CN101260471B - Complete set of cleaning producing technique for extracting soluble manganese from manganese residue by using anode liquor - Google Patents
Complete set of cleaning producing technique for extracting soluble manganese from manganese residue by using anode liquor Download PDFInfo
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- CN101260471B CN101260471B CN2008101051077A CN200810105107A CN101260471B CN 101260471 B CN101260471 B CN 101260471B CN 2008101051077 A CN2008101051077 A CN 2008101051077A CN 200810105107 A CN200810105107 A CN 200810105107A CN 101260471 B CN101260471 B CN 101260471B
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Abstract
The invention discloses a unitized cleaning production technique for extracting soluble manganese from the manganese slag by adopting anode liquor, comprising the following steps that: a. the manganese and the anode liquor generated in the process of electrolytic manganese metal production are transported to an extracting device, the sulphuric acid with a volume 0 to 0.025 times of the anode liquor is added, the solid-to-liquid weight ratio of manganese slag to the added fluid ranges from 1:1 to 1:15; b. the manganese slag and the anode liquor are mixed evenly by stirring to obtain the extracting fluid; c. the extracting fluid is let stand in the extracting device to ensure that the solid substance in the extracting fluid subsides; d. the clear solution after the sediment is filtered and returns directly to the leaching oxidizing process in the process of electrolytic manganese metal production for preparing the electrolysing solution; the filtration residue and the dregginess in the extracting device are transported to an efficient filter pressing device to dewater, the water ratio of the slag is reduced to below 25 percent, the slag is transported to a manganese slag filed or becomes resource, the filter pressing fluid after filtered returns to the leaching oxidizing process for preparing the electrolysing solution. The invention also provides an electrolytic manganese metal producing technique.
Description
Technical field
The present invention relates to recycle of electrolytic metal Mn industry resource and environment protection novel method, be specifically related to a kind of complete set of cleaning producing technique that from the manganese slag that electrolytic metal Mn produces, reclaims soluble manganese.
Background technology
In recent years, because the fast development of steel industry both at home and abroad, sharply increase the also fast development thereupon of the electrolytic metal manganese industry of China as the demand of the manganese of the deoxidation in ironmaking and the steelmaking process, sweetening agent.But simultaneously; because the electrolytic metal manganese industry is one " high material-consumption, high energy consumption, high pollution " " three high industry "; in recent years in fast development; face manganese resource scarcity, the environmental protection pressure problem and the challenge of aspect such as strictness day by day, have a strong impact on and restricting the health of industry, in order, Sustainable development.
Steps such as what current electrolytic metal Mn adopted is sulfuric acid to leach one electrolytic hydrometallurgy production technique, and its production process comprises powder process, sulfuric acid leaching, iron removal by oxidation, press filtration, purification, secondary press filtration, deep purifying, smart filter, electrolysis, passivation, rinsing, dry, peel off.In the production process of electrolytic metal Mn, need to consume resources such as a large amount of manganese carbonate ores, pyrolusite, sulfuric acid, ammoniacal liquor, electricity, produce a large amount of " waste water,waste gas and industrial residue " simultaneously.Protect reasons such as consciousness is not high, Technology backwardness, environment protection insufficient investment owing to the most of electrolytic metal Mn corporate environments of China; and enterprise distributes more concentrated relatively; to the on-site ecological environmental pollution of enterprise with destroy greatlyyer, have a strong impact on and threatening local resident's health and wellbeing.
At present in the electrolytic metal manganese industry, 1 ton of electrolytic metal Mn of every production produces 6～7 tons manganese slag, wherein owing to the reasons such as restriction of production technique, pressure filtering technique, make also residual many soluble manganese in the manganese slag, also contain a large amount of vitriol, ammonia nitrogen in the manganese slag simultaneously, the content of heavy metals such as arsenic, mercury, selenium is also higher.The annual manganese slag that produces 210,000 tons of enterprise of producing 30000 tons of electrolytic metal Mns per year, the whole outdoor storages of these manganese slags, in depositing process, especially when raining, produce a large amount of percolates, soluble manganese, vitriol, ammonia nitrogen etc. flow away thereupon, the severe contamination surrounding enviroment become the main Environmental Problems of electrolytic metal manganese industry.
