CN115261604A - Method for leaching magnesium by using serpentine acid - Google Patents
Method for leaching magnesium by using serpentine acid Download PDFInfo
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- CN115261604A CN115261604A CN202210212360.2A CN202210212360A CN115261604A CN 115261604 A CN115261604 A CN 115261604A CN 202210212360 A CN202210212360 A CN 202210212360A CN 115261604 A CN115261604 A CN 115261604A
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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
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/22—Magnesium silicates
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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
The invention belongs to the field of ore leaching and comprehensive utilization thereof, and particularly relates to a method for leaching magnesium from serpentine, wherein the serpentine is subjected to activation pretreatment and then acid leaching treatment to obtain leachate enriched with magnesium; the activation pretreatment comprises at least one of supercritical fluid treatment, subcritical fluid treatment, ultrasonic treatment and microwave treatment. According to the invention, researches show that the activation pretreatment of the serpentine by the process can regulate and control the physical and chemical structures of the serpentine, so that the acid leaching efficiency and effect of the serpentine can be unexpectedly improved, the magnesium extraction rate can be improved, the selectivity of magnesium and silicon can be improved, and the purity of magnesium leaching solution can be further improved.
Description
Technical Field
The invention belongs to the technical field of mining and metallurgy, and particularly relates to the technical field of comprehensive utilization of serpentine.
Background
The serpentine mineral resources in China are rich and have good quality, and most serpentine minerals are often accompanied by various metal minerals such as iron, nickel, cobalt, chromium and the like. Although China has abundant serpentine resources, the comprehensive utilization level of serpentine is not high, and particularly the enrichment of valuable components and the utilization efficiency of all components are low. Therefore, how to extract valuable elements in serpentine efficiently and greenly becomes a current research hotspot. In addition, serpentine is often symbiotic with and associated with a variety of minerals, producing nearly millions of tons of serpentine tailings every year throughout the country. Therefore, the comprehensive utilization of the serpentine is particularly important, the direct utilization of the serpentine ore is researched, the comprehensive recovery of the serpentine tailings is also considered, the natural ecological environment can be improved, the secondary recovery of resources can be realized, new benefits and development are added for mine enterprises, and the method is also a main direction for development and utilization in the future.
The serpentine is mainly applied to the following aspects: manufacturing chemical fertilizers, preparing refractory materials, preparing industrial products, preparing lubricating self-repairing agents and the like. The serpentine contains about 30-40% magnesium oxide and 30-40% silicon dioxide. Nowadays, the key problem of serpentine is to extract magnesium from serpentine so as to obtain magnesium salt products.
The scheme for extracting magnesium element at present mainly comprises two schemes of wet leaching and fire roasting. The former mainly uses inorganic strong acid (sulfuric acid, hydrochloric acid, etc.) to leach serpentine directly, or carries out acid leaching after certain pretreatment. The latter is mainly to mix concentrated sulfuric acid or ammonium sulfate with serpentine, then to roast at high temperature, and then to extract magnesium by water. In any of these methods, the leaching rate of magnesium is 90% or less, which results in a large amount of waste of magnesium and also hinders the recovery and reuse of other elements.
Disclosure of Invention
Aiming at the problem that the effect of the existing serpentine acid leaching magnesium is not ideal, the invention aims to provide a method for leaching magnesium by using serpentine acid, aiming at improving the effect of the serpentine acid leaching magnesium.
Serpentine is in fact an aqueous magnesium silicate rich mineral, an ideal compound of which should be Mg8(Si4O10)(OH)8Its main chemical components are MgO and SiO2And may also contain minor amounts of other components. The crystal structure of serpentine is mainly formed by overlapping multiple layers of metal ions in the crystal. The crystal is ideally of the trioctahedral type, consisting of a combination of a layer of silica tetrahedra and a layer of magnesium hydroxide octahedra, and has relatively weak van der waals forces with adjacent serpentine platelets. The serpentine has a stable silicate structure, so that magnesium in the serpentine is difficult to be out of the constraint and enter the solution. On the other hand, many scholars have learned that the serpentine has many active groups through intensive research on the crystal structure and chemical components of the serpentine, and the serpentine has relatively high chemical activity due to the existence of the active groups. These active groups are easily oxidized by oxygen in the air or the like to lose their activity, so that the activated serpentine powder becomes more difficult to leach out, and therefore the activated serpentine powder should be vacuum-sealed. Snake linesThe melting point of the stone itself is low, but if the content of magnesium oxide is too high, the melting point of serpentine becomes very high and is less prone to leaching.
Aiming at the problems of non-ideal effect of serpentine acid leaching magnesium and non-ideal selectivity of magnesium-silicic acid leaching separation, the invention provides the following improvement methods:
a method for leaching magnesium from serpentine with acid comprises activating serpentine, and performing acid leaching to obtain magnesium-enriched leachate;
the activation pretreatment comprises at least one of supercritical fluid treatment, subcritical fluid treatment, ultrasonic treatment and microwave treatment.
