CN109321747B - Method for leaching manganese concentrate from low-grade calciummanganese ore and regenerating leaching medium - Google Patents
Method for leaching manganese concentrate from low-grade calciummanganese ore and regenerating leaching medium Download PDFInfo
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- 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
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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Abstract
The invention discloses a method for leaching manganese concentrate from low-grade manganite and regenerating leaching medium, which comprises the following steps: crushing low-grade manganosite, and soaking the crushed low-grade manganosite particles into a hydrochloric acid solution for reaction; after the reaction is finished, filtering the reaction solution to obtain filtrate and filter residue; cleaning and drying filter residues to obtain manganese concentrate; and adding sulfuric acid into the filtrate, reacting by adopting a hydrothermal method, and filtering after the reaction is finished to obtain a hydrochloric acid solution and calcium sulfate whiskers. The invention has the beneficial effects that: the low-grade manganosite is treated by a chemical method, so that the manganese concentrate with the manganese element more than 40 percent is directly obtained, the process flow is simple, and the manganese content of the obtained manganese concentrate is high. The calcium sulfate crystal whisker is obtained by taking the pickle liquor of the byproduct calcium chloride obtained in the production of manganese concentrate as a raw material and adopting a hydrothermal method, the preparation process is simple, no crystal form control agent is added in the preparation process, no dirt is discharged, the pollution to the environment is reduced, the cost is saved, and the economic benefit is improved.
Description
Technical Field
The invention relates to the technical field of manganese extraction, in particular to a method for leaching manganese concentrate from low-grade manganite and regenerating a leaching medium.
Background
Manganese is a metal with very wide application, is the second most important metal after iron in the steel industry, almost more than 90 percent of manganese is consumed in the steel industry, manganese ore is an important mineral resource and is the most main refining source of manganese metal, the storage amount of manganese ore in China is the sixth world, but most of manganese ore has poor taste. Manganese ores are mainly divided into two major types, namely manganese carbonate ores and manganese oxide ores, and in recent years, in order to relieve the situation of tight supply of magnesium carbonate, a new process flow of electrolyzing manganese dioxide is developed in China so as to utilize manganese dioxide ores with huge reserves. However, the cost of electrolytic manganese dioxide is high, a large amount of low-grade manganese dioxide ores cannot be used for electrolytic industrial production, how to produce high-grade manganese ore powder by using the low-grade manganese dioxide ores provides raw materials for numerous domestic electrolytic manganese production enterprises, and the method becomes a hotspot of current research.
Chinese patent CN 101716556A discloses a flotation enrichment method of low-grade manganese dioxide ore, which comprises the steps of finely grinding raw ore, adjusting the concentration and pH value of the ore pulp, adding an inhibitor consisting of oxalic acid, citric acid and dextrin according to a certain proportion, stirring to enable the inhibitor to be fully contacted with ore particles, adding a collecting agent consisting of alkyl sulfate and fatty acid into the adjusted ore pulp, selecting a proper process flow according to the manganese grade in the raw ore, carrying out multistage selection and scavenging, and finally filtering flotation tailings to obtain manganese-rich tailings with the manganese grade of more than 32%. But the method has the disadvantages of complex process, long flow and low manganese ore enrichment efficiency.
Chinese patent CN 103468928A discloses a method for enriching manganese oxide ore, which comprises the steps of performing strong magnetic preselection on manganese oxide ore to obtain a first product, mixing the first product with a reducing agent, roasting to obtain calcine, grinding the calcine, and performing weak magnetic separation to obtain manganese oxide concentrate and iron concentrate.