It is reported that the someone utilizes water as extraction agent the soluble manganese in the manganese slag to be extracted, but because water consumption is bigger, calculate at 1: 10 by solid-to-liquid ratio, 1 ton of manganese slag needs 7 tons of water, calculate by the scale of producing 30000 tons of electrolytic metal Mn enterprises per year, produce 600～700 tons of manganese slags every day, need about 7000 tons water, and the electrolytic metal Mn factory of this scale only need to replenish 300 every day surplus ton water, will inevitably cause the system water can't balance if extracting solution is directly returned production process, problems such as water expansion occur.Therefore, extract soluble manganese in the manganese slag if use water as extraction agent, just can turn back in the production process after extracting solution need concentrate, and owing to the reason of current concentration technique, equipment, power consumption etc., cause spissated cost height, this method is infeasible economically.Therefore, using water as agent in advance, to extract the method for soluble manganese in the manganese slag inadvisable in actual production.
Therefore, the manganese slag is carried out recycling treatment, soluble manganese becomes one of bottleneck problem that needs to be resolved hurrily in the electrolytic metal Mn industry development in the recovery manganese slag.
Summary of the invention
The objective of the invention is soluble manganese in the manganese slag is extracted and utilization again.
For achieving the above object, adopt the lower concentration that produces in the electrolytic metal Mn production process to contain manganese liquid, be that anolyte is an extraction agent, soluble manganese in the manganese slag is extracted, improve the concentration of manganese in the anolyte, and turn back to system liquid process and make electrolytic solution again, when having avoided problems such as water expansion to occur, realized the purpose of resource utilization, can obviously improve economic benefit and cleaner production level that enterprise produces, meet the theory and the thinking of cleaner production and recycling economy, help increasing the sustained development of enterprises ability.
Particularly, the invention provides a kind of complete set of cleaning producing technique that adopts anolyte to extract soluble manganese in the manganese slag, it may further comprise the steps:
A. the anolyte that produces in manganese slag, the electrolytic metal Mn production process is transported in the extraction equipment, adds the sulfuric acid of 0～0.025 times of anolyte volume simultaneously, the manganese slag is 1: 1～1: 15 with the solid-liquid weight ratio that adds liquid;
B. make manganese slag and the abundant mixing of liquid by stirring, can obtain extracting solution;
C. extracting solution leaves standstill in extraction equipment, makes solid deposits in the extracting solution;
D. with the leaching oxidation operation that directly is back to behind the supernatant liquid filtering of post precipitation in the electrolytic metal Mn production process, be used for making electrolytic solution; Sediment in filter residue and the extraction equipment is transported to efficient filtering equipment carries out processed, the water ratio in the slag is reduced to below 25%, slag is sent to manganese slag field or resource utilization, and pressing filtering liquid returns the leaching oxidation operation after filtering, be used for making electrolytic solution.
Above-mentioned employing anolyte extracts the complete set of cleaning producing technique of soluble manganese in the manganese slag, and wherein this manganese slag can be the manganese slag that produces in the electrolytic metal Mn production process.
Above-mentioned employing anolyte extracts the complete set of cleaning producing technique of soluble manganese in the manganese slag, and wherein this anolyte can wherein contain Mn for the anolyte that produces after the electrolysis in sulfuric acid to leach-electrolytic metal Mn production process
2+10g/L～18g/L.
Above-mentioned employing anolyte extracts the complete set of cleaning producing technique of soluble manganese in the manganese slag, and wherein the abstraction reaction time of this step b can be 15～240 minutes.
Above-mentioned employing anolyte extracts the complete set of cleaning producing technique of soluble manganese in the manganese slag, and wherein the time of staticly settling of this step c can be 15～60 minutes.
