CN113666400A - Fine purification process of boron-magnesium mine tailing slag - Google Patents
Fine purification process of boron-magnesium mine tailing slag Download PDFInfo
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- CN113666400A CN113666400A CN202110965973.9A CN202110965973A CN113666400A CN 113666400 A CN113666400 A CN 113666400A CN 202110965973 A CN202110965973 A CN 202110965973A CN 113666400 A CN113666400 A CN 113666400A
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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
- C01F5/24—Magnesium carbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/10—Preparation of bicarbonates from carbonates
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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
- C01F5/40—Magnesium sulfates
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
Abstract
The invention relates to boron mud processing, which belongs to the field of mineral refining processing, and discloses a fine purification process of boron-magnesium ore tailing slag. According to the process, boron and magnesium elements are purified in batches after boron mud is solidified, impurities such as silicon and the like are retained in a wetting column, and extraction of magnesium and separation of slag are realized by a one-step method; and the acid and alkali are purified step by step and then the filtrate is neutralized, so that the waste discharge amount is reduced to zero. The process directly adopts the slime of boron-magnesium ore refinery, not only solves the pollution problem of boron slime, but also solves the raw material source problem of magnesium. Meanwhile, the energy consumption step of preprocessing the moisture of the slime in other processes is solved by adding materials such as bentonite and the like in the process.
Description
Technical Field
The invention relates to mineral processing, in particular to a fine purification process of boron-magnesium mine tailing slag.
Background
Ascharite (ashalite) is a borate mineral, which is the main mineral from which industrial boron is extracted. Borax is generally associated with minerals such as magnetite and their shadows are visible in magnesium sunscreens. The ludwigite is white or grey and yellowish, the crystals of the ludwigite can be in a fiber shape, a column shape or a plate shape, the crystals can be in a fiber shape or a block shape when being gathered together, but the block-shaped ludwigite has dull luster and does not give out silk-like luster like the fiber-shaped ludwigite. The method is mainly used for producing boric acid, borax, boron compounds and the like, and the boromagnesite is easy to smelt, is a main source of boron and is a mineral raw material for refining boron. The boron-magnesium stone mineral after purification by adopting the processes of carbon-alkali method and the like is converted into industrial waste residue boron mud.
The boric sludge is waste residue generated in the production of boric acid, borax and other products, is offwhite and yellowish white powdery solid, is alkaline, contains boron oxide, magnesium oxide and other components, and is commonly called as boric sludge. The stockpiling and disposal of the boric sludge not only occupies a large amount of land, but also can alkalize soil near a storage yard and cause migration and transformation of boron, thereby causing environmental pollution. The boron mud has the main chemical composition of MgO and SiO2, and contains certain amounts of Fe2O3, B2O3, small amounts of CaO, Al2O3 and the like. Boron is present in trace amounts therein and does not form a separate boron-containing mineral.
The water content of the boric sludge discharged by a factory in a wet discharging mode is about 30-35%, the boric sludge is a sludge-like substance, the boric sludge is dark brown when being wet, the granularity is fine, the boric sludge has better plasticity, and the boric sludge is formed into sludge blocks after being dried, but is extremely easy to crush and grind. In the prior art, boron mud waste is generally roasted, and then acidolysis or alkali treatment is carried out to extract elements such as magnesium, but a large amount of high-temperature heat is consumed during roasting, so that the recycling cost of the boron mud is greatly improved, the whole purification process becomes a non-economic industry with high energy consumption, high pollution and low yield, and the boron mud waste belongs to a production process strictly prohibited by governments in many areas and even boron mine areas. Under the condition, the recycling process of the boron mud faces great environmental pressure and cost pressure, the boron mud is strong in alkalinity, and the problem that the boron mud pollutes the environment cannot be solved due to simple stacking and burying.
Therefore, the process for purifying the boron mud with low energy consumption, high efficiency and low cost is urgently needed by the current boron mud waste mineral recycling industry.
Disclosure of Invention
The invention aims to solve the technical problem of providing a fine purification process of boron-magnesium ore tailing slag, and solves the problems of high energy consumption, heavy pollution, high cost and no support by national policies in the existing boron mud recycling process.