Chinese patent CN 102677177A discloses a preparation method of calcium sulfate hemihydrate crystal whisker with large length-diameter ratio, which comprises the steps of taking soluble inorganic calcium salt and inorganic sulfate as raw materials, firstly carrying out coprecipitation at 10-90 ℃, carrying out activation treatment for 1-6 h at 40-150 ℃ after filtering and washing to obtain a precursor, adding the precursor into a hydrothermal medium added with a crystal form control agent, carrying out hydrothermal treatment for 2-10 h at 80-180 ℃, washing, filtering and drying a hydrothermal product to obtain the calcium sulfate hemihydrate crystal whisker with the diameter of 0.1-4 um, the length of 20-3000 um, the length-diameter ratio of 50-1000, regular appearance and uniform size. The preparation method has a complex process flow, and the filtrate after the reaction can not be recycled, thereby causing environmental pollution.
Disclosure of Invention
The invention aims to provide a method for leaching manganese concentrate from low-grade manganite and regenerating a leaching medium, wherein the method is simple in process flow, low in equipment investment and high in manganese element content in the extracted manganese concentrate.
A method for leaching manganese concentrate from low-grade manganite and regenerating leaching medium comprises the following steps:
(1) crushing low-grade manganosite, and soaking the crushed low-grade manganosite particles into a hydrochloric acid solution for reaction; because the main impurities contained in the low-grade manganosite are calcium element and also contain a small amount of magnesium element and silicon element, the low-grade manganosite is crushed and immersed into a hydrochloric acid solution, and the calcium element contained in the low-grade manganosite reacts with the hydrochloric acid to produce a calcium chloride substance dissolved in water;
(2) after the reaction is finished, filtering the reaction solution to obtain filtrate and filter residue; the main component of the filtrate is calcium chloride, and the main component of the filter residue is manganese concentrate;
(3) cleaning and drying filter residues to obtain manganese concentrate;
(4) and adding sulfuric acid into the filtrate, reacting by adopting a hydrothermal method, and filtering after the reaction is finished to obtain a hydrochloric acid solution and calcium sulfate whiskers. Because the main component in the filtrate is calcium chloride, sulfuric acid is added into the filtrate, the sulfuric acid and the calcium chloride react to produce calcium sulfate precipitation insoluble in water and a hydrochloric acid aqueous solution, and the produced hydrochloric acid aqueous solution can be recycled to react with the calcium manganese ore, so that the raw materials are saved, and no pollutant is discharged.
Further, in the step (1), the content of manganese element in the low-grade manganosite is 10-20%; the particle size of the low-grade manganosite particles is less than 2 mm.
Further, in the step (1), the pH of the solution after the reaction is 2 to 4.
Further, in the step (1), the weight ratio of the low-grade manganosite particles in the reaction liquid to the hydrochloric acid is 1: 4-1: 2.
further, in the step (1), the reaction temperature is 20-100 ℃.
Further, in the step (1), the stirring speed of the stirring reaction is 150-300 r/min, and the reaction time is 1-3 h.
Further, in the step (4), the addition amount of the sulfuric acid is 85-100% of the amount of the sulfuric acid required for completely precipitating the calcium ions contained in the filtrate. The addition amount of the sulfuric acid is less than or equal to the sulfuric acid amount required by the complete precipitation of calcium ions contained in the filtrate, so that the sulfuric acid can be completely consumed, and if the sulfate ions are excessive, the excessive sulfate ions are left in the hydrochloric acid solution, so that the leaching of manganese elements in the low-grade calbirnessite can be influenced when the hydrochloric acid aqueous solution is repeatedly utilized.
Further, in the step (4), the added sulfuric acid is sulfuric acid diluted by water; and the volume ratio of the sulfuric acid to the water is as follows: 1: 0-1: 10.
further, in the step (4), the concentration of calcium ions in the reaction solution is controlled to be 5-60 g/L, and then the reaction is carried out by a hydrothermal method. Because the added sulfuric acid is the sulfuric acid diluted by water, the concentration of the sulfuric acid is adjusted by controlling the volume ratio of the sulfuric acid to the water, and the concentration of calcium ions in the reaction liquid is adjusted by the concentration of the sulfuric acid, so that the concentration of the calcium ions in the reaction liquid is 5-60 g/L.
The hydrothermal method refers to a method for preparing a material by dissolving and recrystallizing powder in a sealed pressure vessel using water as a solvent.
