CN109433213A - A kind of method of red mud selectivity dealkalize and enriched iron - Google Patents
A kind of method of red mud selectivity dealkalize and enriched iron Download PDFInfo
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- CN109433213A CN109433213A CN201811446397.1A CN201811446397A CN109433213A CN 109433213 A CN109433213 A CN 109433213A CN 201811446397 A CN201811446397 A CN 201811446397A CN 109433213 A CN109433213 A CN 109433213A
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- red mud
- acid
- amount
- iron
- reaction
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 32
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 70
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 239000007787 solid Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 14
- 239000003513 alkali Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000004876 x-ray fluorescence Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims 1
- 238000010298 pulverizing process Methods 0.000 claims 1
- 238000004611 spectroscopical analysis Methods 0.000 claims 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 9
- 229910052782 aluminium Inorganic materials 0.000 abstract description 6
- 229910052719 titanium Inorganic materials 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 3
- 239000002910 solid waste Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 230000000717 retained effect Effects 0.000 abstract 1
- 239000012065 filter cake Substances 0.000 description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- 239000003054 catalyst Substances 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 150000007513 acids Chemical class 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 239000000706 filtrate Substances 0.000 description 9
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 9
- 238000000926 separation method Methods 0.000 description 9
- 238000003828 vacuum filtration Methods 0.000 description 9
- 239000004615 ingredient Substances 0.000 description 8
- 239000011575 calcium Substances 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 238000005554 pickling Methods 0.000 description 5
- 239000000779 smoke Substances 0.000 description 5
- 238000013019 agitation Methods 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 4
- 239000000292 calcium oxide Substances 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 3
- 239000003546 flue gas Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 238000004131 Bayer process Methods 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 235000019738 Limestone Nutrition 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 229910052663 cancrinite Inorganic materials 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002506 iron compounds Chemical class 0.000 description 1
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052665 sodalite Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Treatment Of Sludge (AREA)
Abstract
本发明涉及一种赤泥选择性脱碱并富集铁的方法，属于环境保护及固废回收利用领域，选择性的脱除赤泥中所含有的碱性物质，使其中碱性物质基本完全去除，而氧化铁成分基本完全保留，从而达到富集铁的效果。通过控制反应酸量、液固比、搅拌时间和温度等参数，使赤泥中所含有的碱性物质与酸尽可能反应，并通过过滤的方式将碱性物质转移到溶液中，而在整个反应过程中，氧化铁成分基本保持原有含量，达到相对富集的目的。通过控制反应的进程使得到的赤泥中的铁的含量较高，同时保留适当组成的Al、Ti等金属元素。
The invention relates to a method for selective dealkalization and iron enrichment of red mud, which belongs to the field of environmental protection and solid waste recycling, and selectively removes alkaline substances contained in red mud, so that the alkaline substances in it are basically completely removed, while the iron oxide component is basically completely retained, thereby achieving the effect of enriching iron. By controlling the reaction acid amount, liquid-solid ratio, stirring time and temperature and other parameters, the alkaline substances contained in the red mud can react with the acid as much as possible, and the alkaline substances can be transferred to the solution by filtration, while the whole During the reaction process, the iron oxide component basically maintains the original content to achieve the purpose of relative enrichment. By controlling the process of the reaction, the content of iron in the obtained red mud is relatively high, while retaining appropriate composition of metal elements such as Al and Ti.
Description
Technical field
The invention belongs to environmental protection and solid waste recycling fields, and in particular to a kind of red mud selectivity dealkalize is simultaneously enriched with
The method of iron.
Background technique
Red mud is the solid waste generated in aluminum oxide industry production process, and current global red mud adds up volume of cargo in storage
4,000,000,000 tons are alreadyd exceed, Chinese production quantity is increased with the speed more than 70,000,000 tons/year, and adding up volume of cargo in storage is more than 500,000,000 tons.Mesh
The comprehensive utilization ratio of red mud is no more than 10% in preceding global range, can only be stacked and be handled with the stockyard of large area, resource wave
Also ecological environment is caused potentially to seriously threaten while expense.Valuable metal element resource rich in red mud, mainly
Chemical component includes Fe2O3、SiO2、Al2O3、TiO2、Na2O, CaO etc. is a kind of important secondary with potential using value
Resource.But the feature that red mud alkalinity is high, salinity is strong comprehensively utilize metallic element therein cannot, constrain the money of red mud
Sourceization development.It is the Main way for solving red mud integrated application that red mud alkalinity, which is adjusted and reduced,.About containing 20%~50% in red mud
Iron oxide, the iron oxide content in iron red mud are even as high as 65% or more, as can removing alkaline matter therein, retain red iron
Mine ingredient, obtained material can be used as iron-smelting raw material, iron-based carrier or catalyst carry out using.Currently, the method for red mud dealkalization
WATER-WASHING METHOD, limestone-based process, ion exchange method, salt lixiviation process, acid leaching process etc. are mostly used, but these methods are in removing basic species
While matter, the loss that a large amount of valuable elements include Fe is also resulted in, forms secondary pollution and the wasting of resources.
