CN106745290B - A kind of technique for applying of manganese spar - Google Patents
A kind of technique for applying of manganese spar Download PDFInfo
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- CN106745290B CN106745290B CN201710034902.0A CN201710034902A CN106745290B CN 106745290 B CN106745290 B CN 106745290B CN 201710034902 A CN201710034902 A CN 201710034902A CN 106745290 B CN106745290 B CN 106745290B
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- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 36
- 239000011572 manganese Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 19
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 43
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 37
- VASIZKWUTCETSD-UHFFFAOYSA-N oxomanganese Chemical compound [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002386 leaching Methods 0.000 claims abstract description 15
- ISPYRSDWRDQNSW-UHFFFAOYSA-L manganese(II) sulfate monohydrate Chemical compound O.[Mn+2].[O-]S([O-])(=O)=O ISPYRSDWRDQNSW-UHFFFAOYSA-L 0.000 claims abstract description 14
- 239000002893 slag Substances 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 239000000706 filtrate Substances 0.000 claims abstract description 9
- 229940099596 manganese sulfate Drugs 0.000 claims abstract description 9
- 235000007079 manganese sulphate Nutrition 0.000 claims abstract description 9
- 239000011702 manganese sulphate Substances 0.000 claims abstract description 9
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims abstract description 9
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003546 flue gas Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 8
- 235000011149 sulphuric acid Nutrition 0.000 claims abstract description 7
- 239000001117 sulphuric acid Substances 0.000 claims abstract description 7
- 230000009257 reactivity Effects 0.000 claims abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 5
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 5
- 230000008569 process Effects 0.000 claims abstract description 5
- 238000002425 crystallisation Methods 0.000 claims abstract description 4
- 230000008025 crystallization Effects 0.000 claims abstract description 4
- 238000004821 distillation Methods 0.000 claims abstract description 3
- 239000012065 filter cake Substances 0.000 claims abstract description 3
- 238000003801 milling Methods 0.000 claims abstract description 3
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 3
- 238000004073 vulcanization Methods 0.000 claims abstract description 3
- 230000003647 oxidation Effects 0.000 claims abstract 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- 239000005864 Sulphur Substances 0.000 claims description 4
- 238000010304 firing Methods 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 2
- 235000003283 Pachira macrocarpa Nutrition 0.000 claims 1
- 241001083492 Trapa Species 0.000 claims 1
- 235000014364 Trapa natans Nutrition 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 235000009165 saligot Nutrition 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract description 2
- 230000035800 maturation Effects 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 11
- 239000002994 raw material Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 235000006748 manganese carbonate Nutrition 0.000 description 2
- 239000011656 manganese carbonate Substances 0.000 description 2
- 229940093474 manganese carbonate Drugs 0.000 description 2
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- GSFSVEDCYBDIGW-UHFFFAOYSA-N 2-(1,3-benzothiazol-2-yl)-6-chlorophenol Chemical compound OC1=C(Cl)C=CC=C1C1=NC2=CC=CC=C2S1 GSFSVEDCYBDIGW-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- IXHOXXFTTQTNQS-UHFFFAOYSA-N [Ca].[Na].[K] Chemical compound [Ca].[Na].[K] IXHOXXFTTQTNQS-UHFFFAOYSA-N 0.000 description 1
- GOPYZMJAIPBUGX-UHFFFAOYSA-N [O-2].[O-2].[Mn+4] Chemical class [O-2].[O-2].[Mn+4] GOPYZMJAIPBUGX-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 150000002696 manganese Chemical class 0.000 description 1
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 1
- ZWXOQTHCXRZUJP-UHFFFAOYSA-N manganese(2+);manganese(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Mn+2].[Mn+3].[Mn+3] ZWXOQTHCXRZUJP-UHFFFAOYSA-N 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- KNLQKHUBPCXPQD-UHFFFAOYSA-N manganese;sulfuric acid Chemical compound [Mn].OS(O)(=O)=O KNLQKHUBPCXPQD-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/10—Sulfates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of technique for applying of manganese spar, specifically include：(1) manganese spar is milled and obtains manganese sulfate solution and leached mud through leaching oxidation neutralization vulcanization press filtration；(2) manganese sulfate solution is delivered into electrolytic manganese dioxide workshop to be electrolysed, stripped rinsing neutralization is dried to obtain electrolytic manganese dioxide；(3) by electrolytic manganese dioxide with reducing agent is baking mixed obtains manganese monoxide, filtrate is back to Leaching of rhodochrosite ore after washing press filtration again, and adding sulfuric acid in filter cake is leached, and ore pulp carries out press filtration, filter residue is returned and is calcined again, and filtrate carries out distillation crystallization and obtains manganese sulfate monohydrate；(4) leached mud is dried, then slag reactivity powder is obtained through high-temperature roasting cooling milling；(5) industrial sulphuric acid is made respectively in flue gas caused by (3) (4) and analytical pure sulfuric acid is recycled.There are the present invention simple industrial flow, each link process equipment maturation, good product quality, the three wastes to be effectively addressed, resource utilization height, high financial profit.
