaching process of magnesium ions in serpentine comprises the following steps:
(1) the reaction conditions were the same as in the step (1) in example 1;
(2) after stirring for 3min, adding fluorite ore powder serving as an auxiliary leaching agent, wherein the adding amount of the fluorite ore powder is 7 percent of the mass of the serpentine ore sample; continuously stirring, leaching the ore sample for 2 hours, filtering, leaching, recovering the leaching solution, drying leaching residues, weighing, preparing a sample, detecting, and calculating the leaching rate; the leaching rate of the magnesium oxide was 88.91%.
As can be seen from the embodiments 1, 2, 3 and 4, in the leaching process of magnesium ions in serpentine, the optimal dosage of fluorite mineral powder is 5%, and the leaching rate of magnesium oxide can reach 94.88%.
Example 5
A leaching process of magnesium ions in serpentine comprises the following steps:
(1) weighing 15g of serpentine sample to be treated at normal pressure, putting the serpentine sample into a beaker, adding a leaching agent according to a liquid-solid ratio of 3: 1, mixing, and pouring into a three-neck flask, wherein the addition of sulfuric acid serving as the leaching agent is 1.1 times of the theoretical dosage; placing the three-neck flask in a water bath kettle at 90 ℃, and continuously stirring at the rotating speed of 300 r/min;
(2) after stirring for 3min, adding fluorite mineral powder serving as an auxiliary leaching agent, wherein the adding amount of the fluorite mineral powder is 5% of the mass of the serpentine mineral sample; continuously stirring, leaching the ore sample for 2 hours, filtering, leaching, recovering the leaching solution, drying leaching residues, weighing, preparing a sample, detecting, and calculating the leaching rate; the leaching rate of magnesium oxide was 92.31%.
Example 6
A leaching process of magnesium ions in serpentine comprises the following steps:
(1) weighing 15g of serpentine sample to be treated at normal pressure, putting the serpentine sample into a beaker, adding a leaching agent according to a liquid-solid ratio of 5: 1, mixing, and pouring into a three-neck flask, wherein the addition of sulfuric acid serving as the leaching agent is 1.1 times of the theoretical dosage; placing the three-neck flask in a water bath kettle at 90 ℃, and continuously stirring at the rotating speed of 300 r/min;
(2) after stirring for 3min, adding fluorite mineral powder serving as an auxiliary leaching agent, wherein the adding amount of the fluorite mineral powder is 5% of the mass of the serpentine mineral sample; continuously stirring, leaching the ore sample for 2 hours, filtering, leaching, recovering the leaching solution, drying leaching residues, weighing, preparing a sample, detecting, and calculating the leaching rate; the leaching rate of magnesium oxide was 93.71%.
Example 7
A leaching process of magnesium ions in serpentine comprises the following steps:
(1) weighing 15g of serpentine sample to be treated at normal pressure, putting the serpentine sample into a beaker, adding a leaching agent according to a liquid-solid ratio of 4: 1, mixing, and pouring into a three-neck flask, wherein the addition amount of sulfuric acid serving as the leaching agent is 1.3 times of the theoretical dosage; placing the three-neck flask in a water bath kettle at 70 ℃, and continuously stirring at the rotating speed of 300 r/min;
(2) after stirring for 3min, adding fluorite mineral powder serving as an auxiliary leaching agent, wherein the adding amount of the fluorite mineral powder is 5% of the mass of the serpentine mineral sample; continuously stirring, leaching the ore sample for 2 hours, filtering, leaching, recovering the leaching solution, drying leaching residues, weighing, preparing a sample, detecting, and calculating the leaching rate; the leaching rate of the magnesium oxide is 89.75%.
Example 8
A leaching process of magnesium ions in serpentine comprises the following steps:
(1) weighing 15g of serpentine sample to be treated at normal pressure, putting the serpentine sample into a beaker, adding a leaching agent according to a liquid-solid ratio of 4: 1, mixing, and pouring into a three-neck flask, wherein the addition amount of sulfuric acid serving as the leaching agent is 1.3 times of the theoretical dosage; placing the three-neck flask in a water bath kettle at 80 ℃, and continuously stirring at the rotating speed of 300 r/min;
(2) after stirring for 3min, adding fluorite mineral powder serving as an auxiliary leaching agent, wherein the adding amount of the fluorite mineral powder is 5% of the mass of the serpentine mineral sample; continuously stirring, leaching the ore sample for 2 hours, filtering, leaching, recovering the leaching solution, drying leaching residues, weighing, preparing a sample, detecting, and calculating the leaching rate; the leaching rate of magnesium oxide was 91.00%.