Further, in the step (4), the reaction is: reacting for 3-5 h at the temperature of 125-.
The calcium sulfate whisker is a novel acicular fiber sub-nanometer material which grows in a single crystal form, has a uniform cross section, is complete in appearance and has a perfect internal structure. The calcium sulfate whisker has a plurality of excellent physical and chemical properties such as high strength, high modulus, high toughness, high insulativity, wear resistance, high temperature resistance, acid and alkali resistance, corrosion resistance, good infrared reflectivity, easy surface treatment, easy polymer compounding, no toxicity and the like. The calcium sulfate whisker has excellent performance and low price, so the calcium sulfate whisker has excellent cost performance, and is a novel material with wider application field and extremely wide market prospect.
The calcium sulfate crystal whisker is named as gypsum crystal whisker and gypsum fiber and is synthesized by taking gypsum as a raw material.
At present, gypsum is generally used as a raw material in a synthesis method of calcium sulfate whiskers, a crystal form control agent needs to be added in the synthesis process, and filtrate generated in the reaction process cannot be recycled, so that economic investment is increased, and environmental pollution is also caused.
The invention adopts the pickle liquor of calcium chloride as the raw material, prepares the calcium sulfate crystal whisker by a hydrothermal method, has no pollutant discharge in the preparation process, can repeatedly utilize the produced hydrochloric acid, has simple process, reduces the environmental pollution, saves the economic expenditure
The invention has the beneficial effects that: according to the method for leaching manganese concentrate from low-grade manganite and regenerating the leaching medium, the low-grade manganite is treated by a chemical method, so that the manganese concentrate containing more than 40% of manganese elements is directly obtained, compared with the traditional preparation method of the manganese concentrate, the method disclosed by the invention is simple in process flow, and the manganese content of the obtained manganese concentrate is higher.
The method for leaching manganese concentrate from low-grade manganite and regenerating the leaching medium further obtains the calcium sulfate crystal whisker by taking the pickle liquor of the byproduct calcium chloride obtained in the production of the manganese concentrate as a raw material and adopting a hydrothermal method, has the advantages of simple preparation process, no addition of a crystal form control agent in the preparation process, no pollution discharge, environmental pollution reduction, cyclic utilization of the generated byproduct hydrochloric acid in the production of the manganese concentrate, effective reduction of acid consumption, cost saving and improvement of economic benefit.
Detailed Description
Example one
A method for leaching manganese concentrate from low-grade manganite and regenerating leaching medium comprises the following steps:
(1) crushing low-grade manganosite, and soaking the crushed low-grade manganosite particles into a hydrochloric acid solution for reaction;
(2) after the reaction is finished, filtering the reaction solution to obtain filtrate and filter residue;
(3) cleaning and drying filter residues to obtain manganese concentrate;
(4) and adding sulfuric acid into the filtrate, reacting by adopting a hydrothermal method, and filtering after the reaction is finished to obtain a hydrochloric acid solution and calcium sulfate whiskers.
Example two
A method for leaching manganese concentrate from low-grade manganite and regenerating leaching medium comprises the following steps:
(1) crushing low-grade manganite containing 10% of manganese element into particles with the diameter less than 2mm, and immersing the crushed low-grade manganite particles into a hydrochloric acid solution, wherein the weight ratio of the low-grade manganite particles to the hydrochloric acid in the reaction solution is 1: 4, stirring the reaction solution at the temperature of 20 ℃ at the stirring speed of 150r/min for reacting for 1 h; obtaining a reaction solution with the pH value of 2, wherein the concentration of hydrochloric acid in the reaction solution cannot be too high, so that the phenomenon that the too high concentration of hydrochloric acid reacts with manganese elements to influence the content of the manganese elements in the manganese concentrate is avoided;
(2) after the reaction is finished, filtering the reaction solution to obtain filtrate and filter residue; the main component of the obtained filtrate is calcium chloride, and the main component of the obtained filter residue is manganese concentrate;
(3) cleaning and drying filter residues to obtain manganese concentrate;
(4) adding sulfuric acid into the filtrate, wherein the adding amount of the sulfuric acid is 85% of the amount of the sulfuric acid required by complete precipitation of calcium ions contained in the filtrate, ensuring that the concentration of the calcium ions in the reaction solution is 25g/L during reaction (the amount of the sulfuric acid is adjusted, the added sulfuric acid is diluted by water for convenient adjustment, and the volume ratio of the sulfuric acid to the water is 1: 2), reacting by using a hydrothermal method, reacting for 3 hours at the temperature of 125 ℃ to obtain calcium sulfate hemihydrate whiskers, heating to 170 ℃, continuing to react for 2 hours, and filtering to obtain a hydrochloric acid solution and the calcium sulfate whiskers after the reaction is finished.
