CN115432714A - Comprehensive utilization method of electrolytic manganese slag and demanganization building material - Google Patents
Comprehensive utilization method of electrolytic manganese slag and demanganization building material Download PDFInfo
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- CN115432714A CN115432714A CN202211364977.2A CN202211364977A CN115432714A CN 115432714 A CN115432714 A CN 115432714A CN 202211364977 A CN202211364977 A CN 202211364977A CN 115432714 A CN115432714 A CN 115432714A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/022—Preparation of aqueous ammonia solutions, i.e. ammonia water
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
- C04B11/26—Calcium sulfate cements strating from chemical gypsum; starting from phosphogypsum or from waste, e.g. purification products of smoke
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D1/00—Fertilisers containing potassium
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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
- C22B47/00—Obtaining manganese
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G1/00—Mixtures of fertilisers belonging individually to different subclasses of C05
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Ceramic Engineering (AREA)
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- Processing Of Solid Wastes (AREA)
- Fertilizers (AREA)
Abstract
The invention relates to a comprehensive utilization technology of industrial solid wastes, in particular to a comprehensive utilization method of electrolytic manganese slag and a demanganization building material. The method comprises the following steps: s1, desalting electrolytic manganese slag; s2, deaminating the desalted manganese slag; s3, selecting manganese from the deamination manganese slag; s4, preparing the building material by using the demanganized slag. The invention adopts the modes of water washing desalination, alkaline volatilization and wet magnetic separation to remove ammonia, and can simultaneously recover ammonia, magnesium and manganese in the electrolytic manganese slag. Meanwhile, the building material is prepared from the demanganized waste residues, calcium sulfate in the electrolytic manganese residues is fully utilized, the electrolytic manganese residue building material is prepared by adopting a super-sulfate cement principle, and zero emission of the electrolytic manganese residues is realized.
Description
Technical Field
The invention relates to a comprehensive utilization technology of industrial solid wastes, in particular to a comprehensive utilization method of electrolytic manganese residues and a demanganization building material.
Background
Electrolytic manganese slag is generated in the process of producing electrolytic manganese metal by utilizing manganese carbonate ore. It is investigated that 7-9t of electrolytic manganese slag is produced per 1t of electrolytic manganese metal produced. In the current stage, manganese slag is stockpiled by adopting a damming wet method, so that not only is the land occupied, but also heavy metals and the like are easy to permeate into soil, underground water and surface water and finally enter human bodies under the action of a food chain, and serious environmental pollution and potential safety hazards exist. Therefore, the harmlessness and reclamation of the manganese slag are necessary and urgent.
The manganese oxide content of the electrolytic manganese slag is generally about 10-14%, and the electrolytic manganese slag has high manganese content. Along with the increase of the price of manganese, the value of manganese in the original waste electrolytic manganese slag is greatly increased, and the method has important economic significance if the manganese can be recycled. The electrolytic manganese slag belongs to II-class industrial solid wastes, and Mn is also the most main pollutant in the electrolytic manganese slag. Therefore, manganese is a resource and a pollution source, ideal treatment is carried out on the manganese slag, and good economic and environmental significance is achieved.
Disclosure of Invention
Aiming at the problem that the manganese slag in the prior art is not well utilized, the invention provides a comprehensive utilization method of electrolytic manganese slag, which comprises the following steps:
s1, electrolytic manganese slag desalination: dissolving electrolytic manganese slag in water, fully stirring and performing solid-liquid separation to obtain desalted manganese slag and a salt solution;
s2, deamination of the desalted manganese slag: drying the desalted manganese slag to obtain a desalted manganese slag dry material, adding 1-5% of calcium oxide and 5-15% of water into the desalted manganese slag dry material, and fully stirring to volatilize ammonia gas to obtain deaminated manganese slag;
s3, manganese is selected from the deamination manganese slag: adding water into the deamination manganese slag to fully disperse the deamination manganese slag in the water, performing wet magnetic separation by using a magnetic separator to obtain high-manganese magnetic slag and demanganization slurry, and performing solid-liquid separation on the demanganization slurry to obtain demanganization slag and filtrate;
s4, preparing the building material by using the demanganized slag: and adding calcium oxide, micro powder and water into the demanganized slag, uniformly stirring, and forming to obtain the demanganized building material.
If the manganese is removed by a magnetic separation method to prepare the building material, the manganese slag needs to be dissolved in a large amount of water for magnetic separation. In the case of a large amount of soluble salts, the effect of magnetic manganese separation is affected, and the release of ammonia gas in the magnetic separation process is caused by the presence of ammonium, so that the salts and the ammonia gas are removed in advance. If the ammonia gas is removed first and then the salt is removed, the pH value of the solution is increased after the ammonia gas is removed, and the precipitation of the salts such as magnesium hydroxide is easily caused. If other alkaline substances are added to remove ammonia in the ammonia removal process, salt is easily introduced into the solution, after calcium oxide is used for removal, extra salt ions are not introduced and generate heat, ammonia removal is facilitated, and the calcium ions can also be used as a raw material for subsequently preparing building materials. In addition, when the calcium ions are added within the range of 1-5%, ammonia gas can be removed, the solution viscosity cannot be increased due to the addition of calcium oxide, and the magnetic separation effect cannot be influenced.
