CN111285526A - Method for treating magnesium-containing wastewater from nickel smelting - Google Patents
Method for treating magnesium-containing wastewater from nickel smelting Download PDFInfo
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- CN111285526A CN111285526A CN202010162916.2A CN202010162916A CN111285526A CN 111285526 A CN111285526 A CN 111285526A CN 202010162916 A CN202010162916 A CN 202010162916A CN 111285526 A CN111285526 A CN 111285526A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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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
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/02—Temperature
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/44—Time
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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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
Abstract
The invention provides a method for treating magnesium-containing wastewater from nickel smelting, which is characterized by comprising the following steps: adding sodium sulfide to precipitate heavy metal, introducing tail gas to remove manganese ions, adding magnesium oxide to further remove manganese ions, concentrating, and spray drying to obtain magnesium sulfate product. The method has the advantages of simple process flow, high production efficiency, small occupied area, low investment, high product purity, good quality and the like, and the problem of difficult treatment of magnesium-containing wastewater is fundamentally solved.
Description
Technical Field
The invention relates to a method for treating magnesium-containing wastewater, in particular to a method for treating nickel smelting magnesium-containing wastewater, and belongs to the technical field of magnesium-containing wastewater treatment.
Background
A large amount of magnesium-containing wastewater can be generated in the nickel smelting production process, and the treatment process of the magnesium-containing wastewater in the prior art comprises the following steps: the process comprises the following steps of concentration evaporation, crystallization, solid-liquid separation and drying, and has the following defects: the method has the advantages of long process flow, complex equipment structure, large occupied area, low production efficiency, large investment and low value of byproduct magnesium sulfate heptahydrate, and a large amount of magnesium-containing wastewater generated at the same time is directly discharged without being treated, thereby causing serious pollution to the environment. Therefore, the research and development of a new method which has simple flow, high production efficiency, high byproduct value, no pollution discharge and investment saving has important significance.
Disclosure of Invention
In order to solve the problem of high treatment difficulty of the traditional magnesium-containing wastewater, the invention provides the method for treating the magnesium-containing wastewater in nickel smelting, which not only solves the environmental protection problem of treating the magnesium-containing wastewater, but also generates economic benefits.
The invention is realized by the following technical scheme: a method for treating magnesium-containing wastewater from nickel smelting is characterized by comprising the following steps:
(1) adding sodium sulfide into the magnesium-containing wastewater from nickel smelting to precipitate heavy metals, wherein the addition amount of the sodium sulfide is 1.0-2.5 times of the amount of the heavy metals in the wastewater, reacting for 60-120 minutes at the temperature of 30-70 ℃ to convert the heavy metals into sulfide precipitates, and separating the heavy metal precipitates and magnesium-containing liquid from solid and liquid;
(2) introducing tail gas into the magnesium-containing liquid in the step (1), cooling the tail gas, introducing dust in the tail gas into the liquid, oxidizing bivalent manganese ions in the solution into high-valence manganese precipitates by using oxygen in the tail gas, and separating the manganese precipitates and the magnesium-containing liquid from solid and liquid;
(3) adding magnesium oxide into the magnesium-containing liquid obtained in the step (2) until the pH value of the liquid is 8.0-9.5, reacting for 60-150 minutes at the reaction temperature of 30-70 ℃ to oxidize divalent manganese ions in the magnesium-containing liquid into high-valence manganese precipitates, and separating the manganese precipitates and the magnesium-containing liquid from solid and liquid;
(4) evaporating and concentrating the magnesium-containing liquid obtained in the step (3) to obtain magnesium sulfate concentrated solution, and feeding the evaporated condensed water back to the nickel smelting process to be reused as process water;
(5) and (3) carrying out spray drying on the magnesium sulfate concentrated solution in the step (4) to obtain a magnesium sulfate product, and returning tail gas generated by spray drying to a nickel smelting process or the step (2) to be used as a heat source or an oxidant.
The magnesium-containing wastewater from nickel smelting in the step (1) is produced after purifying and removing impurities and depositing nickel in a nickel-containing ore wet nickel extraction process, or magnesium-containing wastewater generated after desulfurization in the industries of thermal power generation, steel, cement, petrifaction and the like, or magnesium-containing wastewater generated after evaporation or solarization concentration, wherein the concentration of magnesium sulfate in the magnesium-containing wastewater is 15-60%.
The effective content of the magnesium oxide added in the step (3) is 75-90%, the activity is 50-90, and the magnesium oxide is added to maintain the pH value of the magnesium-containing wastewater, so that manganese ions in the magnesium-containing liquid can be removed more effectively and more thoroughly.
