CN109626853B - Harmless treatment process for electrolytic manganese slag - Google Patents
Harmless treatment process for electrolytic manganese slag Download PDFInfo
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- CN109626853B CN109626853B CN201811513350.2A CN201811513350A CN109626853B CN 109626853 B CN109626853 B CN 109626853B CN 201811513350 A CN201811513350 A CN 201811513350A CN 109626853 B CN109626853 B CN 109626853B
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D3/00—Calcareous fertilisers
- C05D3/02—Calcareous fertilisers from limestone, calcium carbonate, calcium hydrate, slaked lime, calcium oxide, waste calcium products
Abstract
The invention discloses a harmless treatment process of electrolytic manganese slag, which comprises the steps of adding calcium hydroxide into the electrolytic manganese slag to obtain a first product, adding a compound agent into a sodium chloride solution with the concentration of 10-25% to obtain a second product, and mixing the first product and the second product according to the prepared solid-liquid ratio: 1: 3.5-5.5 to obtain a third product; and heating the product III, washing with hot water after heating, filtering, and drying to obtain a product IV. When the method is used for treating the electrolytic manganese slag, the treatment cost is low, the energy consumption is low, the treatment steps are simple, the operation is easy, and the pollution of the stacking of the electrolytic manganese slag to the surrounding environment is avoided.
Description
Technical Field
The invention belongs to the technical field of manganese production, and particularly relates to a process for treating electrolytic manganese slag.
Background
At present, China is the first major manganese producing country in the world, manganese metal is used in the steel industry, and manganese is one of important basic materials and important strategic national resources of national economy in China, so that manganese production is very important.
The production process of manganese mainly comprises an electrolytic method, an aluminothermic method and an electric silicothermic method, and the industrial production method of manganese is the electrolytic method. The production cost of the electrolytic method is high, a large amount of electrolytic manganese slag can be generated, and the purity of the produced manganese is good.
The electrolytic manganese slag is the largest and most dangerous pollution source in the electrolytic manganese industry, and the recycling of the electrolytic manganese metal slag is a worldwide problem. China is the biggest world for producing, consuming and exporting electrolytic manganese metal, and the capacity of China exceeds 200 million tons, which accounts for 98 percent of the total production capacity of the electrolytic manganese. The electrolytic manganese slag is the filtered acid slag generated after the metal manganese is electrolyzed, and is a key pollutant in the electrolytic manganese industry. The production of electrolytic manganese slag reaches 7-11 tons/ton of manganese, the production per year is about 2000 ten thousand tons, the annual accumulation is more than 8000 ten thousand tons, and the stock is huge. At present, enterprises do not find a method for properly treating electrolytic manganese slag, and the electrolytic manganese slag is generally transported to a storage yard to be built into a dam for stacking. The domestic electrolytic manganese slag tailing dam occupies a large area, has low safety coefficient, and pollutes large cultivated land and underground water sources under the effect of weathering eluviation for a long time, thus causing serious damage to the ecological environment.
The traditional treatment modes of the electrolytic manganese slag mainly comprise the following two treatment modes:
the first is electrolytic manganese slag sorting treatment technology. The technology separates various components by utilizing different physicochemical characteristics of each mineral phase of the electrolytic manganese slag, for example, a magnetic separation concentrate obtained by utilizing the magnetism of manganese can be used as a qualified raw material for producing electrolytic manganese.
The other is electrolytic manganese slag solidification treatment technology. The technology fixes or wraps harmful components in the electrolytic manganese slag in an inert solidified base material, and is a harmless treatment method. The cement is generally used as a base material for solidification addition, and the addition amount of the cement is not less than 45%.
In recent years, the grade of manganese ore has been gradually reduced. Meanwhile, along with the improvement of the production process level, the efficiency of the production link is continuously improved, the content of manganese in the electrolytic manganese slag is further reduced, and the manganese in the electrolytic manganese slag is difficult to recycle again by a separation treatment method. Although the solidification treatment effect is good, for the electrolytic manganese slag piled up into a mountain, the method can consume a large amount of cement, the treatment cost is increased, and the industrial application prospect is general.