Preferably, in the step S1, the salt solution is evaporated to dryness to obtain a crude compound mineral fertilizer. The salt solution contains abundant magnesium ions, calcium ions, potassium ions and the like, and can be used as a raw material for preparing the fertilizer.
Preferably, in the step S1, the mass ratio of the electrolytic manganese slag to the water is 1:5 to 10. Under the dosage, not only can salt ions be fully dissolved out, but also the concentration of the salt solution can be ensured, and the subsequent evaporation cost is reduced.
Preferably, in the step S2, the addition amount of the water is 5 to 15 percent of the mass of the manganese slag desalination. Adding 5-15% of water to fully mix the calcium oxide with the desalted manganese slag, transferring the residual ammonia salt into a liquid phase, and adding water to make the calcium oxide be alkaline and generate heat, thereby being beneficial to ammonia removal.
Preferably, in the step S2, the ammonia gas volatilized is introduced into water to prepare ammonia water. The prepared ammonia water can be further used as an industrial raw material.
Preferably, in step S3, the weight ratio of the deaminated manganese slag to water is 1:2 to 5. The deamination manganese slag can be fully dispersed in water by adding the water with the dosage, which is beneficial to magnetic separation.
Preferably, in the step S3, the filtrate is returned to the wet magnetic separation for recycling, so that process water can be reduced.
Preferably, in the step S4, the weight ratio of the demanganized slag to the calcium oxide to the micro powder to the water is 1:0.5-1.5:0.1-0.2:0.8 to 1.5. The baking-free brick building material with excellent performance can be prepared in the range.
Preferably, the demanganized building material is obtained after forming by a pulp flow method or a semi-dry method and curing in the step S4.
Preferably, the electrolytic manganese slag contains 7-11% of manganese, 15-40% of calcium sulfate and 0.5-3% of ammonia by mass.
The invention also protects the demanganized building material prepared by the method of the invention.
The invention has the following beneficial effects:
the method ideally realizes the recovery of manganese in the electrolytic manganese slag waste, the manganese enrichment ratio of wet magnetic separation is high, and the manganese in the magnetic slag can reach more than 20%. Meanwhile, ammonia and magnesium in the electrolytic manganese slag can be recovered simultaneously by adopting water washing desalination and alkaline volatilization and deamination by wet magnetic separation, and recycling of ammonia, magnesium and manganese is realized simultaneously.
Furthermore, the invention fully utilizes calcium sulfate in the electrolytic manganese slag, adopts the super-sulfate cement principle to prepare the electrolytic manganese slag building material, and realizes zero emission of the electrolytic manganese slag. The method effectively solves the problem of recycling the electrolytic manganese slag, is simple to operate, can recover ammonia and manganese, and can obtain good economic benefit and ecological benefit.
Drawings
FIG. 1 is an overall process flow diagram of the present invention;
FIG. 2 shows the main components of a crude compound mineral fertilizer;
FIG. 3 is an XRD spectrum of the deaminated slag;
FIG. 4 is an experimental test block prepared using demanganized slag.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
The embodiment relates to a comprehensive utilization method of electrolytic manganese slag, which comprises the following steps (figure 1 is a general process flow chart of the invention):
s1: desalting electrolytic manganese slag: 100kg of water is added into 20kg of electrolytic manganese slag, and after fully stirring for 15 minutes, the mixture is filtered to obtain 16.2kg of desalted manganese slag and salt solution. The salt solution was evaporated to dryness to obtain 3.8kg of crude compound mineral fertilizer. The crude compound mineral fertilizer is detected to be free of heavy metals, and the main substances comprise magnesium ammonium sulfate hexahydrate (magnesium ammonium sulfate), magnesium sulfate, potassium (or sodium) manganese sulfate, gypsum (calcium sulfate) and the like, and the main component diagram of the crude compound mineral fertilizer is shown in figure 2.
S2: and (3) deaminating the desalted manganese slag: and (2) after drying the desalted manganese slag obtained in the step (S1), adding 0.3kg of quicklime and 1kg of water into 10kg of desalted manganese slag dry material, and stirring for 10 minutes to volatilize ammonia gas so as to obtain deamination slag (the XRD pattern of which is shown in figure 3). The ammonia gas removed is purified water as an absorption liquid to obtain ammonia water. As can be seen from the XRD pattern of the deamination slag, no ammonia salt can be basically detected in the slag.
S3: magnetic separation of manganese-rich magnetic slag: adding 30kg of water into 10kg of deamination slag to fully disperse electrolytic manganese slag into the water, respectively carrying out magnetic separation by using a 12000Gs industrial magnetic separator to obtain high-manganese magnetic slag and demanganization slurry, carrying out solid-liquid separation on the demanganization slurry to obtain demanganization slag and filtrate, and returning the filtrate to wet magnetic separation for recycling.