Technical scheme
A fine purification process of boron-magnesium mine tailing slag is characterized by comprising the following steps:
a. mixing bentonite and fine quartz sand into boric sludge discharged from the ascharite, and granulating to obtain mineral particles;
b. curing the mineral particle shell at high temperature;
c. compacting the solidified mineral particles, filling the compacted mineral particles into a leaching tank for leaching, leaching with weak alkali solution to remove boron-aluminum impurities in the mineral particles, and leaching with acid solution to extract magnesium-containing solution.
Further, the leaching step specifically comprises:
I. leaching with clear water, and soaking the mineral particles;
II. Soaking and leaching residual boron and active aluminum impurities by using a weak alkali solution to obtain an alkaline leaching solution;
III, soaking in an acid solution to obtain an acidic magnesium-containing solution, adding sodium carbonate to precipitate magnesium carbonate, and filtering to obtain a magnesium carbonate solid and a sodium carbonate solution;
IV, introducing carbon dioxide into the alkaline leacheate to precipitate flocculent aluminum hydroxide and boric acid precipitate adsorbed by the flocculent precipitate, and filtering to obtain a carbonic acid water solution;
and V, using the carbonic acid aqueous solution obtained in the step IV for neutralizing the sodium carbonate aqueous solution obtained in the step III to obtain a sodium bicarbonate aqueous solution.
Further, the water content of the boron mud is 20-40%, and the bentonite is 0.2-0.8% of the water content of the boron mud;
further, the particle size of the mineral particles is 2-5 mm;
further, the particle size of the fine quartz sand is 0.1-0.5 mm;
further, the fine quartz sand accounts for 5% -10% of the solid content of the boric sludge;
further, the high-temperature curing temperature of the mineral particles is 400-450 ℃;
further, the weak base is selected from a sodium hydroxide aqueous solution with the pH value of 8.0-9.5; the acid solution is selected from aqueous sulfuric acid;
further, the soaking time of the clean water in the step I is 20-60 min;
further, the high-temperature curing time of the mineral particles is 1-5 min.
Advantageous effects
The fine purification process of the boron-magnesium ore slag comprises the following steps:
1. boron mud is solidified and then purified with boron and magnesium elements in batches, impurities such as silicon and the like are left in a soaking column, and the extraction of magnesium and the separation of slag are realized by a one-step method;
2. in the process, acid and alkali are purified step by step and then are neutralized, the waste discharge is reduced to zero, the concentrated boron element is returned to a boron-magnesium ore smelting plant while magnesium carbonate is produced, and byproducts such as sodium bicarbonate and the like are produced;
3. the process directly adopts the slime of the boron-magnesium ore refinery, not only solves the pollution problem of the boron slime, but also solves the raw material source problem of magnesium;
4. the process solves the energy consumption step of preprocessing the moisture of the slime in other processes by adding materials such as bentonite and the like;
5. the process obtains the infiltration particles by rapid skin sintering, thereby avoiding time-consuming and complex processes such as slurry treatment and the like in charge of the conventional extraction process;
6. residual slime in the leaching tank is used as a raw material to prepare the steam brick, so that zero pollution emission in the whole process is realized.
Drawings
FIG. 1 is a schematic diagram of a refining process according to the present invention;
FIG. 2 is a diagram of a boron mud slurry of the present invention;
FIG. 3 is a diagram of a magnesium carbonate refining product according to the present invention.
Detailed Description
The present invention will be further described with reference to specific examples 1 to 5 and accompanying drawings 1 to 3.
The invention provides a fine purification process of boron-magnesium mine tailing slag, which is directly connected with a mineral refinery generating boron mud in the industry, and the boron mud slurry originally removed from waste slag is used for extracting magnesium.
Example 1
The discharged boron mud slurry is directly obtained from the periphery of the boron magnesium ore refinery, and the water content is about 30 percent. Then adding 5% of quartz sand, simultaneously mixing 0.24% of sodium bentonite, reducing the free water content in the slurry, improving the viscosity of the slurry, then directly introducing the slurry into a granulator after uniformly mixing and stirring to obtain mineral particles with the particle size of 5 mm. And then drying the mineral particles, and curing at 450 ℃ for 3min to solidify the mineral outer skins, improve the structural strength of the mineral particles and prevent pulverization in the soaking process.