On the other hand, the present invention also provides a kind of production technique of electrolytic metal Mn, comprise sulfuric acid to leach oxidation, purification and electrolysis step, wherein, use the anolyte that produces after the electrolysis in the electrolysis step that the manganese slag that produces in the purifying step is carried out second extraction, with directly being back to the leaching oxidation operation behind the supernatant liquid filtering after extracting, be used for making electrolytic solution, wherein this second extraction may further comprise the steps:
A. the anolyte that produces in manganese slag, the electrolytic metal Mn production process is transported in the extraction equipment, adds the sulfuric acid of 0～0.025 times of anolyte volume simultaneously, the manganese slag is 1: 1～1: 15 with the solid-liquid weight ratio that adds liquid;
B. make manganese slag and the abundant mixing of liquid by stirring, can obtain extracting solution;
C. extracting solution leaves standstill in extraction equipment, makes solid deposits in the extracting solution;
D. with the leaching oxidation operation that directly is back to behind the supernatant liquid filtering in the extraction equipment in the electrolytic metal Mn production process, be used for making electrolytic solution; Sediment in filter residue and the extraction equipment is transported to efficient filtering equipment carries out processed, the water ratio in the slag is reduced to below 25%, slag is sent to manganese slag field or resource utilization, and pressing filtering liquid returns the leaching oxidation operation after filtering, be used for making electrolytic solution.
Beneficial effect of the present invention is, this technology is improved on the basis of the existing production technique of electrolytic metal Mn enterprise, utilize the soluble manganese in the anolyte extraction manganese slag, and extracting solution is turned back to production process make electrolytic solution, problems such as water expansion when reclaiming manganese, have been avoided, also reduce the discharging of pollutent in the manganese slag simultaneously, reduced the manganese ore consumption and the production cost of unit product, helped continuing, developing in a healthy way of enterprise.This process for cleanly preparing technology has less investment, easy to operate, low cost and other advantages, has good economic benefit and environmental benefit.Extract soluble manganese in the manganese slag by the present invention, at least can extract in the manganese slag 50% soluble manganese, it is 1.7t/100t manganese slag, to electrolytic metal Mn enterprise (the manganese slag year generation: 210,000 t) of producing 30000 t per year, manganese about recyclable 3600t of year, the 1t electrolytic metal Mn is by 20000 yuan/t, can directly increase by 7,200 ten thousand yuan of the output values, the production cost of deduction 50%, 3,600 ten thousand yuan of direct economic benefits, reduce about 25000 tons of consumptions of manganese ore (ore grade 18), annual simultaneously the minimizing about pollutent manganese discharging 3600t.
Description of drawings
Fig. 1 is that the present invention adopts anolyte to extract the process flow sheet of soluble manganese in the manganese slag.
Fig. 2 is electrolytic metal Mn technological process of production figure in the prior art.
Fig. 3 is the improved electrolytic metal Mn technological process of production of the present invention figure.
Embodiment
The invention will be further described below in conjunction with embodiment, but protection scope of the present invention is not limited to following embodiment.
Figure 1 shows that the present invention adopts anolyte to extract the process flow sheet of a preferred implementation of soluble manganese in the manganese slag.Processing step comprises: the anolyte that a. produces after with electrolysis in manganese slag, the electrolytic metal Mn production process is transported in the extraction equipment, add a certain proportion of industrial sulphuric acid simultaneously, add-on is 0～0.025 (with the volume ratio of anolyte), and the manganese slag is 1: 1～1: 15 with the solid-liquid weight ratio that adds liquid; B. make manganese slag and the abundant mixing of liquid by stirring, can obtain extracting solution; C. extracting solution leaves standstill in extraction equipment, makes solid deposits in the extracting solution to realize solid-liquid separation; D. with the leaching oxidation operation that directly is back to behind the supernatant liquid filtering of post precipitation in the electrolytic metal Mn production process, be used for making electrolytic solution; Sediment in filter residue and the extraction equipment is transported to efficient filtering equipment carries out processed, the water ratio in the slag is reduced to below 25%, slag is sent to manganese slag field or resource utilization, and pressing filtering liquid returns the leaching oxidation operation after filtering, be used for making electrolytic solution.