S4: preparing a building material by using the demanganized slag: adding quicklime, micro powder and water into the demanganized slag, uniformly stirring, wherein 100 parts of demanganized slag, 137.5 parts of micro powder, 16.5 parts of quicklime and 127 parts of water are formed by adopting a pulp flow method, and curing to obtain the electrolytic manganese slag building material for preparing the building product, wherein the appearance figure of the building product is shown in figure 4.
Example 2
Compared with the embodiment 1, the difference is that 7500Gs industrialized magnetic field is adopted for magnetic separation in the step S3.
Example 3
Compared with the embodiment 1, the difference is that in the step S4, 125 parts of demanganized slag, 112.5 parts of micro powder, 17.5 parts of quicklime and 127.5 parts of water are used.
Example 4
Compared with the embodiment 1, the difference is that in the step S4, 150 parts of demanganized slag, 87.5 parts of micro powder, 18.5 parts of quicklime and 128 parts of water are used.
Example 5
The difference from example 1 is that the amount of quicklime added in step S2 was 0.1kg.
Example 6
The difference from example 1 is that the amount of quicklime added in step S2 was 0.5kg.
Comparative example 1
The difference from example 1 is that the amount of quicklime added in step S2 was 1kg.
Comparative example 2
Compared with the embodiment 1, the difference is that in the step S4, 175 parts of demanganized slag, 62.5 parts of micro powder, 19.5 parts of quicklime and 128.5 parts of water are used.
Comparative example 3
Compared with the embodiment 1, the difference is that in the step S4, 200 parts of demanganized slag, 37.5 parts of micro powder, 20.5 parts of quicklime and 129 parts of water are used.
Examples of the experiments
The components of the manganese-enriched high-manganese magnetic slag obtained in step S3 were analyzed, and the results are shown in table 1.
TABLE 1
From the table above, the manganese content in the high-manganese magnetic slag obtained by magnetic separation can reach more than 21%, and the high-manganese magnetic slag can be sold as manganese powder ore and used for preparing metal manganese or manganese sulfate. In comparative example 1, since a large amount of calcium oxide was added, the liquid in step S3 was extremely viscous and magnetic separation could not be smoothly performed, and comparative example 2 and comparative example 3 gave the same results as in example 1.
TABLE 2
The compressive strength of the demanganized building material was measured and the results are shown in table 3:
TABLE 3
Toxicity leaching experiments were performed on the demanganized building materials of examples 1 to 6 according to the solid waste related toxicity leaching standard "horizontal oscillatory method for leaching toxicity leaching method of solid waste (HJ 557-2010)". The leaching toxicity of the heavy metal and the manganese can reach the standard of surface water III. The leaching amount of ammonia nitrogen can reach the III-class standard of surface water, and the method has good environmental safety.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (9)
1. The comprehensive utilization method of the electrolytic manganese slag is characterized by comprising the following steps of:
s1, electrolytic manganese slag desalination: dissolving electrolytic manganese slag in water, fully stirring and carrying out solid-liquid separation to obtain desalted manganese slag and a salt solution;
s2, deamination of the desalted manganese slag: drying the desalted manganese slag to obtain a desalted manganese slag dry material, adding 1-5% of calcium oxide and 5-15% of water into the desalted manganese slag dry material, and fully stirring to volatilize ammonia gas to obtain deaminated manganese slag;
s3, selecting manganese from the deamination manganese slag: adding water into the deamination manganese slag to fully disperse the deamination manganese slag in the water, performing wet magnetic separation by using a magnetic separator to obtain high-manganese magnetic slag and demanganized slurry, and performing solid-liquid separation on the demanganized slurry to obtain demanganized slag and filtrate;
s4, preparing the building material by using the demanganized slag: and adding calcium oxide, micro powder and water into the demanganized slag, uniformly stirring, and forming to obtain the demanganized building material.
2. The utilization method according to claim 1, wherein in the step S1, the salt solution is evaporated to dryness to obtain the crude composite mineral fertilizer.
3. The utilization method according to claim 1 or 2, wherein in the step S1, the mass ratio of the electrolytic manganese slag to the water is 1:5 to 10.
4. The utilization method according to claim 1, wherein in the step S2, ammonia gas volatilized is introduced into water to prepare ammonia water.
5. The utilization method of claim 1, wherein in the step S3, the mass ratio of the deaminated manganese slag to water is 1:2 to 5.
6. The utilization method according to claim 1, wherein in the step S3, the filtrate is returned to wet magnetic separation for recycling.
7. The utilization method according to claim 1, wherein in the step S4, the mass ratio of the demanganized slag to the calcium oxide to the micro powder to the water is 1:0.5-1.5:0.1-0.2:0.8 to 1.5.
8. The utilization method of claim 1, wherein the step S4 is performed by a slurry flow method or a semi-dry method, and the demanganized building material is obtained after curing.
9. A demanganized building material, characterized in that it is obtained by the process according to any one of claims 1 to 8.
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Cited By (1)
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| CN117024098A (en) * | 2023-08-14 | 2023-11-10 | 北京建工环境修复股份有限公司 | Electrolytic manganese slag hydrothermal self-curing building material and preparation method thereof |
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