Then pouring the mineral particles into a leaching tank, gradually injecting clear water from the upper layer to soak for 60min, then discharging the leachate, then filling clear water from the upper layer of the particles again, then gradually injecting a sodium hydroxide aqueous solution (pH 9.5) into the upper layer, soaking for 60min and then discharging, soaking and leaching the boron and active aluminum impurities remained in the mineral particles by using a weak alkali solution, returning the impurities to a boromagnesite ore plant for refining again, and simultaneously obtaining an alkaline leaching solution;
introducing excessive carbon dioxide into the alkaline leacheate to precipitate a small amount of solid matters such as silicic acid, aluminum hydroxide and the like, and filtering to obtain a carbonic acid aqueous solution;
and then, soaking in clear water again, discharging, pouring clear water, injecting a sulfuric acid solution, and soaking for 30min to obtain a magnesium sulfate aqueous solution.
Adding excessive sodium carbonate into magnesium sulfate solution, precipitating, and filtering to obtain magnesium carbonate product; and neutralizing the residual mixed filtrate of sodium sulfate and sodium carbonate with a carbonic acid aqueous solution to obtain a sodium bicarbonate and sodium sulfate aqueous solution for other industrial production, and preparing the residual slime in the leaching tank into a steam brick as a raw material to realize zero pollution emission in the whole process.
Example 2
The discharged boron mud slurry is directly obtained from the periphery of the boron magnesium ore refinery, and the water content is about 30 percent. Then 4.5 percent of quartz sand is added, 0.2 percent of sodium bentonite is mixed at the same time, the free water content in the slurry is reduced, the viscosity of the slurry is improved, and then the slurry is directly introduced into a granulator after being uniformly mixed and stirred, so as to obtain mineral particles with the particle size of 4 mm. And then drying the mineral particles, and curing at 450 ℃ for 5min to solidify the mineral outer skins, improve the structural strength of the mineral particles and prevent pulverization in the soaking process.
Then pouring the mineral particles into a leaching tank, gradually injecting clear water from the upper layer to soak for 50min, then discharging the leachate, then filling clear water from the upper layer of the particles, then gradually injecting a sodium hydroxide aqueous solution (pH 9.0) into the upper layer, soaking for 50min, then discharging, and soaking and leaching the boron and active aluminum impurities remained in the mineral particles by using a weak base solution to obtain an alkaline leaching solution;
introducing excessive carbon dioxide into alkaline leacheate to precipitate a small amount of solid matters such as silicic acid, aluminum hydroxide and the like, and filtering to obtain a carbonic acid aqueous solution
And then, soaking in clear water again, discharging, pouring clear water, injecting a sulfuric acid solution, and soaking for 20min to obtain a magnesium sulfate aqueous solution.
Adding excessive sodium carbonate into magnesium sulfate solution, precipitating, and filtering to obtain magnesium carbonate product; and neutralizing the residual mixed filtrate of sodium sulfate and sodium carbonate with a carbonic acid aqueous solution to obtain a sodium bicarbonate and sodium sulfate aqueous solution for other industrial production, and preparing the residual slime in the leaching tank into a steam brick as a raw material to realize zero pollution emission in the whole process.
Example 3
The discharged boron mud slurry is directly obtained from the periphery of the boron magnesium ore refinery, and the water content is about 30 percent. Then 3.8 percent of quartz sand is added, 0.12 percent of sodium bentonite is mixed at the same time, the free water content in the slurry is reduced, the viscosity of the slurry is improved, and then the slurry is directly introduced into a granulator after being uniformly mixed and stirred, so as to obtain mineral particles with the particle size of 3 mm. And then drying the mineral particles, and curing at the high temperature of 420 ℃ for 1min to solidify the mineral outer skin, improve the structural strength of the mineral particles and prevent pulverization in the soaking process.
Then pouring the mineral particles into a leaching tank, gradually injecting clear water from the upper layer to soak for 30min, then discharging the leachate, then filling clear water from the upper layer of the particles, then gradually injecting a sodium hydroxide aqueous solution (pH 8.5) into the upper layer, soaking for 20min, then discharging, and soaking and leaching the boron and active aluminum impurities remained in the mineral particles by using a weak base solution to obtain an alkaline leaching solution;
introducing excessive carbon dioxide into the alkaline leacheate to precipitate a small amount of solid matters such as silicic acid, aluminum hydroxide and the like, and filtering to obtain a carbonic acid aqueous solution;
and then, soaking in clear water again, discharging, pouring clear water, injecting a sulfuric acid solution, and soaking for 20min to obtain a magnesium sulfate aqueous solution.