The accumulation of a large amount of electrolytic manganese slag brings great pressure to the environmental protection work of China. The electrolytic manganese slag is recycled, so that the problem of environmental pollution can be solved, benefits can be created for enterprises, and the production cost is reduced. At present, the electrolytic manganese slag is mainly recycled in the following ways:
firstly, recovering valuable metals. The manganese resource in the electrolytic manganese slag accounts for 9-13%. The recovery method of manganese mainly comprises three methods, namely a biological method, an acid leaching method and a water washing precipitation method. The biological method mainly utilizes sulfur oxidizing bacteria and iron oxidizing bacteria to leach manganese in the electrolytic manganese slag, and the leaching rate of the manganese can reach over 90 percent. The acid leaching method is characterized in that acid leaching liquid and leaching auxiliary agent are added into electrolytic manganese slag, and a manganese sulfate product with higher purity can be obtained after ultrasonic treatment and impurity removal. The washing precipitation method adopts a method of 'washing slag with clear water and ammonium salt precipitation' to recover soluble manganese, the recovery rate of manganese can reach more than 99%, and the content of manganese in the recovered manganese-rich precipitation material can reach more than 30%. The acid leaching method and the water washing precipitation method have limited application due to complex process, high cost and secondary pollution. The biological method is a method for recovering manganese and other metal ions in electrolytic manganese slag with great potential, but has higher requirements on strains and leaching conditions, and the bacterial leaching time is generally longer. In addition, the culture of the strains is complicated, and the most suitable strains cannot be found at present.
And secondly, preparing a complete fertilizer. The electrolytic manganese slag is rich in organic substances and a large amount of nutrient elements required by plants, such as manganese, selenium, potassium, sodium, iron, boron and the like, which provides possibility for preparing the complete fertilizer by utilizing the electrolytic manganese slag. At present, although the full-value fertilizer prepared by electrolytic manganese slag can increase certain fertilizer efficiency, the fertilizer efficiency is inferior to that of common nitrogen fertilizer and phosphate fertilizer. In addition, the electrolytic manganese residues also contain a plurality of harmful elements, promote the growth of crops and pollute soil, thus being harmful to human health. If the electrolytic manganese residue fertilizer can be subjected to harmless treatment before being applied, the electrolytic manganese residue fertilizer can be widely applied to agricultural actual production.
And thirdly, producing the wall material. The electrolytic manganese slag mainly contains silicon dioxide, calcium oxide, iron oxide, aluminum oxide and the like, and is suitable for brick making. At present, the main products produced by utilizing the electrolytic manganese slag comprise baking-free bricks, sintered bricks, ceramic bricks, autoclaved bricks and insulating bricks. The main problems of the electrolytic manganese slag in preparing the wall material are as follows: firstly, the doping proportion of the electrolytic manganese slag is relatively small, and the increase of the doping amount can cause the strength of the brick body to be reduced; and secondly, heavy metal and toxic impurities in the electrolytic manganese slag need to be further removed.
Fourthly, producing the roadbed material. The electrolytic manganese residue powder is added with the fly ash and the carbide mud to prepare the clinker-free asphalt mixture, so that the stability, the strength, the adhesiveness and the corrosion resistance of the asphalt mixture can be effectively improved. The compressive strength of the asphalt mixture after 1 year of use can still reach 10 MPa, and the requirement of traffic road construction is met. When the addition amount of the electrolytic manganese slag reaches 80%, the performance and the economical efficiency of the prepared asphalt cement and asphalt mixture are the best. Certainly, the application of the electrolytic manganese slag in the highway subgrade material is popularized on a large scale, and the toxic effect of heavy metal ions in the electrolytic manganese slag is also considered. Heavy metal ions in the electrolytic manganese slag can permeate into soil near the roadbed through rainwater, so that the surrounding environment is affected.
At present, most of the research on the resource utilization technology of electrolytic manganese slag is in the theoretical research stage and is applied to the actual industrialization for a few reasons, which are mainly as follows: firstly, good economic benefit cannot be obtained by recycling the manganese metal in the electrolytic manganese slag, and the secondary utilization value is not large. Secondly, in the resource utilization process of the electrolytic manganese slag in the fields of cement industry, wall materials, preparation of complete fertilizers and the like, the harmless treatment of harmful elements or heavy metals needs to be considered, and the cost is high.