Description
Technical field
The present invention relates to a kind of field of chemical preparation, specifically a kind of technique for applying of manganese spar.
Background technology
World's manganese resource very abundant, Oreforming age are recorded to the ground of each different geologic ages in the Quaternary Period from preceding Cambrian epoch
Layer has manganese ore deposit distribution.The manganese ore reserves with economic value for being available for utilization are about hundred million tons of 9-10, and the overwhelming majority is
Oxidized ore, including pyrolusite, hausmannite, braunite etc., it is manganese carbonate ore, i.e. manganese spar to also have part, in addition with some
Manganese ore is with mixed rawore stone, i.e., a variety of miscellaneous lifes of manganese form.
Manganese spar is mainly the raw material for producing electrolytic manganese metal, is also used for preparing high-purity manganese carbonate concentrate, is production sulfuric acid
The primary raw material of manganese, electrolytic manganese metal, activated manganese dioxide, electrolytic manganese dioxide, mangano-manganic oxide etc..It is also used for manufacturing magnetic conduction
Material, it is one of main component of soft magnetic ferrite, is additionally operable to the catalyst of desulfurization, enamel pigment, varnish drier and making
The raw material and feed addictive, health products etc. of other manganese salts.
The manganese spar in China is concentrated mainly on the ground such as Guangxi, Hunan, Guizhou at present, is mainly used in the production of electrolytic manganese.Should
Production technology obtains manganese sulfate solution after the press filtration that cleans, then obtained by being electrolysed only by the manganese in manganese spar through sulfuric acid leaching
Manganese metal, other are all put into the accumulation processing of slag storehouse in the form of sulfate slag.This production technology produces substantial amounts of waste water and waste residue,
Environment and safety of workers are endangered, it is necessary to spend substantial amounts of funds to be handled, and increase production cost.
The content of the invention
It is used to prepare electrolytic manganese dioxide, manganese dioxide roasting reduction it is an object of the invention to provide a kind of manganese spar
High purity manganese sulfate is prepared, leached mud roasting reduction prepares slag reactivity powder, flue gas combined manganese dioxide roasting caused by roasting
The production technology of the flue gas co-producing sulfuric acid of reduction.
To achieve the above object, the present invention provides following technical scheme：
A kind of technique for applying of manganese spar, comprises the following steps：
(1) manganese spar is milled to 100 mesh, the sulfuric acid for neutralizing vulcanization press filtration and being conformed to quality requirements is aoxidized by leaching
Manganese solution and Leaching of rhodochrosite ore slag；
(2) manganese sulfate solution to conform to quality requirements is delivered into electrolytic manganese dioxide workshop to be electrolysed, stripped rinsing
Neutralization is dried to obtain electrolytic manganese dioxide；
(3) by electrolytic manganese dioxide and reducing agent in mass ratio 1：0.45 dispensing is delivered in firing equipment, at 700-900 DEG C
Roasting obtains manganese monoxide, manganese monoxide is directly poured into pure water by liquid-solid ratio 1:3 are washed, and filtrate is back to after press filtration
Leaching of rhodochrosite ore, filter cake are delivered to addition analytical pure sulfuric acid in leaching barrel and leached, and pulp PH value to 5.5 ± 0.2 carries out press filtrations,
Filter residue is back to burden process and is calcined again, and filtrate carries out distillation crystallization and obtains high-purity manganese sulfate monohydrate；
(4) by the drying of Leaching of rhodochrosite ore slag, it is broken be delivered in rotary kiln, control 1100-1200 DEG C of progress high-temperature roasting,
Obtained clinker obtains slag reactivity powder through cooling down milling；
(5) flue gas caused by flue gas combined boiling roaster electrolytic manganese dioxide caused by rotary kiln baking leached mud is pressed
Industrial sulphuric acid and analytical pure sulfuric acid are made respectively according to acid-making process；Industrial sulphuric acid returns to step (1) and recycled, and analyzes bright sulfur
Acid returns to step (3) and recycled.
As the further scheme of the present invention：Reducing agent uses sulphur in step (3).
As the further scheme of the present invention：Firing equipment is fluidized bed furnace in step (3).
As the further scheme of the present invention：Roasting obtains manganese monoxide at 800 DEG C in step (3).
As the further scheme of the present invention：Kiln is rotary kiln in step (4).
As the further scheme of the present invention：1100-1200 DEG C of progress high-temperature roasting of control in step (4).
Compared with prior art, the beneficial effects of the invention are as follows：
(1) the advantage of the invention is that using manganese spar to prepare manganese dioxide and high purity manganese sulfate monohydrate for raw material, for electricity
Pond production provides quality raw materials, improves the economic value of manganese；
(2) the advantage of the invention is that obtaining slag reactivity powder by calcination process to leached mud, resource utilization is improved；
(3) the advantage of the invention is that can be used for the leaching system of manganese spar to industrial sulphuric acid made of flue gas caused by roasting
Manganese sulfate solution needed for standby electrolytic manganese dioxide；Manufactured analytical pure sulfuric acid can be used for the leaching of manganese monoxide to prepare high purity sulphur
Sour manganese；
(4) present invention is made full use of to the manganese in manganese spar, while the three wastes are handled, and improves the utilization of resources
Rate, solve environmental issue, produce economic benefit；
(5) present invention prepares electrolytic manganese dioxide by manganese spar, preferentially eliminates potassium sodium calcium and magnesium, simplifies high-purity sulphuric acid
Manganese production technology；
(6) all techniques and equipment of the present invention have the market of maturation, and controllability is strong, is suitable for scale metaplasia
Production.