The evaporation and concentration equipment in the step (4) is a conventional MVR evaporator or a multi-effect evaporator, negative-pressure countercurrent evaporation is adopted, the content of magnesium sulfate in the evaporation and concentration solution is 30-50%, and the temperature of the concentration solution is 70-110 ℃.
And (3) the spray drying in the step (5) is implemented by using conventional pressure type or centrifugal spray fluidized bed granulation drying equipment, the heat source is natural gas or high-temperature waste heat flue gas, and the hot air temperature is 250-450 ℃.
The magnesium sulfate product in the step (5) is magnesium sulfate monohydrate or anhydrous magnesium sulfate, and the bulk specific gravity is 0.2-1.2.
The invention has the advantages and effects that: by adopting the process method, not only can heavy metal ions be removed, but also the removal rate is high, impurities such as manganese and the like can be removed by utilizing heat energy and oxygen in industrial tail gas, the tail gas can be cooled and subjected to dust removal and purification treatment, the cost of additionally putting into dust removal equipment for tail gas treatment is saved, the process method is beneficial to environmental protection, the pH value of magnesium-containing waste water is maintained by adding magnesium oxide, the impurity ions are effectively removed, then magnesium-containing liquid is concentrated and dried, and finally a high-quality magnesium sulfate solid product is obtained.
Drawings
FIG. 1 is a process flow diagram of the present invention
Detailed Description
The invention is further illustrated by the following examples.
Example 1
The magnesium-containing wastewater treated by the embodiment is produced after purifying, impurity removing and nickel depositing in the process of extracting nickel from nickel-containing ore by a wet method, and the components of the magnesium-containing wastewater are shown in a table 1:
TABLE 1 magnesium-containing waste water composition g/L
| Mg | Ca | Fe | Na | Heavy metals (in Pb) | Mn | pH |
| 38.17 | 0.41 | 0.003 | 0.15 | 0.001 | 0.075 | 8.1 |
The method comprises the following steps:
(1) adding sodium sulfide into the magnesium-containing wastewater to precipitate heavy metals, wherein the addition amount of the sodium sulfide is 1.0 time of the amount of the heavy metals in the wastewater, reacting for 120 minutes at the temperature of 30 ℃ to convert the heavy metals into sulfide precipitates, and carrying out solid-liquid separation to obtain the heavy metal precipitates and a magnesium-containing liquid;
(2) introducing tail gas into the magnesium-containing liquid in the step (1), cooling the tail gas, introducing dust in the tail gas into the liquid, oxidizing bivalent manganese ions in the solution into high-valence manganese precipitates by using oxygen in the tail gas, and separating the manganese precipitates and the magnesium-containing liquid from solid and liquid;
(3) adding magnesium oxide with effective content of 90% and activity of 90% into the magnesium-containing liquid in the step (2) until the pH value of the liquid is 8.3, reacting for 150 minutes at the reaction temperature of 30 ℃ to oxidize bivalent manganese ions in the magnesium-containing liquid into high-valence manganese precipitates, and separating the manganese precipitates and the magnesium-containing liquid from solid and liquid, wherein the components of the magnesium-containing liquid are shown in Table 2:
TABLE 2 composition g/L of the solution after impurity removal
| Mg | Ca | Fe | Na | Heavy metals (in Pb) | Mn | pH |
| 38.05 | 0.40 | 0.0008 | 0.25 | 0.0005 | 0.001 | 8.3 |
(4) Sending the magnesium-containing liquid obtained in the step (3) into a conventional MVR evaporator, evaporating and concentrating to obtain magnesium sulfate concentrated solution with the content of magnesium sulfate of 30 percent and the temperature of the concentrated solution of 70 ℃, and sending the evaporated condensed water back to the nickel smelting process to be reused as process water;
(5) and (3) feeding the magnesium sulfate concentrated solution obtained in the step (4) into conventional pressure type or centrifugal spray fluidized bed granulation drying equipment, wherein the heat source is high-temperature waste heat flue gas, the hot air temperature is 260 ℃, spray drying is carried out to obtain a magnesium sulfate product (the components of the product are shown in the table 3), and tail gas generated by spray drying is returned to the nickel smelting process or the step (2) and is used as a heat source or an oxidant.