The application publication number is CN107649488A, the publication date is 2018, 2.2.2018, and the application person is the Chinese invention patent application of the Qinghua university, which discloses a harmless method for treating electrolytic manganese slag, and the method comprises the following steps: (1) the electrolytic manganese slag is processed at the temperature of 450-900 ℃ and the oxygen partial pressure of 10-2Pa～104Roasting for 0.5-4 hours under the condition of Pa; (2) immersing the electrolytic manganese slag obtained in the step (1) for 0.5-2 hours by using an aqueous solution containing a chelating agent or dilute sulphuric acid; (3) and (3) carrying out filter pressing on the product obtained in the step (2), and drying a filter cake to obtain harmless electrolytic manganese slag. The method can ensure that the color of the electrolytic manganese slag after the harmless treatment is the same as that of local clay, and the concentration of harmful substances including heavy metals reaches the national agricultural soil standard. The harmless electrolytic manganese slag can be used as soil for improving cultivated land and can also be used for re-cultivation of local desertification land. However, in the method, the electrolytic manganese slag is roasted for 0.5-4 hours at the high temperature of 450-900 ℃, so that the energy consumption is high; the treatment cost is high.
Disclosure of Invention
In order to overcome the defects of the existing harmless treatment process of the electrolytic manganese slag, the invention provides the harmless treatment process of the electrolytic manganese slag, the process for treating the electrolytic manganese slag has the advantages of low treatment cost, low energy consumption, simple treatment steps and easy operation, and the pollution of stacking of the electrolytic manganese slag to the surrounding environment is avoided.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a harmless treatment process of electrolytic manganese slag is characterized by comprising the following steps: comprises a first product preparation step, a second product preparation step, a third product preparation step and a fourth product preparation step,
the preparation step of the first product comprises the following specific steps:
adding calcium hydroxide into the electrolytic manganese slag to obtain a product I, wherein the content of the added calcium hydroxide is as follows: according to the weight parts, 20-30 parts of calcium hydroxide are added into 100 parts of electrolytic manganese slag;
the preparation steps of the product II are as follows: adding 0.5-2 parts of a compound agent into 400-600 parts of a sodium chloride solution according to parts by weight to obtain a second product, wherein the compound agent comprises 0.5-2 parts of citrate and 10-25 parts of aluminum sulfate according to parts by weight;
the preparation steps of the third product are as follows: uniformly mixing the first product and the second product, and preparing a solid-liquid ratio: 1: 3.5-5.5 to obtain a third product;
the fourth preparation step of the product comprises the following specific steps: and heating the product III, washing with hot water after heating, filtering, and drying to obtain a product IV.
In the first product preparation step, the water content of the electrolytic manganese slag is controlled to be 40-50%.
And in the preparation step of the first product, adding calcium hydroxide into the electrolytic manganese slag, stirring for 20-40 min, and standing for more than 2h after stirring to obtain the first product.
In the second preparation step of the product, the concentration of the sodium chloride solution is 10-25%.
In the third preparation step of the product, the first product and the second product are uniformly mixed in a stirring mode, and the stirring time is 1-2 min.
In the fourth preparation step of the product, the heating temperature is controlled to be 90-130 ℃, and the heating time is 3-5 hours.
In the fourth preparation step of the product, the temperature of the hot water is more than or equal to 93 ℃.
And fourthly, obtaining harmless electrolytic manganese slag. The manganese slag forms a substance with gelling property, and provides a manganese slag-based raw material for application in putty powder, decorative boards and the like.
Compared with the prior art, the invention has the following beneficial effects:
after the electrolytic manganese slag is treated by the process provided by the invention, harmful substances (manganese ions and ammonia nitrogen) in the electrolytic manganese slag are treated to become harmless electrolytic manganese slag. The obtained electrolytic manganese slag is no longer a toxic substance and is harmless to the surrounding environment. Forming a substance with gelling property, and providing a manganese slag-based raw material for the application of putty powder, decorative boards and the like. The obtained electrolytic manganese slag is used for preparing the complete fertilizer, so that the soil is not polluted, the human health is not damaged, and the roadbed material is produced, so that the soil nearby the roadbed can not be permeated by rainwater, and the surrounding environment is not influenced. The wall material is made without worrying about the emission of harmful substances and the influence on the health of the body. The process has simple operation steps, and the electrolytic manganese slag does not need to be roasted for 0.5-4 hours at the high temperature of 450-900 ℃, so that the energy consumption is obviously reduced, and the treatment cost is obviously reduced.
Detailed Description
The present invention will be further described with reference to the following examples, which are intended to illustrate only some, but not all, of the embodiments of the present invention. Based on the embodiments of the present invention, other embodiments used by those skilled in the art without any creative effort belong to the protection scope of the present invention.