According to the invention, researches show that the activation pretreatment of the serpentine by the process can regulate and control the physical and chemical structures of the serpentine, so that the acid leaching efficiency and effect of the serpentine can be improved unexpectedly, the magnesium extraction rate can be improved, the selectivity of magnesium and silicon can be improved, and the purity of magnesium leaching liquid can be further improved.
In the invention, the serpentine can be any raw ore, waste material and the like containing serpentine in the industry.
The serpentine has no particular requirement for its composition and content, and for example, has 30 to 40% magnesium oxide, which contains nickel and other impurities as an allowance, and the balance is silica.
In the present invention, the serpentine can be subjected to crushing, pulverizing, sieving, etc. by conventional means, followed by the activation pretreatment according to the present invention.
In the present invention, the particle size of the serpentine is not particularly required, and for example, the particle size of the serpentine may be adjusted as necessary, and in view of the treatment economy, the serpentine has a particle size of 150 to 200 mesh;
the research of the invention finds that the activation process of supercritical fluid treatment, subcritical fluid treatment, ultrasonic treatment and microwave treatment is the key for improving the physical and microstructure of serpentine and improving the subsequent acid leaching effect.
In the present invention, the fluid component in the supercritical fluid treatment and the subcritical fluid treatment is at least one of water and carbon dioxide. For example, serpentine can be subjected to an activation pretreatment in a system of supercritical water, subcritical water, supercritical gas such as supercritical carbon dioxide. In the present invention, the serpentine can be in the supercritical and subcritical system based on the existing means, for example, a corresponding critical fluid can be directly introduced into the system, or the serpentine can be placed in a fluid solvent, and the temperature and pressure are controlled to convert the solvent of the system into a fluid state.
In the invention, the ultrasonic power is 300-800W.
In the invention, the power of the microwave treatment process is 300-800W. Preferably, the temperature for heating by microwave is 300-500 ℃.
In the invention, the time of the activation pretreatment is 5-60 min.
In the invention, after the activation pretreatment, the high-efficiency magnesium extraction can be realized based on the conventional acid leaching treatment.
For example, in the invention, the acid solution used in the acid leaching process is an aqueous solution of inorganic strong acid; the inorganic strong acid is at least one of sulfuric acid, nitric acid and hydrochloric acid.
In the present invention, the concentration of the strong inorganic acid in the acid solution is 1 to 5mol/L, and more preferably 1 to 3mol/L.
In the invention, the liquid-solid ratio of the acid leaching city can be adjusted according to the needs, for example, the liquid-solid ratio is 1-50 mL/g; further preferably 5 to 20mL/g;
preferably, the acid leaching temperature is 20-80 ℃;
preferably, the acid leaching time is 0.5 to 3 hours.
In the invention, the white carbon black is prepared from the slag obtained by acid leaching.
The invention relates to a specific method for leaching magnesium by serpentine acid, which comprises the following steps:
the first step is as follows:
crushing large serpentine ores, crushing, and sieving to obtain serpentine powder with proper meshes;
the second step is that:
activating pretreatment is carried out on the serpentine powder by adopting high-energy equipment, wherein the activating pretreatment comprises at least one of supercritical fluid treatment, subcritical fluid treatment, ultrasonic treatment and microwave treatment; the time of the activation pretreatment is 5-60 min;
the third step: acid leaching:
and leaching the serpentine powder treated in the second step by adopting inorganic strong acid, and then carrying out liquid-solid separation to obtain leachate and leaching residues, wherein the leachate is used for obtaining pure magnesium sulfate, and the leaching residues are used for obtaining the white carbon black product.
Advantageous effects
In the invention, the serpentine is innovatively subjected to the activation pretreatment of the process, so that the physical and chemical structures in the serpentine can be unexpectedly regulated, the magnesium leaching effect can be unexpectedly improved, and the selective acid leaching separation of magnesium and silicon is facilitated.
Drawings
FIG. 1 is a process flow diagram of the present invention;
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited to the following examples.
In the following cases, the serpentine is mainly from asbestos tailings, contains 30-40% of magnesium oxide, about 50% of silicon dioxide and about 1% of nickel oxide, and is produced by a certain asbestos production company in Xinjiang.
Example 1:
(1) crushing and screening: crushing the block serpentine with the diameter of about 10mm into small blocks with the diameter of 2mm by a crusher, then crushing the small blocks with the diameter of 2mm into powder by a disc powder machine, and sieving to obtain the serpentine powder with the diameter of 150-200 meshes.