The effective component for adequately utilizing red mud, the comprehensive utilization for carrying out red mud is larger problem in red mud reuse.
Summary of the invention
For above-mentioned problems of the prior art, the object of the present invention is to provide a kind of red mud selectivity dealkalize and richnesses
Collect the method for iron.Alkaline matter contained in the removing red mud of selectivity, make wherein alkaline matter substantially completely remove, and oxygen
Change ferrous components substantially completely to retain, to achieve the effect that enriched iron.By control reaction acid amount, liquid-solid ratio, mixing time and
The parameters such as temperature react alkaline matter contained in red mud as far as possible with acid, and by alkaline matter by way of filtering
It is transferred in solution, and in entire reaction process, iron oxide composition keeps original content substantially, reaches the mesh of opposite enrichment
's.
In order to solve the above technical problems, the technical solution of the present invention is as follows:
A kind of method of red mud selectivity dealkalize and enriched iron, specific steps are as follows:
1) each element content contained by red mud is analyzed, according to the general chemical valence state selected under acid system, it is complete to calculate red mud
The dosage of the acid consumed needed for reaction calculates the sour dosage consumed needed for contained alkaline matter in red mud；
2) red mud drying crushes, and smashed red mud and acid-mixed are closed；
The acid amount is that red mud reacts the 30%-80% that need to consume theoretical acid amount completely, and acid is measured control in red mud alkali
Property substance reacted between the 200%-600% of consumption acids amount completely, control solid-to-liquid ratio be 3-15:1.
3) red mud and the mixed mixed liquor of acid are filtered, washs to neutrality, dry red mud filter cake.
The dosage of above-mentioned acid refers to mole, and it is complete that red mud reacts the elements such as Fe, Al, Ca, Na, Ti, the K referred in red mud completely
Full response, the alkaline matter are the compound of the predominantly elements such as Na, Ca, mainly include sodalite, cancrinite and slaked lime
Garnet etc..
The method of the dealkalize red mud of the application preparation is by the sour ratio with red mud of control, according under selected acid system
General chemical valence state, according to following formula: Mn++Ab-=MAn/b(wherein, Mn+Represent metal ion, Ab-Represent selected acid group from
Son) it is calculated, red mud is carried out being crushed to mesh number appropriate first, guarantees that ingredient sufficiently dissolves in red mud, then by not
Disconnected test obtains the suitable acid amount under the mesh number that this red mud crushes, and selected acid amount is according in obtained dealkalize red mud
The content of Fe, Al, Ca, Na, Ti element be determined, retain iron to the greatest extent, while retaining suitable Al and Ti.
Preferably, the type of each element in the step 1) before red mud dealkalization and content are analyzed by X-ray fluorescence spectra
(X Ray Fluorescence) analysis measurement.
Preferably, red mud is crushed to 60-200 mesh after drying in the step 2).
The purpose of crushing is the contact area in order to improve red mud and acid solution.
Preferably, the amount of acid described in the step 2) reacts the 30%-50% that need to consume theoretical acid amount for red mud completely, and
By acid amount control between the 300%-500% that red mud alkaline matter reacts consumption acids amount completely.
Preferably, control solid-to-liquid ratio is 8:1 in the step 2).
Control liquid-solid ratio purpose dissolves red mud sufficiently, conducive to stirring and reacting uniform.
Preferably, in the step 2) hybrid reaction temperature at 30-100 DEG C；Preferably 70-80 DEG C.
Control temperature be make acid-base neutralization reaction velocity-stabilization and W-response process it is controllable, higher temperature can be appropriate
Promote reaction to carry out, reduces the reaction time.
Preferably, mixing time is 20-300 minutes in the step 2)；Preferably 100-150 minutes.
Preferably, the time of dry red mud filter cake is 6-10h in the step 3).
Above-mentioned preparation method obtains the red mud after dealkalize.
