CN104016357B - A kind of manganese slag for comprehensive utilizes the method for producing industrial chemicals - Google Patents
A kind of manganese slag for comprehensive utilizes the method for producing industrial chemicals Download PDFInfo
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- CN104016357B CN104016357B CN201410262578.4A CN201410262578A CN104016357B CN 104016357 B CN104016357 B CN 104016357B CN 201410262578 A CN201410262578 A CN 201410262578A CN 104016357 B CN104016357 B CN 104016357B
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Abstract
The present invention relates to industrial residue method of comprehensive utilization, specifically, relate to a kind of manganese slag for comprehensive and utilize the method for producing industrial chemicals.The present invention adopts chemical method to decompose manganese slag, the valuable element in manganese slag is effectively extracted by steps such as reaction, absorption, neutralization, release, crystallizations, and fully utilize various valuable element production basis industrial chemicals, can not only realize turning waste into wealth, and greatly can reduce the secondary pollution of manganese slag to environment.
Description
Technical field
The present invention relates to industrial residue method of comprehensive utilization, specifically, relate to a kind of manganese slag for comprehensive and utilize the method for producing industrial chemicals.
Background technology
In prior art, the method extracting manganese element from manganese ore mainly contains pickling process and flue gas desulfurization process.Wherein, pickling process mainly utilizes sulfuric acid to leach the manganese element in manganese ore, produces a large amount of waste residue containing silicon, aluminium, manganese element after leaching; Flue gas desulfurization process utilizes the sulphur-containing exhaust gas of the discharges such as power plant and manganese ore slurry to carry out reaction to produce manganous sulfate, can produce a large amount of waste residue containing valuable elements such as silicon, aluminium, manganese equally.
At present, China mainly concentrates on cement additire, concrete promotor, other fertilizer of blending as manganese fertilizer, as roadbed material etc. to the utilization of manganese slag.Such as: 1, publication number is disclose a kind of manganese slag lightweight aggregate wall block in the patent of invention open source literature of CN101831980A, as binding agent with cement, with manganese slag as light skeletal, with volcanic tuff stone flour as stopping composition, with flyash as cement retardative material, use water as blender, through mix and blend, compacting, maintenance, make walling unit; 2, publication number is disclose a kind of Meng Zha composite fertilizer and preparation method thereof in the patent of invention open source literature of CN102674965A, manganese ore leached mud is used to be main raw material, adding carbonato chemical fertilizer makes the calcium sulfate in manganese slag be converted into calcium carbonate, then with containing the additive of xylogen and the fertilizer of wanting that is made up of one or more in nitrogenous fertilizer, phosphate fertilizer, potash fertilizer three prepares Meng Zha composite fertilizer.
In addition, to the utilization of manganese slag also have by washing or again acidleach manganese slag reclaim manganese element wherein.Such as: publication number is a kind of method disclosing leaching of manganese from Mn-rich slag in the patent of invention open source literature of CN102367522A, comprises the following steps: a) mixed with metallurgical manganese and sulfurous iron ore powder by described Mn-rich slag, obtains rich manganese mixed powder; B) make sulphuric acid soln mix with described rich manganese mixed powder, obtain slurry; And carry out pressure leaching while c) described slurry being stirred, and the slurry after leaching is filtered, obtain leach liquor and filter residue.
But, but no matter be that manganese slag is used agriculturally or building aspect, all do not make the valuable element in manganese slag be fully utilized, cause the waste of a large amount of available resources and the secondary pollution of environment.Thus, find the valuable element such as manganese, silicon, iron, aluminium in a set of comprehensive utilization manganese slag, the technique producing industrial chemicals is the task of top priority.
Summary of the invention
The object of the invention is to, provide a kind of manganese slag for comprehensive to utilize the method for producing industrial chemicals, to solve above-mentioned technical problem.
For achieving the above object, the technical solution adopted in the present invention is:
Manganese slag for comprehensive utilizes a method of producing industrial chemicals, it is characterized in that: comprise the following steps:
1, react: first manganese ground-slag is broken to 80-200 order, is then that the ammonium fluoride solution of 10%-35% mixes with concentration, is placed in main reaction still reacting by heating 0.5-2.5 hour; Described manganese slag mixes according to the ratio that mass volume ratio is 1:0.2-8 with ammonium fluoride solution; Solid-liquid separation after reaction, obtains solid A and liquid A;
2, absorb: the gas produced in reaction process described in step 1 is absorbed by condenser, obtains liquid B;
3, neutralize: liquid A, liquid B are mixed according to the ratio that mass volume ratio is 1:0.5-2:0.1-1 with neutralizing agent, fully after reaction, obtain white carbon black suspension liquid; Solid-liquid separation, obtains white carbon black and liquid C, and liquid C, after adjusting agent process, returns in main reaction still as auxiliary agent; Described adjusting agent is ammoniacal liquor;
4, discharge: in solid A, add releasing agent various plasma diffusing W,Mo is gone out, then add neutralizing agent by twice and obtain ironic hydroxide, aluminium hydroxide, manganese sulfate solution; The sulfuric acid of described releasing agent to be concentration be 60%-98%;
5, crystallization: manganese sulfate solution step 4 obtained is concentrated by single-action or Multi-effect concentration device, then, at high temperature separates out manganous sulfate solid.
say further:
In described step 1, temperature of reaction is 80 DEG C-110 DEG C.