EXAMPLE III
A method for leaching manganese concentrate from low-grade manganite and regenerating leaching medium comprises the following steps:
(1) crushing low-grade manganite containing 15% of manganese element into particles with the diameter less than 2mm, and immersing the crushed low-grade manganite particles into a hydrochloric acid solution, wherein the weight ratio of the low-grade manganite particles to the hydrochloric acid in the reaction solution is 1: 3, stirring the reaction solution at the temperature of 50 ℃ at the stirring speed of 200r/min for reaction for 2 hours; obtaining reaction liquid with the pH value of 3, wherein the concentration of hydrochloric acid in the reaction liquid cannot be too high, so that the phenomenon that the too high concentration of hydrochloric acid reacts with manganese elements to influence the content of the manganese elements in the manganese concentrate is avoided;
(2) after the reaction is finished, filtering the reaction solution to obtain filtrate and filter residue; the main component of the obtained filtrate is calcium chloride, and the main component of the obtained filter residue is manganese concentrate;
(3) cleaning and drying filter residues to obtain manganese concentrate;
(4) adding sulfuric acid into the filtrate, wherein the adding amount of the sulfuric acid is 90% of the amount of the sulfuric acid required by complete precipitation of calcium ions contained in the filtrate, ensuring that the concentration of the calcium ions in the reaction solution is 50g/L during reaction (the amount of the sulfuric acid is adjusted, the added sulfuric acid is diluted by water for convenient adjustment, and the volume ratio of the sulfuric acid to the water is 1: 5), reacting by using a hydrothermal method, reacting for 4 hours at the temperature of 130 ℃ to obtain calcium sulfate hemihydrate whiskers, heating to 180 ℃, continuing to react for 2 hours, and filtering to obtain a hydrochloric acid solution and the calcium sulfate whiskers after the reaction is finished.
Example four
A method for leaching manganese concentrate from low-grade manganite and regenerating leaching medium comprises the following steps:
(1) crushing low-grade manganite containing 20% of manganese element into particles with the diameter less than 2mm, and immersing the crushed low-grade manganite particles into a hydrochloric acid solution, wherein the weight ratio of the low-grade manganite particles to the hydrochloric acid in the reaction solution is 1: 2, stirring the reaction solution at the temperature of 100 ℃ at the stirring speed of 300r/min for reaction for 3 hours; obtaining a reaction solution with the pH value of 4, wherein the concentration of hydrochloric acid in the reaction solution cannot be too high, so that the phenomenon that the too high concentration of hydrochloric acid reacts with manganese elements to influence the content of the manganese elements in the manganese concentrate is avoided;
(2) after the reaction is finished, filtering the reaction solution to obtain filtrate and filter residue; the main component of the obtained filtrate is calcium chloride, and the main component of the obtained filter residue is manganese concentrate;
(3) cleaning and drying filter residues to obtain manganese concentrate;
(4) adding sulfuric acid into the filtrate, wherein the adding amount of the sulfuric acid is 95% of the amount of the sulfuric acid required by complete precipitation of calcium ions contained in the filtrate, ensuring that the concentration of the calcium ions in the reaction solution is 60g/L during reaction (the amount of the sulfuric acid is adjusted, the added sulfuric acid is diluted by water for convenient adjustment, and the volume ratio of the sulfuric acid to the water is 1: 10), reacting by using a hydrothermal method, reacting for 5 hours at the temperature of 140 ℃ to obtain calcium sulfate hemihydrate whiskers, heating to 200 ℃, continuing to react for 3 hours, and filtering to obtain a hydrochloric acid solution and the calcium sulfate whiskers after the reaction is finished.