Adding excessive sodium carbonate into magnesium sulfate solution, precipitating, and filtering to obtain magnesium carbonate product; and neutralizing the residual mixed filtrate of sodium sulfate and sodium carbonate with a carbonic acid aqueous solution to obtain a sodium bicarbonate and sodium sulfate aqueous solution for other industrial production, and preparing the residual slime in the leaching tank into a steam brick as a raw material to realize zero pollution emission in the whole process.
Example 4
The discharged boron mud slurry is directly obtained from the periphery of the boron magnesium ore refinery, and the water content is about 30 percent. Then 3.5 percent of quartz sand is added, 0.1 percent of sodium bentonite is mixed at the same time, the free water content in the slurry is reduced, the viscosity of the slurry is improved, and then the slurry is directly introduced into a granulator after being uniformly mixed and stirred, so as to obtain mineral particles with the particle size of 2.5 mm. And then drying the mineral particles, and curing at 445 ℃ for 2min to solidify the mineral outer skin, improve the structural strength of the mineral particles and prevent pulverization in the soaking process.
Then pouring the mineral particles into a leaching tank, gradually injecting clear water from the upper layer to soak for 25min, then discharging the leachate, then filling clear water from the upper layer of the particles, then gradually injecting a sodium hydroxide aqueous solution (pH is 8.5) into the upper layer, soaking for 26min, then discharging, and soaking and leaching the boron and active aluminum impurities remained in the mineral particles by using a weak base solution to obtain an alkaline leaching solution;
introducing excessive carbon dioxide into alkaline leacheate to precipitate a small amount of solid matters such as silicic acid, aluminum hydroxide and the like, and filtering to obtain a carbonic acid aqueous solution
And then, soaking in clear water again, discharging, pouring clear water, injecting a sulfuric acid solution, and soaking for 20min to obtain a magnesium sulfate aqueous solution.
Adding excessive sodium carbonate into magnesium sulfate solution, precipitating, and filtering to obtain magnesium carbonate product; and neutralizing the residual mixed filtrate of sodium sulfate and sodium carbonate with a carbonic acid aqueous solution to obtain a sodium bicarbonate and sodium sulfate aqueous solution for other industrial production, and preparing the residual slime in the leaching tank into a steam brick as a raw material to realize zero pollution emission in the whole process.
Example 5
The discharged boron mud slurry is directly obtained from the periphery of the boron magnesium ore refinery, and the water content is about 30 percent. Then 3.5 percent of quartz sand is added, 0.06 percent of sodium bentonite is mixed at the same time, the free water content in the slurry is reduced, the viscosity of the slurry is improved, and then the slurry is directly introduced into a granulator after being uniformly mixed and stirred, so as to obtain mineral particles with the particle size of 2 mm. And then drying the mineral particles, and curing at the high temperature of 400 ℃ for 5min to solidify the mineral outer skins, improve the structural strength of the mineral particles and prevent pulverization in the soaking process.
Then pouring the mineral particles into a leaching tank, gradually injecting clear water from the upper layer to soak for 20min, then discharging the leachate, then filling clear water from the upper layer of the particles, then gradually injecting a sodium hydroxide aqueous solution (pH 8.0) into the upper layer, soaking for 20min, then discharging, and soaking and leaching the boron and active aluminum impurities remained in the mineral particles by using a weak base solution to obtain an alkaline leaching solution;
introducing excessive carbon dioxide into alkaline leacheate to precipitate a small amount of solid matters such as silicic acid, aluminum hydroxide and the like, and filtering to obtain a carbonic acid aqueous solution
And then, soaking in clear water again, discharging, pouring clear water, injecting a sulfuric acid solution, and soaking for 10min to obtain a magnesium sulfate aqueous solution.
Adding excessive sodium carbonate into magnesium sulfate solution, precipitating, and filtering to obtain magnesium carbonate product; and neutralizing the residual mixed filtrate of sodium sulfate and sodium carbonate with a carbonic acid aqueous solution to obtain a sodium bicarbonate and sodium sulfate aqueous solution for other industrial production, and preparing the residual slime in the leaching tank into a steam brick as a raw material to realize zero pollution emission in the whole process.