(2) Activation pretreatment: weighing 100g of serpentine powder with the particle size, heating to 450 ℃ by using microwave (the power is 450W), and keeping the temperature for 10min;
(3) acid leaching: immediately after the temperature is reduced to below 100 ℃, 5g (in the present invention, dry weight) of the above microwave-activated serpentine powder is taken and placed in a 100mL beaker, and the mass ratio of the serpentine powder to the total mass ratio of 10:1, adding 2mol/L sulfuric acid prepared in advance into the liquid-solid ratio, placing the beaker into a water bath stirring pot with the constant temperature of 30 ℃, and setting the reaction time to be 2 hours;
and filtering the acid leaching solution to obtain acid leaching solution and acid leaching residue. The content of magnesium ions in the pickle liquor is obtained by ICP test, and the leaching rate of the magnesium ions is calculated to be 99.3 percent. The leached residues are directly used for producing white carbon black, the DPB oil absorption value of the white carbon black is 3.42mL/g, and the purity reaches 99%.
Example 2:
compared with example 1, the only difference is that the activation pretreatment conditions of step (2) are adjusted to be: a: the microwave power is 300W, the heating temperature is 300 ℃, and the processing time is 50min; b: the microwave power is 800W, the heating temperature is 500 ℃, and the treatment time is 5min.
The acid leaching treatment was carried out by the method of example 1, and the measurement was carried out, the results were:
group A: the leaching rate of magnesium ions was 99.5%. The leached residues are directly used for producing white carbon black, the DPB oil absorption value of the white carbon black is 3.39mL/g, and the purity reaches 98.9%.
Group B: the leaching rate of magnesium ions was 99.1%. The leached residues are directly used for producing white carbon black, the DPB oil absorption value of the white carbon black is 3.43mL/g, and the purity reaches 99.2%.
Example 3:
(1) crushing and screening: the method comprises the following steps of crushing the blocky serpentine with the size of about 10mm into small blocks with the size of 2mm by using a crusher, then crushing the small blocks with the size of 2mm into powder by using a disc powder machine, and sieving the powder to obtain the serpentine powder with the size of 150-200 meshes.
(2) Activation pretreatment: weighing 10g of serpentine powder with the particle size in a beaker, and mixing the serpentine powder with the powder according to the weight ratio of 10: adding deionized water into the solution-solid ratio of 1, mixing the solution and the solid, adding the mixture into a supercritical (subcritical) reaction kettle, and activating for 10min under the supercritical conditions that the reaction temperature is 180 ℃, the subcritical reaction pressure is 18MPa or the reaction temperature is 380 ℃ and the reaction pressure is 28 MPa;
(3) acid leaching: after the activation reaction is finished, a solid sample obtained by solid-liquid separation is washed in ice bath, 5g of dried serpentine powder (in the invention, all refer to dry weight) is taken after filtration and freeze drying, and is put into a 100mL beaker, and then the weight ratio of the serpentine powder is calculated according to the following formula: adding 2mol/L sulfuric acid prepared in advance into the liquid-solid ratio of 1, placing the beaker in a water bath stirring pot with the constant temperature of 30 ℃, and setting the reaction time to be 2 hours;
and filtering the acid leaching solution to obtain acid leaching solution and acid leaching residue. The content of magnesium ions in the pickle liquor is obtained by ICP test, and the leaching rate of the magnesium ions is calculated to be 98.8 percent (subcritical) and 99.8 percent (supercritical). The leaching residue obtained by supercritical treatment and separation is directly used for producing the white carbon black, the DPB oil absorption value of the white carbon black is 3.38mL/g, and the purity reaches 99.2%.
Example 4
Compared with the example 1, the difference is only that in the activation pretreatment (2), the activation pretreatment is carried out by adopting an ultrasonic process, and the treatment parameters are as follows: (A): the ultrasonic power is 300W, and the ultrasonic time is 50min; (B): the ultrasonic power is 800W, and the ultrasonic time is 10min;
the acid leaching treatment was carried out by the method of example 1, and the measurement was carried out, the results were:
group A: the leaching rate of magnesium ions was 99.5%. The leached residues are directly used for producing white carbon black, the DPB oil absorption value of the white carbon black is 3.35mL/g, and the purity reaches 99.4%.
Group B: the leaching rate of magnesium ions was 99.6%. The leached residues are directly used for producing white carbon black, the DPB oil absorption value of the white carbon black is 3.43mL/g, and the purity reaches 99.6%.
Comparative example 1:
the difference from example 1 is only that (2) in the activation pretreatment, the heating temperature of the microwave was 200 ℃ and other parameters and measurement methods were the same as those of example 1.
Under the condition, the leaching rate of the obtained magnesium ions is 87%, the DPB oil absorption value of the white carbon black is 1.81mL/g, and the purity reaches 87.2%.