Embodiment 1:
Adopting above-mentioned processing step, is raw material with the manganese slag, is extraction agent (Mn wherein with the anolyte that produces in the electrolytic metal Mn production process
2+Concentration is 14.5g/L), add the sulfuric acid of 0.025 times of anolyte volume simultaneously, be under 1: 2 the condition in solid-to-liquid ratio, manganese slag and anolyte be abundant mixing in extraction equipment, under 30～65 ℃ condition, and 60 minutes abstraction reaction time, can obtain yellowish extracting solution, Mn in the extracting solution
2+Concentration be 25g/L, extracting solution leaches operation through the oxidation that directly turns back to after filtering in the production process, is used for making electrolytic solution.
Embodiment 2:
Adopting above-mentioned processing step, is raw material with the manganese slag, is extraction agent (Mn wherein with the anolyte that produces in the electrolytic metal Mn production process
2+Concentration is 14g/L), be under 1: 6 the condition in solid-to-liquid ratio, manganese slag and anolyte abundant mixing in extraction equipment under 15～45 ℃ condition, 30 minutes abstraction reaction time, can obtain yellowish extracting solution, Mn in the extracting solution
2+Concentration be 22g/L, extracting solution leaches operation through the oxidation that directly turns back to after filtering in the production process, is used for making electrolytic solution.
Embodiment 3:
Adopting above-mentioned processing step, is raw material with the manganese slag, is extraction agent (Mn wherein with the anolyte that produces in the electrolytic metal Mn production process
2+Concentration is 14g/L), be under 1: 10 the condition in solid-to-liquid ratio, manganese slag and anolyte abundant mixing in extraction equipment under 30～45 ℃ condition, 20 minutes abstraction reaction time, can obtain yellowish extracting solution, Mn in the extracting solution
2+Concentration be 17g/L, extracting solution leaches operation through the oxidation that directly turns back to after filtering in the production process, is used for making electrolytic solution.
Embodiment 4:
Adopting above-mentioned processing step, is raw material with the manganese slag, is extraction agent (Mn wherein with the anolyte that produces in the electrolytic metal Mn production process
2+Concentration is 13.5g/L,), add industrial sulphuric acid simultaneously, add-on is 0.015 (with the volume ratio of anolyte), is under 1: 15 the condition in solid-to-liquid ratio, manganese slag and anolyte abundant mixing in extraction equipment, under 15～30 ℃ condition, 15 minutes abstraction reaction time can obtain yellowish extracting solution, Mn in the extracting solution
2+Concentration be 14.5g/L, extracting solution leaches operation through the oxidation that directly turns back to after filtering in the production process, is used for making electrolytic solution.
On the other hand, the present invention also provides a kind of production technique of electrolytic metal Mn, Figure 2 shows that the electrolytic metal Mn technological process of production in the prior art.Its step comprises powder process, sulfuric acid leaching, press filtration, purification, secondary press filtration, deep purifying, smart filter, electrolysis, passivation, rinsing, dries, peels off etc.Figure 3 shows that the electrolytic metal Mn technological process of production of a kind of preferred implementation of the present invention.Relatively two kinds of schemas as seen, improvements of the present invention are to have increased the manganese slag that uses the anolyte that produces after the electrolysis in the electrolysis step to produce in to purifying step to carry out second extraction on the basis of original process, and directly be back to the leaching oxidation operation behind the supernatant liquid filtering after will extracting, be used for making electrolytic solution.Its technology and equipment are simple, but can be implemented in not produce under the water swellable prerequisite soluble manganese in the manganese slag is extracted and utilization again.