In described step 3,4, described neutralizing agent is sodium hydroxide or ammoniacal liquor.
In described step 2, described condenser is shell and tube heat exchanger, tube-sheet heat exchanger, packed absorber or spray absorber.
In described step 3, the temperature of reaction is 50 DEG C-90 DEG C.
beneficial effect:compared with prior art, the present invention adopts chemical method to decompose manganese slag, the valuable element in manganese slag is effectively extracted by steps such as reaction, absorption, neutralization, release, crystallizations, and fully utilize various valuable element production basis industrial chemicals, can not only realize turning waste into wealth, and greatly can reduce the secondary pollution of manganese slag to environment.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described with concrete enforcement embodiment.
embodiment 1:
With reference to Fig. 1, manganese slag for comprehensive described in the present embodiment utilizes the method for producing industrial chemicals, comprises the following steps:
1, react: first manganese ground-slag is broken to 80 orders, be then that the ammonium fluoride solution of 10% mixes with concentration, be placed in main reaction still reacting by heating 0.5 hour, temperature of reaction is 80 DEG C; Described manganese slag mixes according to the ratio that mass volume ratio is 1:8 with ammonium fluoride solution; Solid-liquid separation after reaction, obtains solid A and liquid A;
2, absorb: the gas produced in reaction process described in step 1 is absorbed by shell and tube heat exchanger, obtains liquid B;
3, neutralize: liquid A, liquid B are mixed according to the ratio that mass volume ratio is 1:0.5:0.1 with sodium hydroxide solution, after fully reacting under 50 DEG C of temperature condition, obtain white carbon black suspension liquid; Solid-liquid separation, obtains white carbon black and liquid C; Liquid C, after ammonia treatment, returns in main reaction still as auxiliary agent;
4, discharge: in solid A, add releasing agent various plasma diffusing W,Mo is gone out, then add neutralizing agent by twice and obtain ironic hydroxide, aluminium hydroxide, manganese sulfate solution; Described releasing agent to be concentration be 60% sulfuric acid;
5, crystallization: manganese sulfate solution step 4 obtained is concentrated by single-action or Multi-effect concentration device, then, at high temperature separates out manganous sulfate solid.
embodiment 2:
With reference to Fig. 1, manganese slag for comprehensive described in the present embodiment utilizes the method for producing industrial chemicals, comprises the following steps:
1, react: first manganese ground-slag is broken to 150 orders, be then that the ammonium fluoride solution of 20% mixes with concentration, be placed in main reaction still reacting by heating 1.5 hours, temperature of reaction is 90 DEG C; Described manganese slag mixes according to the ratio that mass volume ratio is 1:4 with ammonium fluoride solution; Solid-liquid separation after reaction, obtains solid A and liquid A;
2, absorb: the gas produced in reaction process described in step 1 is absorbed by packed absorber, obtains liquid B;
3, neutralize: liquid A, liquid B are mixed according to the ratio that mass volume ratio is 1:1:0.5 with sodium hydroxide solution, after fully reacting under 70 DEG C of temperature condition, obtain white carbon black suspension liquid; Solid-liquid separation, obtains white carbon black and liquid C; Liquid C, after ammonia treatment, returns in main reaction still as auxiliary agent;
4, discharge: in solid A, add releasing agent various plasma diffusing W,Mo is gone out, then add neutralizing agent by twice and obtain ironic hydroxide, aluminium hydroxide, manganese sulfate solution; Described releasing agent to be concentration be 80% sulfuric acid;
5, crystallization: manganese sulfate solution step 4 obtained is concentrated by single-action or Multi-effect concentration device, then, at high temperature separates out manganous sulfate solid.
embodiment 3:
With reference to Fig. 1, manganese slag for comprehensive described in the present embodiment utilizes the method for producing industrial chemicals, comprises the following steps:
1, react: first manganese ground-slag is broken to 200 orders, be then that the ammonium fluoride solution of 35% mixes with concentration, be placed in main reaction still reacting by heating 2.5 hours, temperature of reaction is 110 DEG C; Described manganese slag mixes according to the ratio that mass volume ratio is 1:0.2 with ammonium fluoride solution; Solid-liquid separation after reaction, obtains solid A and liquid A;
2, absorb: the gas produced in reaction process described in step 1 is absorbed by spray absorber, obtains liquid B;
3, neutralize: liquid A, liquid B are mixed according to the ratio that mass volume ratio is 1:2:1 with sodium hydroxide solution, after fully reacting under 90 DEG C of temperature condition, obtain white carbon black suspension liquid; Solid-liquid separation, obtains white carbon black and liquid C; Liquid C, after ammonia treatment, returns in main reaction still as auxiliary agent;
4, discharge: in solid A, add releasing agent various plasma diffusing W,Mo is gone out, then add neutralizing agent by twice and obtain ironic hydroxide, aluminium hydroxide, manganese sulfate solution; Described releasing agent to be concentration be 98% sulfuric acid;
5, crystallization: manganese sulfate solution step 4 obtained is concentrated by single-action or Multi-effect concentration device, then, at high temperature separates out manganous sulfate solid.