Comparative example 2
The only difference compared to example 1 is that (2) the activation pretreatment step was not performed. Other parameters and measurement methods were the same as in example 1.
The leaching rate of magnesium ions was 72%. The leached residues are directly used for producing white carbon black, the DPB oil absorption value of the white carbon black is 1.26mL/g, and the purity reaches 74%.
Comparative example 3:
compared with example 1, the difference is only that: the microwave pretreatment was replaced by mechanical ball milling (at 500 r/min) for 1h, and other parameters and measurement methods were the same as in example 1. Under the condition, the leaching rate of the obtained magnesium ions is 80%, the DPB oil absorption value of the white carbon black is 1.33mL/g, and the purity only reaches 80%.
Comparative example 4:
compared with example 1, the difference is only that: the microwave pretreatment of the activation pretreatment of (2) is replaced by an electric heating method, the temperature of the electric heating stage is 450 ℃ or 700 ℃, and other parameters and measuring methods are the same as those of the example 1.
The results were: the leaching rate of magnesium ions is 80.2% at the temperature of 450 ℃. The leached residues are directly used for producing white carbon black, the DPB oil absorption value of the white carbon black is 1.42mL/g, and the purity reaches 81.6%.
At the temperature of 700 ℃, the leaching rate of magnesium ions is 85.3 percent, the DPB oil absorption value of the white carbon black is 1.78mL/g, and the purity reaches 84.3 percent.
Comparative example 5:
compared with example 1, the difference is only that: (2) in the activation pretreatment, the microwave pretreatment of example 1 is replaced by an activation process of mechanical ball milling (rotating speed 500 r/mi) for 1h and then calcining in a muffle furnace at 700 ℃ for 1h, and other parameters and measuring methods are the same as those of example 1. The leaching rate of the treated magnesium ions is 86.9 percent, the DPB oil absorption value of the white carbon black is 1.81mL/g, and the purity only reaches 86 percent.
Comparative example 6:
compared with example 3, the only difference is that (2) in the activation pretreatment, the temperature and pressure of the treatment do not reach the subcritical state, for example, the temperature of the treatment process is 150 ℃, the pressure is set to 1MPa, and other parameters and measuring methods are the same as those of example 1. The leaching rate after treatment is 81.1 percent, the DPB oil absorption value of the white carbon black is 1.41mL/g, and the purity only reaches 80.9 percent.
Comparative example 7:
compared with example 1, the difference is only that (2) is not carried out, and in (3), the ultrasonic assistance with the power of 200W is adopted for acid leaching, and other parameters and operations are the same as those of example 1.
The leaching rate of magnesium ions was calculated to be 84.9%. The leached residues are directly used for producing white carbon black, the DPB oil absorption value of the white carbon black is 1.84mL/g, and the purity reaches 86.3%.
Claims (10)
1. A method for leaching magnesium from serpentine by acid is characterized in that serpentine is subjected to activation pretreatment and then to acid leaching treatment to obtain leachate enriched with magnesium;
the activation pretreatment comprises at least one of supercritical fluid treatment, subcritical fluid treatment, ultrasonic treatment and microwave treatment.
2. The method for leaching magnesium with serpentine acid as claimed in claim 1, wherein the fluid component in the supercritical fluid treatment and/or subcritical fluid treatment is at least one of water and carbon dioxide.
3. The method for acid leaching of magnesium with serpentine as claimed in claim 1, wherein the ultrasonic power is 300-800W.
4. A method of serpentine acid leaching of magnesium as claimed in claim 1, wherein the microwave treatment process has a power of 300 to 800W.
5. The method for acid leaching of magnesium with serpentine according to claim 1, wherein the time of the activation pre-treatment is 5 to 60min.
6. The method for acid leaching of magnesium with serpentine as claimed in claim 1, wherein the serpentine has a particle size of 150 to 200 mesh;
preferably, the serpentine is obtained by crushing, crushing and sieving raw ores.
7. The method of acid leaching magnesium according to claim 1, wherein the acid solution used in the acid leaching process is an aqueous solution of a strong inorganic acid; the inorganic strong acid is at least one of sulfuric acid, nitric acid and hydrochloric acid.
8. A method for the acid leaching of magnesium according to claim 7, wherein the concentration of strong inorganic acid in the acid liquor is 1 to 5mol/L, more preferably 1 to 3mol/L.
9. The method for acid leaching of magnesium with serpentine as claimed in claim 7, wherein the acid leach liquor solid ratio is 1-50 mL/g; further preferably 5 to 20mL/g;
preferably, the acid leaching temperature is 20-80 ℃;
preferably, the acid leaching time is 0.5 to 3 hours.
10. The method for acid leaching of magnesium according to any of the claims 1 to 9, wherein the residue obtained from the acid leaching is used to prepare white carbon black.
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