Example 9
A leaching process of magnesium ions in serpentine comprises the following steps:
(1) weighing 15g of serpentine sample to be treated at normal pressure, putting the serpentine sample into a beaker, adding a leaching agent according to a liquid-solid ratio of 4: 1, mixing, and pouring into a three-neck flask, wherein the addition of sulfuric acid serving as the leaching agent is 1.2 times of the theoretical dosage; placing the three-neck flask in a water bath kettle at 90 ℃, and continuously stirring at the rotating speed of 300 r/min;
(2) after stirring for 3min, adding fluorite mineral powder serving as an auxiliary leaching agent, wherein the adding amount of the fluorite mineral powder is 5% of the mass of the serpentine mineral sample; continuously stirring, leaching the ore sample for 2 hours, filtering, leaching, recovering the leaching solution, drying leaching residues, weighing, preparing a sample, detecting, and calculating the leaching rate; the leaching rate of the magnesium oxide is 94.65%.
Example 10
A leaching process of magnesium ions in serpentine comprises the following steps:
(1) weighing 15g of serpentine sample to be treated at normal pressure, putting the serpentine sample into a beaker, adding a leaching agent according to a liquid-solid ratio of 4: 1, mixing, and pouring into a three-neck flask, wherein the addition of sulfuric acid serving as the leaching agent is 1.4 times of the theoretical dosage; placing the three-neck flask in a water bath kettle at 90 ℃, and continuously stirring at the rotating speed of 300 r/min;
(2) after stirring for 3min, adding fluorite mineral powder serving as an auxiliary leaching agent, wherein the adding amount of the fluorite mineral powder is 5% of the mass of the serpentine mineral sample; continuously stirring, leaching the ore sample for 2 hours, filtering, leaching, recovering the leaching solution, drying leaching residues, weighing, preparing a sample, detecting, and calculating the leaching rate; the leaching rate of the magnesium oxide is 88.92%.
Example 11
A leaching process of magnesium ions in serpentine comprises the following steps:
(1) weighing 15g of serpentine sample to be treated at normal pressure, putting the serpentine sample into a beaker, adding a leaching agent according to a liquid-solid ratio of 4: 1, mixing, and pouring into a three-neck flask, wherein the addition amount of sulfuric acid serving as the leaching agent is 1.3 times of the theoretical dosage; placing the three-neck flask in a water bath kettle at 90 ℃, and continuously stirring at the rotating speed of 300 r/min;
(2) after stirring for 3min, adding fluorite mineral powder serving as an auxiliary leaching agent, wherein the adding amount of the fluorite mineral powder is 5% of the mass of the serpentine mineral sample; continuously stirring, filtering and leaching the ore sample after leaching for 1h, recovering the leaching solution, drying leaching residues, weighing, preparing a sample, detecting, and calculating the leaching rate; the leaching rate of the magnesium oxide is 92.06%.
Example 12
(1) The reaction conditions were the same as in step (1) in example 11;
(2) after stirring for 3min, adding fluorite mineral powder serving as an auxiliary leaching agent, wherein the adding amount of the fluorite mineral powder is 5% of the mass of the serpentine mineral sample; continuously stirring, leaching the ore sample for 2.5h, filtering, leaching, recovering the leaching solution, drying, weighing, preparing a sample, detecting leaching residues, and calculating the leaching rate; the leaching rate of magnesium oxide was 93.76%.
Example 13
A leaching process of magnesium ions in serpentine comprises the following steps:
(1) weighing 15g of serpentine sample to be treated at normal pressure, putting the serpentine sample into a beaker, adding a leaching agent according to a liquid-solid ratio of 4: 1, mixing, and pouring into a three-neck flask, wherein the addition amount of sulfuric acid serving as the leaching agent is 1.3 times of the theoretical dosage; placing the three-neck flask in a water bath kettle at 90 ℃, and continuously stirring at the rotating speed of 200 r/min;
(2) after stirring for 3min, adding fluorite mineral powder serving as an auxiliary leaching agent, wherein the adding amount of the fluorite mineral powder is 5% of the mass of the serpentine mineral sample; continuously stirring, leaching the ore sample for 2 hours, filtering, leaching, recovering the leaching solution, drying leaching residues, weighing, preparing a sample, detecting, and calculating the leaching rate; the leaching rate of the magnesium oxide is 89.07%.
Example 14
A leaching process of magnesium ions in serpentine comprises the following steps:
(1) weighing 15g of serpentine sample to be treated at normal pressure, putting the serpentine sample into a beaker, adding a leaching agent according to a liquid-solid ratio of 4: 1, mixing, and pouring into a three-neck flask, wherein the addition amount of sulfuric acid serving as the leaching agent is 1.3 times of the theoretical dosage; placing the three-neck flask in a water bath kettle at 90 ℃, and continuously stirring at the rotating speed of 600 r/min;
(2) after stirring for 3min, adding fluorite mineral powder serving as an auxiliary leaching agent, wherein the adding amount of the fluorite mineral powder is 5% of the mass of the serpentine mineral sample; continuously stirring, leaching the ore sample for 2 hours, filtering, leaching, recovering the leaching solution, drying leaching residues, weighing, preparing a sample, detecting, and calculating the leaching rate; the leaching rate of the magnesium oxide is 93.94%.