The present invention is not limited to the above-described preferred embodiments, and various other forms of the product can be obtained by anyone who has come within the teachings of the present invention, but any variation in the details thereof, which is the same as or similar to the present application, falls within the scope of the present invention.
Claims (6)
1. A method for leaching manganese concentrate from low-grade manganite and regenerating a leaching medium is characterized by comprising the following steps of:
(1) crushing low-grade manganosite, and soaking the crushed low-grade manganosite particles into a hydrochloric acid solution for reaction;
(2) after the reaction is finished, filtering the reaction solution to obtain filtrate and filter residue;
(3) cleaning and drying filter residues to obtain manganese concentrate;
(4) adding sulfuric acid into the filtrate, controlling the concentration of calcium ions in the reaction solution to be 5-60 g/L, then reacting by adopting a hydrothermal method, reacting for 3-5 h at the temperature of 125-140 ℃ to obtain calcium sulfate hemihydrate whiskers, heating to the temperature of 170-200 ℃, continuing to react for 2-3 h to obtain anhydrous calcium sulfate whiskers, and filtering to obtain a hydrochloric acid solution and calcium sulfate whiskers after the reaction is finished;
the added sulfuric acid is sulfuric acid diluted by water; and the volume ratio of the sulfuric acid to the water is as follows: 1: 2-1: 10, the addition amount of the sulfuric acid is 85 to 100 percent of the amount of the sulfuric acid required by the complete precipitation of the calcium ions contained in the filtrate.
2. The method for leaching manganese concentrate from low-grade manganite and regenerating leaching media according to claim 1, wherein in the step (1), the content of manganese element in the low-grade manganite is 10-20%; the particle size of the low-grade manganosite particles is less than 2 mm.
3. The method for leaching manganese concentrate from low-grade manganite and regenerating leaching medium according to claim 1, wherein in the step (1), the pH of the solution after reaction is 2-4.
4. The method for leaching manganese concentrate from low-grade manganosite and regenerating leaching media according to claim 1, wherein in the step (1), the weight ratio of low-grade manganosite particles to hydrochloric acid in the reaction solution is 1: 4-1: 2.
5. the method for leaching manganese concentrate from low-grade manganite and regenerating leaching medium according to claim 1, wherein the reaction temperature in the step (1) is 20-100 ℃.
6. The method for leaching manganese concentrate from low-grade manganite and regenerating leaching medium according to claim 1, wherein in the step (1), the stirring speed of stirring reaction is 150-300 r/min, and the reaction time is 1-3 h.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102050495A (en) * | 2009-11-10 | 2011-05-11 | 沈新财 | Process for preparing tetrahydrate manganese chloride by leaching out rhodochrosite with waste acid |
| CN102181627A (en) * | 2011-04-28 | 2011-09-14 | 昆明理工大学 | Method for treating primary low-grade high-phosphorus manganese ore by acid blending curing |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102050495A (en) * | 2009-11-10 | 2011-05-11 | 沈新财 | Process for preparing tetrahydrate manganese chloride by leaching out rhodochrosite with waste acid |
| CN102181627A (en) * | 2011-04-28 | 2011-09-14 | 昆明理工大学 | Method for treating primary low-grade high-phosphorus manganese ore by acid blending curing |
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| Title |
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| 废盐酸浸出菱锰矿扩大试验及除钙工艺优化;李军旗等;《稀有金属》;20120531;第36卷(第3期);473-475 * |
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