Beneficial effects of the present invention:
The red mud dealkalization method of the application compared with the prior art, eliminates the unwanted contributions in red mud, remaining has
The red mud ingredient of preferable catalytic activity, rationally controls the relationship of the amount of sour dosage and red mud, and the ratio of acid is added by control
The dealkalize red mud of utmostly enriched iron is obtained, simultaneously the metallic elements such as Al, Ti containing proper composition；
Obtained red mud matrix loose cellular structure and biggish specific surface area, are conducive to adsorption reaction and heat transfer
The progress of mass transfer.
The difference of control acid amount and control Ph: controlling the Ph value of solution, is the process reacted in acid with the ingredient in red mud
It is controlled, the acid amount for participating in reaction is related with final amount of solution, is unable to control the absolute magnitude of acid used.The application is logical
After the content for first analyzing the ingredient in red mud, acid needed for calculating red mud is measured, and the application is selected according to reaction principle, this
Apply containing a large amount of ferriferous oxide in the catalyst of preparation, because of Fe2O3Reaction is not involved in substantially under weak acid, so control
Acid amount is exactly the reaction process for controlling each ingredient and acid, and reaction process difference directly affects containing for remaining ingredient in red mud
Amount；The amount of acid used in another aspect considers a balance of dealkalize process, if tartaric acid amount is higher, although more Ca can be removed
And Na, but the iron content in remaining residue will be lost, so acid amount needs control could as far as possible within the scope of one
More obtains ferro element.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation are not constituted an undue limitation on the present application for explaining the application.
Attached drawing 1 is red mud dealkalization processing technological flow figure；
Attached drawing 2 is pickling red mud compared with original red mud aperture.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
Below with reference to embodiment, the present invention is further described
The source of substance and instrument in following embodiment is as follows:
Bayer process red mud picks up from Chalco Shandong Co., Ltd；
Hydrochloric acid analyzes pure, Tianjin Ke Miou chemical reagent Co., Ltd；
Sulfuric acid analyzes pure, Tianjin Ke Miou chemical reagent Co., Ltd；
Nitric acid analyzes pure, Tianjin Ke Miou chemical reagent Co., Ltd；
Citric acid analyzes pure, Tianjin Ke Miou chemical reagent Co., Ltd；
Magnetic agitation water-bath, DF-110S, Shanghai Li Chen Instrument Ltd.；
Blowing-type drying box, GZX-9070MBE, Shanghai Bo Xun Industrial Co., Ltd.；
Vacuum pump using circulatory water, SHZ-D (III), Shanghai Li Chen Instrument Ltd..
Embodiment 1
20g red mud is taken, taking hydrochloric acid dosage is that the complete reaction theory of red mud consumes the 30% of dosage, and acid amount is red mud basic species
Matter reacts the 310% of consumption acids amount completely, is diluted to liquid-solid ratio 7:1 with deionized water, red mud is dissolved in solution, and magnetic force is arranged
80 DEG C of water-bath bath temperature of stirring, red mud solution, which is placed in water-bath, to be continuously stirred 1 hour, then takes out vacuum filtration solid-liquid
Separation obtains red mud filter cake and is placed in 100 DEG C drying 12 hours in blowing-type drying box, obtains sample A.It is detected and is taken out by ICP-AES
Material component content contained in filtrate calculates each material composition residual quantity of red mud.
Embodiment 2
20g red mud is taken, taking nitric acid dosage is that the complete reaction theory of red mud consumes the 30% of dosage, and acid amount is red mud basic species
Matter reacts the 310% of consumption acids amount completely, is diluted to liquid-solid ratio 7:1 with deionized water, red mud is dissolved in solution, and magnetic force is arranged
80 DEG C of water-bath bath temperature of stirring, red mud solution, which is placed in water-bath, to be continuously stirred 2 hours, then takes out vacuum filtration solid-liquid
Separation obtains red mud filter cake and is placed in 100 DEG C drying 12 hours in blowing-type drying box, obtains sample B.It is detected and is taken out by ICP-AES
Material component content contained in filtrate calculates each material composition residual quantity of red mud.
Embodiment 3
20g red mud is taken, taking sulfuric acid dosage is that the complete reaction theory of red mud consumes the 30% of dosage, and acid amount is red mud basic species
Matter reacts the 310% of consumption acids amount completely, is diluted to liquid-solid ratio 8:1 with deionized water, red mud is dissolved in solution, and magnetic force is arranged
90 DEG C of water-bath bath temperature of stirring, red mud solution, which is placed in water-bath, to be continuously stirred 1 hour, then takes out vacuum filtration solid-liquid
Separation obtains red mud filter cake and is placed in 100 DEG C drying 12 hours in blowing-type drying box, obtains sample C.It is detected and is taken out by ICP-AES
Material component content contained in filtrate calculates each material composition residual quantity of red mud.