Comparative example 1
(1) Weighing 15g of serpentine sample to be treated at normal pressure, putting the serpentine sample into a beaker, adding a leaching agent according to a liquid-solid ratio of 4: 1, mixing the leaching agent with the serpentine sample, and pouring the mixture into a three-neck flask, wherein the leaching agent is 1.1 times of the theoretical dosage of sulfuric acid; placing the three-neck flask in a water bath kettle at 90 ℃, and continuously stirring at the rotating speed of 300 r/min;
(2) no auxiliary leaching agent fluorite powder is added; continuously stirring, filtering and leaching the ore sample after leaching for 2 hours, recovering the leaching solution, drying, weighing, preparing a sample, detecting leaching residues, and calculating the leaching rate; the leaching rate of magnesium oxide was 56.44%.
From the test data of the above example experiment, compared with the serpentine acid leaching without using the fluorite as the leaching assistant, the fluorite mineral powder as the leaching assistant can significantly improve the leaching rate of MgO, and realize the efficient acid leaching of serpentine under normal pressure.
As shown in FIG. 2, from the top and bottom X-ray diffraction charts of the serpentine in example, the slag in comparative example and the slag in example 3, respectively, it is found that the serpentine in the sample ore has a characteristic diffraction peak d of 7.28,
The strong spectral line at and d 4.62,
d is 2.52, 2.42,
The spectral line is the characteristic diffraction peak of the antigorite. The leaching residue obtained after the serpentine is directly acid-leached by sulfuric acid still has part of serpentine with strong characteristic peak diffraction peak, and the serpentine leaching residue added with the fluorite powder serving as the leaching assistant basically has no obvious characteristic diffraction peak of the serpentine and has a small amount of calcium sulfate and an obvious amorphous silicon dioxide diffraction peak. After the fluorite mineral powder serving as the leaching aid is added, calcium fluoride in the fluorite mineral powder generates hydrofluoric acid (solution) and calcium sulfate (precipitate) in a sulfuric acid system, however, a serpentine structure is composed of a silica tetrahedral layer and a magnesium hydroxide octahedral layer, and the hydrofluoric acid can react with silicon dioxide to generate fluosilicic acid, so that the structure of the silica tetrahedral layer of the serpentine is damaged, more magnesium ions are exposed, the dissolution of the magnesium ions is enhanced, and the leaching rate is improved.
The technical idea of the present invention is described in the above technical solutions, and the protection scope of the present invention is not limited thereto, and any changes and modifications made to the above technical solutions according to the technical essence of the present invention belong to the protection scope of the technical solutions of the present invention.
Claims (7)
1. A leaching process of magnesium ions in serpentine comprises the following steps: mixing serpentine and a leaching agent, carrying out normal-pressure water bath reaction at the stirring speed of 200-600 r/min, adding fluorite mineral powder serving as a leaching aid while stirring for 1-3 min, continuously reacting and leaching for 1-4 h, and filtering to obtain a magnesium ion leaching solution.
2. The process of claim 1, wherein the liquid-solid mass ratio of the serpentine to the leaching agent is 3: 1 to 6: 1.
3. The process of claim 1, wherein the leaching agent is an aqueous solution of sulfuric acid, wherein the amount of sulfuric acid is 1.1 to 1.4 times the theoretical amount.
4. The process for leaching magnesium ions from serpentine according to claim 1, wherein the fluorite ore powder is added in an amount of 1-7% by mass of the serpentine.
5. The process for leaching magnesium ions from serpentine according to claim 1, wherein the temperature of the water bath reaction is 70-90 ℃.
6. The process of claim 1, wherein the serpentine and fluorite fines are sized to have a particle size of-0.074 mm.
7. The process of claim 1, wherein the liquid-to-solid ratio is 4: 1; the dosage of the sulfuric acid is 1.1 times of the theoretical value; the temperature of the water bath is 90 ℃; the adding amount of fluorite mineral powder is 5% of the mass of the serpentine, and the leaching time is 2 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115838183A (en) * | 2023-02-15 | 2023-03-24 | 中南大学 | Method for separating silicon and magnesium from black talc |
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| CN115838183A (en) * | 2023-02-15 | 2023-03-24 | 中南大学 | Method for separating silicon and magnesium from black talc |
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