Embodiment
Fig. 1 is the technique for applying flow chart of manganese spar.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
It is raw material to take manganese spar, first passes through jaw crusher and is crushed, and then wears into 100 mesh powders with grinding machine, will
Powder is delivered to pulp bucket pulp, is leached subsequently into chemical combination bucket, leaches 3-4h, adds hydrogen peroxide and carries out oxidation reaction
30min, add Sodium Dimethyldithiocarbamate with lime regulation PH to 6.0 or so and remove removing heavy metals, then once slightly pressed secondary pressure-sizing to obtain
To qualified filtrate and filter residue.
Filtrate is delivered to electrolytic manganese dioxide workshop, control electric current density 80-100A/m2,95-100 DEG C of electrolysis temperature
It is electrolysed, the manganese dioxide being deposited on anode is passed through into stripping, crushing, rinsing, neutralization, dry as product.
By manganese dioxide and sulphur in mass ratio 1：0.45 in fluidized bed furnace 800 DEG C of roasting reductions obtain manganese monoxide, use
Analytical pure sulfuric acid is added after pure water and leaches obtained manganese sulfate solution, control ph value of reaction concentrates filtrate to press filtration after 5.5
Crystallization is evaporated obtained high purity manganese sulfate monohydrate
By the drying of Leaching of rhodochrosite ore slag, it is broken be delivered in rotary kiln, control 1100-1200 DEG C of temperature, obtain cellular
Slag, slag reactivity powder is made after grinding.
The fume collection of fluidized bed furnace and rotary kiln is prepared into industrial sulphuric acid and analytical pure sulfuric acid according to sulfuric acid production process.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (6)
1. a kind of technique for applying of manganese spar, it is characterised in that comprise the following steps：
(1) manganese spar is milled to 100 mesh, the manganese sulfate to be conformed to quality requirements by leaching oxidation neutralization vulcanization press filtration is molten
Liquid and Leaching of rhodochrosite ore slag；
(2) manganese sulfate solution to conform to quality requirements is delivered into electrolytic manganese dioxide workshop to be electrolysed, stripped rinsing neutralizes
It is dried to obtain electrolytic manganese dioxide；
(3) by electrolytic manganese dioxide and reducing agent in mass ratio 1：0.45 dispensing is delivered in firing equipment, is calcined at 700-900 DEG C
Manganese monoxide is obtained, manganese monoxide is directly poured into pure water by liquid-solid ratio 1:3 are washed, and filtrate is back to water chestnut manganese after press filtration
Ore deposit leaches, and filter cake is delivered to addition analytical pure sulfuric acid in leaching barrel and leached, and pulp PH value to 5.5 ± 0.2 carries out press filtrations, filter residue
It is back to burden process to be calcined again, filtrate carries out distillation crystallization and obtains high-purity manganese sulfate monohydrate；
(4) by the drying of Leaching of rhodochrosite ore slag, it is broken be delivered in rotary kiln, control 1000-1200 DEG C of progress high-temperature roasting, obtain
Clinker through cool down milling obtain slag reactivity powder；
(5) by flue gas caused by flue gas combined boiling roaster electrolytic manganese dioxide caused by rotary kiln baking leached mud according to system
Industrial sulphuric acid and analytical pure sulfuric acid is made in sour technique respectively；Industrial sulphuric acid returns to step (1) and recycled, and analytical pure sulfuric acid returns
Step (3) is returned to recycle.
2. the technique for applying of manganese spar according to claim 1, it is characterised in that reducing agent uses sulphur in step (3).
3. the technique for applying of manganese spar according to claim 1, it is characterised in that firing equipment is boiling in step (3)
Stove.
4. the technique for applying of manganese spar according to claim 1, it is characterised in that be calcined and obtain at 800 DEG C in step (3)
Manganese monoxide.
5. the technique for applying of manganese spar according to claim 1, it is characterised in that kiln is rotary kiln in step (4).
6. the technique for applying of manganese spar according to claim 1, it is characterised in that 1100-1200 DEG C of control in step (4)
Carry out high-temperature roasting.
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| CN201710034902.0A CN106745290B (en) | 2017-01-17 | 2017-01-17 | A kind of technique for applying of manganese spar |
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Effective date of registration: 20200713 Address after: 416400 Chuangye Avenue, Huayuan County, Xiangxi Tujia and Miao Autonomous Prefecture, Hunan Province Patentee after: Xiangxi Mengcheng Technology Co., Ltd Address before: 416400 Hunan Province, Xiangxi Tujia and Miao Autonomous Prefecture Huayuan County town of Minle Valley Shaocun two group No. 54 Patentee before: Shi Chaojun |
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