Embodiment 4
20g red mud is taken, taking hydrochloric acid dosage is that the complete reaction theory of red mud consumes the 40% of dosage, and acid amount is red mud basic species
Matter reacts the 440% of consumption acids amount completely, is diluted to liquid-solid ratio 10:1 with deionized water, red mud is dissolved in solution, and magnetic is arranged
Power stirs 80 DEG C of water-bath bath temperature, and red mud solution, which is placed in water-bath, to be continuously stirred 1 hour, and it is solid then to take out vacuum filtration
Liquid separation obtains red mud filter cake and is placed in 100 DEG C drying 12 hours in blowing-type drying box, obtains sample D.It is detected by ICP-AES
Material component content contained in smoke filtrate calculates each material composition residual quantity of red mud.
Embodiment 5
20g red mud is taken, taking hydrochloric acid dosage is that the complete reaction theory of red mud consumes the 50% of dosage, and acid amount is red mud basic species
Matter reacts the 560% of consumption acids amount completely, is diluted to liquid-solid ratio 15:1 with deionized water, red mud is dissolved in solution, and magnetic is arranged
Power stirs 60 DEG C of water-bath bath temperature, and red mud solution, which is placed in water-bath, to be continuously stirred 1 hour, and it is solid then to take out vacuum filtration
Liquid separation obtains red mud filter cake and is placed in 100 DEG C drying 12 hours in blowing-type drying box, obtains sample E.It is detected by ICP-AES
Material component content contained in smoke filtrate calculates each material composition residual quantity of red mud.
Embodiment 6
20g red mud is taken, taking sulfuric acid dosage is that the complete reaction theory of red mud consumes the 40% of dosage, and acid amount is red mud basic species
Matter reacts the 460% of consumption acids amount completely, is diluted to liquid-solid ratio 10:1 with deionized water, red mud is dissolved in solution, and magnetic is arranged
Power stirs 40 DEG C of water-bath bath temperature, and red mud solution, which is placed in water-bath, to be continuously stirred 1 hour, and it is solid then to take out vacuum filtration
Liquid separation obtains red mud filter cake and is placed in 100 DEG C drying 12 hours in blowing-type drying box, obtains sample F.It is detected by ICP-AES
Material component content contained in smoke filtrate calculates each material composition residual quantity of red mud.
Embodiment 7
20g red mud is taken, taking Citric Acid Dosage is that the complete reaction theory of red mud consumes the 30% of dosage, and acid amount is red mud alkalinity
Substance reacts the 280% of consumption acids amount completely, is diluted to liquid-solid ratio 15:1 with deionized water, red mud is dissolved in solution, setting
40 DEG C of magnetic agitation water-bath bath temperature, red mud solution, which is placed in water-bath, to be continuously stirred 2 hours, then takes out vacuum filtration
It is separated by solid-liquid separation, obtains red mud filter cake and be placed in 100 DEG C drying 12 hours in blowing-type drying box, obtain sample G.It is examined by ICP-AES
Material component content contained in smoke filtrate is surveyed, each material composition residual quantity of red mud is calculated.
Each component residue surplus (ICP-AES retrospectively calculate) in the red mud sample that 1 embodiment 1-7 of table is prepared
Ingredient comparison (XRF analysis) before and after 2 red mud dealkalization of table
Specific surface area comparison (BET analysis) before and after 3 red mud dealkalization of table
Both table 1 and table 2 confirm each other, and the alkaline matter contained in red mud is substantially all in acid cleaning process to be transferred to
In filtrate, and iron compound is not affected by the influence of pickling substantially, thus Fe in the red mud filter cake being obtained by filtration2O3Content is opposite to be mentioned
Height, increase rate are greater than 40%, achieve the purpose that selective dealkalize and relatively enriched iron.In red mud filter cake, with Fe, Al, Ti,
Based on the oxide of 4 kinds of elements such as Si exists, good condition is created to utilization of the red mud in terms of catalyst.Fe2O3It is one
The denitrating catalyst active constituent of kind high-efficiency environment friendly, and Al2O3、TiO2With SiO2It is all good carrier material.As shown in Figure 2,
Pickling does not generate the influence of essence to the pore-size distribution of red mud, still falls within macroporous structure material, but in acid cleaning process,
The duct of red mud is also dredged while alkaline matter removes, and specific surface area substantially improves.