Table 3 product magnesium sulfate composition%
| Mg | Ca | Fe | Na | Heavy metals (in Pb) | Mn | pH |
| 17.12 | 0.15 | 0.0003 | 0.07 | 0.0001 | 0.002 | 7.0 |
Example 2
The components of the magnesium-containing wastewater treated in this example are shown in Table 4:
TABLE 4 magnesium-containing waste water composition g/L
| Mg | Ca | Fe | Na | Heavy metals (in Pb) | Mn | pH |
| 42.09 | 0.39 | 0.002 | 0.13 | 0.001 | 0.067 | 8.2 |
The method comprises the following steps:
(1) adding sodium sulfide into the magnesium-containing wastewater to precipitate heavy metal, wherein the addition amount of the sodium sulfide is 2.5 times of the amount of the heavy metal in the wastewater, reacting for 60 minutes at the temperature of 70 ℃ to convert the heavy metal into sulfide precipitate, and carrying out solid-liquid separation to obtain the heavy metal precipitate and magnesium-containing liquid;
(2) introducing tail gas into the magnesium-containing liquid in the step (1), cooling the tail gas, introducing dust in the tail gas into the liquid, oxidizing bivalent manganese ions in the solution into high-valence manganese precipitates by using oxygen in the tail gas, and separating the manganese precipitates and the magnesium-containing liquid from solid and liquid;
(3) adding magnesium oxide with effective content of 80% and activity of 70 into the magnesium-containing liquid in the step (2) until the pH value of the liquid is 9.1, reacting for 60 minutes at the reaction temperature of 70 ℃ to oxidize bivalent manganese ions in the magnesium-containing liquid into high-valence manganese precipitates, and carrying out solid-liquid separation to obtain manganese precipitates and magnesium-containing liquid, wherein the components of the magnesium-containing liquid are shown in Table 5:
TABLE 5 composition g/L of solution after impurity removal
| Mg | Ca | Fe | Na | Heavy metals (in Pb) | Mn | pH |
| 41.05 | 0.39 | 0.0009 | 0.24 | 0.0004 | 0.0009 | 9.1 |
(4) Evaporating and concentrating the magnesium-containing liquid in the step (3) in a conventional multi-effect evaporator to obtain magnesium sulfate concentrated solution with the content of magnesium sulfate of 50 percent and the temperature of the concentrated solution of 70 ℃, and feeding the evaporated condensed water back to a nickel smelting process to be reused as process water;
(5) and (3) feeding the magnesium sulfate concentrated solution obtained in the step (4) into conventional pressure type or centrifugal spray fluidized bed granulation drying equipment, wherein the heat source is high-temperature waste heat flue gas, the hot air temperature is 370 ℃, spray drying is carried out to obtain a magnesium sulfate product (the components of the product are shown in a table 6), and tail gas generated by spray drying is returned to a nickel smelting process or the step (2) and is used as a heat source or an oxidant.
Table 6 product magnesium sulfate composition%
| Mg | Ca | Fe | Na | Heavy metals (in Pb) | Mn | pH |
| 16.95 | 0.13 | 0.0002 | 0.05 | 0.0001 | 0.001 | 8.1 |
Example 3
The components of the magnesium-containing wastewater treated in this example are shown in Table 7:
TABLE 7 magnesium-containing waste water composition g/L
| Mg | Ca | Fe | Na | Heavy metals (in Pb) | Mn | pH |
| 40.05 | 0.43 | 0.004 | 0.16 | 0.001 | 0.071 | 8.5 |
The method comprises the following steps:
(1) adding sodium sulfide into the magnesium-containing wastewater to precipitate heavy metals, wherein the addition amount of the sodium sulfide is 1.5 times of the amount of the heavy metals in the wastewater, reacting for 90 minutes at the temperature of 50 ℃ to convert the heavy metals into sulfide precipitates, and carrying out solid-liquid separation to obtain the heavy metal precipitates and magnesium-containing liquid;
(2) introducing tail gas into the magnesium-containing liquid in the step (1), cooling the tail gas, introducing dust in the tail gas into the liquid, oxidizing bivalent manganese ions in the solution into high-valence manganese precipitates by using oxygen in the tail gas, and separating the manganese precipitates and the magnesium-containing liquid from solid and liquid;
(3) adding magnesium oxide with effective content of 85% and activity of 70 into the magnesium-containing liquid in the step (2) until the pH value of the liquid is 9.0, reacting for 100 minutes at the reaction temperature of 50 ℃ to oxidize bivalent manganese ions in the magnesium-containing liquid into high-valence manganese precipitates, and carrying out solid-liquid separation on the manganese precipitates and the magnesium-containing liquid, wherein the components of the magnesium-containing liquid are shown in Table 8:
TABLE 8 composition g/L of solution after impurity removal
| Mg | Ca | Fe | Na | Heavy metals (in Pb) | Mn | pH |
| 41.02 | 0.40 | 0.0006 | 0.22 | 0.0003 | 0.0008 | 9.0 |
(4) Evaporating and concentrating the magnesium-containing liquid obtained in the step (3) in a conventional MVR evaporator to obtain magnesium sulfate concentrated solution with the content of 40% of magnesium sulfate and the temperature of the concentrated solution being 80 ℃, and feeding the evaporated condensed water back to a nickel smelting process to be reused as process water;
(5) and (3) feeding the magnesium sulfate concentrated solution obtained in the step (4) into conventional pressure type spray fluidized bed granulation drying equipment, wherein a heat source is natural gas, the temperature of hot air is 450 ℃, spray drying is carried out to obtain a magnesium sulfate product (the components of the product are shown in a table 6), and tail gas generated by spray drying is returned to a nickel smelting process or the step (2) and is used as a heat source or an oxidant.