Claims (6)
1. complete set of cleaning producing technique that adopts anolyte to extract soluble manganese in the manganese slag is characterized in that may further comprise the steps:
A. the anolyte that produces in manganese slag, the electrolytic metal Mn production process is transported in the extraction equipment, adds the sulfuric acid of 0～0.025 times of anolyte volume simultaneously, the solid-liquid weight ratio in the equipment is 1: 1～1: 15;
B. make manganese slag and the abundant mixing of liquid by stirring, can obtain extracting solution;
C. extracting solution leaves standstill in extraction equipment, makes solid deposits in the extracting solution;
D. with the leaching oxidation operation that directly is back to behind the supernatant liquid filtering of post precipitation in the electrolytic metal Mn production process, be used for making electrolytic solution; Sediment in filter residue and the extraction equipment is transported to efficient filtering equipment carries out processed, the water ratio in the slag is reduced to below 25%, slag is sent to manganese slag field or resource utilization, and pressing filtering liquid returns the leaching oxidation operation after filtering, be used for making electrolytic solution.
2. employing anolyte according to claim 1 extracts the complete set of cleaning producing technique of soluble manganese in the manganese slag, it is characterized in that described manganese slag is the manganese slag that produces in the electrolytic metal Mn production process.
3. employing anolyte according to claim 1 extracts the complete set of cleaning producing technique of soluble manganese in the manganese slag, it is characterized in that described anolyte is the anolyte that produces in the electrolytic metal Mn production process, wherein Mn
2+Content be 10g/L～18g/L.
4. employing anolyte according to claim 1 extracts the complete set of cleaning producing technique of soluble manganese in the manganese slag, and the abstraction reaction time that it is characterized in that described step b is 15～240 minutes.
5. employing anolyte according to claim 1 extracts the complete set of cleaning producing technique of soluble manganese in the manganese slag, and the time of staticly settling that it is characterized in that described step c is 15～60 minutes.
6. the production technique of an electrolytic metal Mn, comprise sulfuric acid to leach oxidation, purification and electrolysis step, it is characterized in that using the anolyte that produces in the electrolytic process that the manganese slag that produces in the scavenging process is carried out second extraction, to directly be back to the leaching oxidation operation behind the supernatant liquid filtering after extracting, be used for making electrolytic solution, wherein said second extraction may further comprise the steps:
A. the anolyte that produces in manganese slag, the electrolytic metal Mn production process is transported in the extraction equipment, adds the sulfuric acid of 0～0.025 times of anolyte volume simultaneously, the solid-liquid weight ratio in the equipment is 1: 1～1: 15;
B. make manganese slag and the abundant mixing of liquid by stirring, can obtain extracting solution;
C. extracting solution leaves standstill in extraction equipment, makes solid deposits in the extracting solution;
D. with the leaching oxidation operation that directly is back to behind the supernatant liquid filtering in the extraction equipment in the electrolytic metal Mn production process, be used for making electrolytic solution; Sediment in filter residue and the extraction equipment is transported to efficient filtering equipment carries out processed, the water ratio in the slag is reduced to below 25%, slag is sent to manganese slag field or resource utilization, and pressing filtering liquid returns the leaching oxidation operation after filtering, be used for making electrolytic solution.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101899583B (en) * | 2009-05-25 | 2012-12-12 | 中国环境科学研究院 | Integrative method of two-stage acid leaching, washing and filter pressing for manganese powder pickle liquor |
| CN102191378B (en) * | 2010-03-15 | 2013-12-18 | 贵州省环境科学研究设计院 | Electrolyte preparation process for electrolyzing manganese |
| CN105274580B (en) * | 2015-11-15 | 2018-01-12 | 王兆兵 | The method that electrolytic manganese produces reclaimed water and manganese slag for comprehensive utilizes |
| CN107699714B (en) * | 2017-09-19 | 2019-08-09 | 四川大学 | A method of manganese sulfate electrolyte is prepared suitable for leaching pyrolusite by sulfur dioxide |
| CN110735155B (en) * | 2018-09-27 | 2021-06-22 | 庞炼红 | Method for producing electrolytic manganese metal and co-producing manganese dioxide |
| CN110479207A (en) * | 2019-07-26 | 2019-11-22 | 铜仁学院 | A kind of method that the alkali fusion activation of electrolytic manganese residues microwave prepares high adsorption value fluorite |
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