Firstly, 500 parts of untreated electrolytic manganese residues are taken, 500 parts of electrolytic manganese residues are equally divided into 5 parts and respectively filled in containers, and labels 1, 2, 3, 4 and 5 are respectively stuck on each container.
The content of harmful substances in the electrolytic manganese slag and the content of the harmful substances in the electrolytic manganese slag in the standard GB8978-1996 are shown in the table I:
table one content of harmful substances in electrolytic manganese slag
As can be seen from the table I, except that the contents of the manganese particles and the ammonia nitrogen in the electrolytic manganese slag are far higher than the standard requirements, the contents of other harmful substances are all lower than the standard limit value, so that the manganese particles and the ammonia nitrogen in the electrolytic manganese slag only need to be treated.
Example 1
Controlling the water content of the electrolytic manganese slag in the container 1 to be 40%, then adding 20 parts of calcium hydroxide into the container 1, stirring for 20min, and standing for more than 2h to obtain a product I;
preparing 400 parts of 10% sodium chloride solution, and adding 0.5 part of compound agent into the sodium chloride solution to obtain a second product; the compound agent contains 0.5 part of citrate and 10 parts of aluminum sulfate;
adding the product I into the product II, stirring for 1min, and preparing a mixed solution with a solid-liquid ratio of 1:3.5 to obtain a product III;
and heating the product III at 90 ℃ for 5h, washing and filtering the product III by using hot water at 93 ℃, and drying the product III to obtain a product IV, wherein the product IV is the electrolytic manganese slag after harmless treatment.
Example 2
Controlling the water content of the electrolytic manganese slag in the container 2 to be 42%, then adding 22 parts of calcium hydroxide into the container 2, stirring for 25min, and standing for more than 2h to obtain a product I;
preparing 450 parts of 15% sodium chloride solution, and adding 1 part of compound agent into the sodium chloride solution to obtain a second product; the compound agent contains 1 part of citrate and 15 parts of aluminum sulfate;
adding the product I into the product II, stirring for 1.2min, and preparing a mixed solution with a solid-liquid ratio of 1:4 to obtain a product III;
and heating the product III at 100 ℃, washing and filtering the product III by using hot water at 94 ℃ after heating for 4.5 hours, and drying the product III to obtain a product IV, namely the electrolytic manganese slag after harmless treatment.
Example 3
Controlling the water content of the electrolytic manganese slag in the container 3 to be 45%, then adding 25 parts of calcium hydroxide into the container 3, stirring for 30min, and standing for more than 2h to obtain a product I;
preparing 500 parts of sodium chloride solution with the concentration of 20%, and adding 1.5 parts of compound agent into the sodium chloride solution to obtain a second product; the compound agent contains 1.5 parts of citrate and 20 parts of aluminum sulfate;
adding the product I into the product II, stirring for 1.5min, and preparing a mixed solution with a solid-liquid ratio of 1:4.5 to obtain a product III;
and heating the product III at 110 ℃, washing and filtering the product III by using hot water at 95 ℃ after heating for 4h, and drying the product III to obtain a product IV, wherein the product IV is the electrolytic manganese slag after harmless treatment.
Example 4
Controlling the water content of the electrolytic manganese slag in the container 4 to be 48%, then adding 28 parts of calcium hydroxide into the container 4, stirring for 35min, and standing for more than 2h to obtain a product I;
preparing 550 parts of 23% sodium chloride solution, and adding 1.8 parts of compound agent into the sodium chloride solution to obtain a second product; the compound agent contains 1.8 parts of citrate and 22 parts of aluminum sulfate;
adding the product I into the product II, stirring for 1.8min, and preparing a mixed solution with a solid-liquid ratio of 1:5 to obtain a product III;
and heating the product III at 125 ℃, washing and filtering the product III by using hot water at 100 ℃ after heating for 3.5 hours, and drying the product III to obtain a product IV, namely the electrolytic manganese slag after harmless treatment.
Example 5
Controlling the water content of the electrolytic manganese slag in the container 5 to be 50%, then adding 30 parts of calcium hydroxide into the container 5, stirring for 40min, and standing for more than 2h to obtain a product I;
preparing 600 parts of 25% sodium chloride solution, and adding 2 parts of a compound agent into the sodium chloride solution to obtain a second product; the compound agent contains 2 parts of citrate and 25 parts of aluminum sulfate;
adding the product I into the product II, stirring for 2min, and preparing a mixed solution with a solid-liquid ratio of 1: 5.5 to obtain a product III;
and heating the product III at 130 ℃, washing and filtering the product III by using hot water at 110 ℃ after heating for 3h, and drying the product III to obtain a product IV, wherein the product IV is the electrolytic manganese slag after harmless treatment.