Table 9 product magnesium sulfate fraction%
| Mg | Ca | Fe | Na | Heavy metals (in Pb) | Mn | pH |
| 16.66 | 0.12 | 0.0001 | 0.04 | 0.0001 | 0.0008 | 8.0 |
Claims (4)
1. A method for treating magnesium-containing wastewater from nickel smelting is characterized by comprising the following steps:
(1) adding sodium sulfide into the magnesium-containing wastewater from nickel smelting to precipitate heavy metals, wherein the addition amount of the sodium sulfide is 1.0-2.5 times of the amount of the heavy metals in the wastewater, reacting for 60-120 minutes at the temperature of 30-70 ℃ to convert the heavy metals into sulfide precipitates, and separating the heavy metal precipitates and magnesium-containing liquid from solid and liquid;
(2) introducing tail gas into the magnesium-containing liquid in the step (1), cooling the tail gas, introducing dust in the tail gas into the liquid, oxidizing bivalent manganese ions in the solution into high-valence manganese precipitates by using oxygen in the tail gas, and separating the manganese precipitates and the magnesium-containing liquid from solid and liquid;
(3) adding magnesium oxide into the magnesium-containing liquid obtained in the step (2) until the pH value of the liquid is 8.0-9.5, reacting for 60-150 minutes at the reaction temperature of 30-70 ℃ to oxidize divalent manganese ions in the magnesium-containing liquid into high-valence manganese precipitates, and separating the manganese precipitates and the magnesium-containing liquid from solid and liquid;
(4) evaporating and concentrating the magnesium-containing liquid obtained in the step (3) to obtain magnesium sulfate concentrated solution, and feeding the evaporated condensed water back to the nickel smelting process to be reused as process water;
(5) and (3) carrying out spray drying on the magnesium sulfate concentrated solution in the step (4) to obtain a magnesium sulfate product, and returning tail gas generated by spray drying to a nickel smelting process or the step (2) to be used as a heat source or an oxidant.
2. The method for treating magnesium-containing wastewater from nickel smelting according to claim 1, characterized in that the effective content of the magnesium oxide added in the step (3) is 75-90%, and the activity is 50-90%.
3. The method for treating magnesium-containing wastewater from nickel smelting according to claim 1, characterized in that the evaporation concentration equipment in the step (4) is a conventional MVR evaporator or a multi-effect evaporator, and is a negative pressure countercurrent evaporation, the magnesium sulfate content of the evaporation concentrate is 30-50%, and the temperature of the concentrate is 70-110 ℃.
4. The method for treating magnesium-containing wastewater from nickel smelting according to claim 1, wherein the spray drying in step (5) is implemented by using conventional pressure type or centrifugal spray fluidized bed granulation drying equipment, the heat source is natural gas or high-temperature waste heat flue gas, and the temperature of hot air is 250-450 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276099A (en) * | 2011-07-29 | 2011-12-14 | 广西银亿科技矿冶有限公司 | Comprehensive treatment method of waste water from laterite-nickel ore wet smelting |
| CN103073125A (en) * | 2013-01-15 | 2013-05-01 | 昆明理工大学 | Method for using acidolysis nickel laterite ore wastewater |
| CN106277417A (en) * | 2015-05-26 | 2017-01-04 | 有研稀土新材料股份有限公司 | The method that smelting waste water comprehensive containing magnesium reclaims |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276099A (en) * | 2011-07-29 | 2011-12-14 | 广西银亿科技矿冶有限公司 | Comprehensive treatment method of waste water from laterite-nickel ore wet smelting |
| CN103073125A (en) * | 2013-01-15 | 2013-05-01 | 昆明理工大学 | Method for using acidolysis nickel laterite ore wastewater |
| CN106277417A (en) * | 2015-05-26 | 2017-01-04 | 有研稀土新材料股份有限公司 | The method that smelting waste water comprehensive containing magnesium reclaims |
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