According to the embodiments 1-5 and the attached figure 1 of the specification, the process purifies the boron and magnesium elements in batches after the boron mud is solidified, impurities such as silicon and the like are retained in the infiltration column, and the extraction of magnesium and the separation of slag are realized by a one-step method; and the acid and alkali are purified step by step and then the filtrate is neutralized, so that the waste discharge is reduced to zero, the concentrated boron element is returned to a boron-magnesium ore smelting plant while magnesium carbonate is produced, and byproducts such as sodium bicarbonate and the like are produced. The process directly adopts the slime of boron-magnesium ore refinery, not only solves the pollution problem of boron slime, but also solves the raw material source problem of magnesium. Meanwhile, the energy consumption step of preprocessing the moisture of the slime in other processes is solved by adding materials such as bentonite and the like in the process. Secondly, infiltration particles are obtained through rapid surface sintering, time-consuming and complex processes such as slurry treatment and the like in charge of a conventional extraction process are avoided, and residual slime in a leaching tank is used as a raw material to prepare a steam brick, so that zero pollution emission in the whole process is realized.
Claims (10)
1. A fine purification process of boron-magnesium mine tailing slag is characterized by comprising the following steps:
a. mixing bentonite and fine quartz sand into boric sludge discharged from the ascharite, and granulating to obtain mineral particles;
b. curing the mineral particle shell at high temperature;
c. compacting the solidified mineral particles, filling the compacted mineral particles into a leaching tank for leaching, leaching with weak alkali solution to remove boron-aluminum impurities in the mineral particles, and leaching with acid solution to extract magnesium-containing solution.
2. The fine purification process of the boromagnesite tailing slag according to claim 1, wherein the leaching step specifically comprises:
I. leaching with clear water, and soaking the mineral particles;
II. Soaking and leaching residual boron and active aluminum impurities by using a weak alkali solution to obtain an alkaline leaching solution;
III, soaking in an acid solution to obtain an acidic magnesium-containing solution, adding sodium carbonate to precipitate magnesium carbonate, and filtering to obtain a magnesium carbonate solid and a sodium carbonate solution;
IV, introducing carbon dioxide into the alkaline leacheate to precipitate flocculent aluminum hydroxide and boric acid precipitate adsorbed by the flocculent precipitate, and filtering to obtain a carbonic acid water solution;
and V, using the carbonic acid aqueous solution obtained in the step IV for neutralizing the sodium carbonate aqueous solution obtained in the step III to obtain a sodium bicarbonate aqueous solution.
3. The fine purification process of the boron-magnesium mine tailing slag according to claim 1, wherein the water content of the boron mud raw material is 20-40%, and the water content of the bentonite is 0.2-0.8% of the water content of the boron mud.
4. The fine purification process of the boromagnesite tailing slag as claimed in claim 1, wherein the particle size of the mineral particles is 2-5 mm.
5. The fine purification process of the boromagnesite tailing slag as claimed in claim 1, wherein the particle size of the fine quartz sand is 0.1-0.5 mm.
6. The fine purification process of the boron magnesium ore tailing slag according to claim 1, wherein the fine quartz sand accounts for 5 to 10 percent of the solid content of the boron mud by mass.
7. The fine purification process of the boromagnesite tailing slag as claimed in claim 1, wherein the temperature of the mineral particles solidified at high temperature is 400-450 ℃.
8. The fine purification process of the boromagnesite tailing slag according to claim 2, wherein the weak base is selected from an aqueous sodium hydroxide solution with a pH of 8.0 to 9.5; the acid solution is selected from aqueous sulfuric acid.
9. The fine purification process of the boromagnesite tailing slag as claimed in claim 2, wherein the soaking time in clean water in the step I is 20-60 min.
10. The fine purification process of the boromagnesite tailing slag as claimed in the claim 1 to 9, wherein the time of high temperature solidification of the mineral particles is 1 to 5 min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114797754A (en) * | 2022-03-29 | 2022-07-29 | 常熟理工学院 | Method for preparing efficient wastewater adsorbent by using boron mud |
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| CN1130708A (en) * | 1995-03-07 | 1996-09-11 | 鞍山市精细化工研究开发中心筹备组 | Borax mud sintered brick without clay and manufacturing method thereof |
| JP2008272542A (en) * | 2006-08-03 | 2008-11-13 | Taiheiyo Cement Corp | Heavy metal elution preventing method for baked material and baked material for civil engineering material |
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| CN114797754A (en) * | 2022-03-29 | 2022-07-29 | 常熟理工学院 | Method for preparing efficient wastewater adsorbent by using boron mud |
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