More than in conjunction with given specific embodiment, processing method of the present invention is illustrated, but does not form any limitation of the invention.
Claims (5)
1. manganese slag for comprehensive utilizes a method of producing industrial chemicals, it is characterized in that: comprise the following steps:
(1) react: first manganese ground-slag is broken to 80-200 order, is then that the ammonium fluoride solution of 10%-35% mixes with concentration, is placed in main reaction still reacting by heating 0.5-2.5 hour; Described manganese slag mixes according to the ratio that mass volume ratio is 1:0.2-8 with ammonium fluoride solution; Solid-liquid separation after reaction, obtains solid A and liquid A;
(2) absorb: the gas produced in step (1) described reaction process is absorbed by condenser, obtains liquid B;
(3) neutralize: liquid A, liquid B are mixed according to the ratio that mass volume ratio is 1:0.5-2:0.1-1 with neutralizing agent, fully after reaction, obtain white carbon black suspension liquid; Solid-liquid separation, obtains white carbon black and liquid C, and liquid C, after adjusting agent process, returns in main reaction still as auxiliary agent; Described adjusting agent is ammoniacal liquor;
(4) discharge: in solid A, add releasing agent various plasma diffusing W,Mo is gone out, then add neutralizing agent by twice and obtain ironic hydroxide, aluminium hydroxide, manganese sulfate solution; The sulfuric acid of described releasing agent to be concentration be 60%-98%;
(5) crystallization: manganese sulfate solution step (4) obtained is concentrated by single-action or Multi-effect concentration device, then, at high temperature separates out manganous sulfate solid.
2. manganese slag for comprehensive according to claim 1 utilizes the method for producing industrial chemicals, and it is characterized in that: in described step (1), temperature of reaction is 80 DEG C-110 DEG C.
3. manganese slag for comprehensive according to claim 1 utilizes the method for producing industrial chemicals, and it is characterized in that: in described step (3), (4), described neutralizing agent is sodium hydroxide or ammoniacal liquor.
4. manganese slag for comprehensive according to claim 1 utilizes the method for producing industrial chemicals, and it is characterized in that: in described step (2), described condenser is shell and tube heat exchanger, tube-sheet heat exchanger, packed absorber or spray absorber.
5. manganese slag for comprehensive according to claim 1 utilizes the method for producing industrial chemicals, and it is characterized in that: in described step (3), the temperature of reaction is 50 DEG C-90 DEG C.
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| CN104016357B true CN104016357B (en) | 2016-04-13 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104495856A (en) * | 2015-01-14 | 2015-04-08 | 辽宁石化职业技术学院 | Method for preparing white carbon black using bauxite acidolysis waste residues |
| CN106495747A (en) * | 2016-11-03 | 2017-03-15 | 铜仁学院 | A kind of method that manganese slag produces Water-soluble silicon fertilizer |
| CN110790594B (en) * | 2019-10-16 | 2022-07-05 | 北京金钰农丰生态农业发展有限公司 | Method for producing secondary element water-soluble fertilizer from manganese slag |
| CN111847518A (en) * | 2020-06-28 | 2020-10-30 | 广西锰华新能源科技发展有限公司 | Efficient recycling method of silicomanganese slag |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973555A (en) * | 2010-10-20 | 2011-02-16 | 中南民族大学 | Method for preparing white carbon black and manganese fertilizer from manganese leaching residue |
| CN102674965A (en) * | 2012-05-18 | 2012-09-19 | 中南大学 | Manganese residue compound fertilizer and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973555A (en) * | 2010-10-20 | 2011-02-16 | 中南民族大学 | Method for preparing white carbon black and manganese fertilizer from manganese leaching residue |
| CN102674965A (en) * | 2012-05-18 | 2012-09-19 | 中南大学 | Manganese residue compound fertilizer and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 锰浸出渣制备白炭黑的工艺研究;农桂银 等;《湖南有色金属》;20120229;第28卷(第1期);第43-45页 * |
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Effective date of registration: 20200806 Address after: 044602 Fenglingdu Industrial Park, Yuncheng City, Shanxi Province Patentee after: Shanxi Shengjia Chemical Co., Ltd Address before: 561011 Guizhou province Tongren area water Bijiang District of Tongren City Road No. 103 Patentee before: TONGREN University |