The results of the tests on the electrolytic manganese slag obtained after the treatment in the above example are shown in table two:
the harmless electrolytic manganese slag obtained in the embodiment has a small amount of metal ion precipitates, free heavy metal ions do not exist any more, the removal rate of the free manganese ions and ammonia radicals is more than 99%, and the rest ammonia radicals generate trace magnesium ammonium phosphate. No harmful substances exist, and the raw materials which are piled up or used as other substances are nontoxic and harmless. Really achieves the effect of harmless treatment of the electrolytic manganese slag.
The electrolytic manganese slag treated by the embodiment is injected into a corresponding mould to obtain the electrolytic manganese slag-based artware, and the harmless resource recycling problem of the next step is solved. Can recycle the electrolytic manganese slag.
Claims (4)
1. A harmless treatment process of electrolytic manganese slag is characterized by comprising the following steps: comprises a first product preparation step, a second product preparation step, a third product preparation step and a fourth product preparation step,
the preparation step of the first product comprises the following specific steps:
adding calcium hydroxide into the electrolytic manganese slag to obtain a product I, wherein the content of the added calcium hydroxide is as follows: according to the weight parts, 20-30 parts of calcium hydroxide are added into 100 parts of electrolytic manganese slag;
the preparation steps of the product II are as follows: adding 0.5-2 parts of a compound agent into 400-600 parts of a sodium chloride solution according to parts by weight to obtain a second product, wherein the compound agent comprises 0.5-2 parts of citrate and 10-25 parts of aluminum sulfate according to parts by weight;
the preparation steps of the third product are as follows: uniformly mixing the first product and the second product, and preparing a solid-liquid ratio: 1: 3.5-5.5 to obtain a third product;
the fourth preparation step of the product comprises the following specific steps: heating the product III, washing with hot water after heating, filtering, and drying to obtain a product IV;
in the first product preparation step, the water content of the electrolytic manganese slag is controlled to be 40-50%;
in the preparation step of the first product, calcium hydroxide is added into electrolytic manganese slag and then stirred for 20-40 min, and the mixture is kept stand for more than 2h after stirring is completed to obtain the first product;
in the second preparation step of the product, the concentration of the sodium chloride solution is 10-25%.
2. The harmless treatment process of the electrolytic manganese slag according to claim 1, which is characterized in that: in the third preparation step of the product, the first product and the second product are uniformly mixed in a stirring mode, and the stirring time is 1-2 min.
3. The harmless treatment process of the electrolytic manganese slag according to claim 1, which is characterized in that: in the fourth preparation step of the product, the heating temperature is controlled to be 90-130 ℃, and the heating time is 3-5 hours.
4. The harmless treatment process of the electrolytic manganese slag according to claim 1, which is characterized in that: in the fourth preparation step of the product, the temperature of the hot water is more than or equal to 93 ℃.
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| CN104690080A (en) * | 2015-03-28 | 2015-06-10 | 重庆大学 | Method for directly carrying out innocent treatment on electrolytic manganese residues in filter pressing plate frames |
| KR20180064006A (en) * | 2016-12-05 | 2018-06-14 | 주식회사 에코마이스터 | Silicon manganese slag light weight aggregate and it's manufacturing method |
| CN108262336A (en) * | 2018-02-24 | 2018-07-10 | 昆明理工大学 | A kind of solidification processing method of electrolytic manganese residues |
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| CN1258269A (en) * | 1997-05-29 | 2000-06-28 | 派里克累斯有限公司 | Encapsulation of hazardous waste materials |
| CN101691633A (en) * | 2009-10-12 | 2010-04-07 | 湖南广义科技有限公司 | Method for innocent treatment and comprehensive utilization of manganese slag |
| CN104690080A (en) * | 2015-03-28 | 2015-06-10 | 重庆大学 | Method for directly carrying out innocent treatment on electrolytic manganese residues in filter pressing plate frames |
| KR20180064006A (en) * | 2016-12-05 | 2018-06-14 | 주식회사 에코마이스터 | Silicon manganese slag light weight aggregate and it's manufacturing method |
| CN108262336A (en) * | 2018-02-24 | 2018-07-10 | 昆明理工大学 | A kind of solidification processing method of electrolytic manganese residues |
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