Embodiment 8
The sample A for taking 20g embodiment 1 to obtain, 1.2 times of acid amount used, are diluted to liquid-solid ratio 5:1's in Example 1
Acid solution stirs evenly after red mud is added；The chromic nitrate of ferro element mole contained by 1/6 red mud is added in solution, is kept for 50 DEG C, stirred
It mixes 4 hours；It using ammonia water titration solution to Ph most 9, then filters, washing to neutrality obtains the composite red mud of chromium doping；
Composite red mud filter cake after drying is placed in Muffle furnace, air atmosphere is kept, 550 DEG C is chosen and calcines 3 hours, room temperature to be down to
After take out, grinding is broken, and screening catalyst particle to 40 mesh obtains de- red mud denox catalyst sample J.
Embodiment 9
The sample D that Example 4 obtains, 1.5 times of acid amount used in Example 4, the acid for being diluted to liquid-solid ratio 5:1 is molten
Liquid stirs evenly after red mud is added；The chromic nitrate of ferro element mole contained by 1/8 red mud is added in solution, is kept for 60 DEG C, stirring 3
Hour；It using ammonia water titration solution to Ph most 9, then filters, washing to neutrality obtains the composite red mud of chromium doping；It will
Composite red mud filter cake after drying is placed in Muffle furnace, keeps air atmosphere, is chosen 530 DEG C and is calcined 5 hours, wait be cooled to room temperature
It takes out, grinding is broken, and screening catalyst particle to 60 mesh obtains red mud denitrating catalyst sample K.
Comparative example 1
20g red mud is taken, liquid-solid ratio 7:1 is diluted to deionized water, red mud is dissolved in solution, magnetic agitation water-bath is set
80 DEG C of bath temperature of pot, hydrochloric acid is instilled in red mud solution and final solution pH value keeps PH=4, is placed in water-bath and is continuously stirred
It 1 hour, then takes out vacuum filtration and is separated by solid-liquid separation, obtain red mud filter cake and be placed in 100 DEG C drying 12 hours in blowing-type drying box, obtain
To sample L.Each main component residual content is (Fe:64.25% in sample L；Al:60.73%；Ca:15.68%；Na:
4.62%).
Control pH value be likely to result in participated in solution reaction total acid content it is excessive, although dealkalize effect is fine, cause
A large amount of losses of ferro element.
Comparative example 2-comparison acid amount is 180%, then adds the technical solution that calcium oxide carries out dealkalize
20g red mud is taken, liquid-solid ratio 7:1 is diluted to deionized water, red mud is dissolved in solution, magnetic agitation water-bath is set
80 DEG C of bath temperature of pot, taking hydrochloric acid dosage is that the complete reaction theory of red mud consumes the 20% of dosage, and acid amount is red mud alkaline matter
The 180% of reaction consumption acids amount completely, then adds calcium oxide dealkalize, and red mud solution is placed in water-bath that continuously stir 1 small
When, it then takes out vacuum filtration and is separated by solid-liquid separation, obtain red mud filter cake and be placed in 100 DEG C drying 12 hours in blowing-type drying box, obtain
Sample H.By ICP-AES detect smoke filtrate contained in material component content, calculate each material composition residual quantity of red mud (Fe:
85.79%；Al:71.48%；Ca:213.24%；Na:5.73%).
Be added calcium oxide after, partial oxidation calcium fails sufficiently to react, through deionized water wash part remain, instead it is possible that
Increase ratio containing alkaloid substance in red mud.
Comparative example 3
It is distinguished as comparative example 1 obtained sample L filter cake being placed in Muffle furnace with comparative example 1, keeps air atmosphere,
It chooses 550 DEG C to calcine 4 hours, be taken out wait be cooled to room temperature, grinding is broken, and screening catalyst particle to 60 mesh obtains red mud denitration
Catalyst sample.
Catalytic test
The red mud denitrating catalyst of embodiment 8 and embodiment 9 carries out the denitrating flue gas rate that denitrating flue gas obtains
4 catalyst sample removal of nitrogen oxide evaluation of result of table
It is available in Fig. 2, based on the pore-size distribution of the original red mud before dealkalize is distributed with macropore, specific surface area compared with
It is low；The pore-size distribution of red mud after pickling and original red mud are essentially identical, the red mud specific surface area based on macropore, after pickling
It increases.For denitrating flue gas reaction principle, the pore-size distribution of composite red mud is more advantageous to the progress of reduction reaction, thus
Denitration efficiency is improved, temperature window is widened.
The foregoing is merely preferred embodiment of the present application, are not intended to limit this application, for the skill of this field
For art personnel, various changes and changes are possible in this application.Within the spirit and principles of this application, made any to repair
Change, equivalent replacement, improvement etc., should be included within the scope of protection of this application.
Claims (10)
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