CN105727886B - A kind of charcoal ferrotitanium sieve and silica-sesquioxide compound and its preparation method and application - Google Patents
A kind of charcoal ferrotitanium sieve and silica-sesquioxide compound and its preparation method and application Download PDFInfo
- Publication number
- CN105727886B CN105727886B CN201610257241.3A CN201610257241A CN105727886B CN 105727886 B CN105727886 B CN 105727886B CN 201610257241 A CN201610257241 A CN 201610257241A CN 105727886 B CN105727886 B CN 105727886B
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- Prior art keywords
- preparation
- ferrotitanium
- sieve
- silica
- sesquioxide
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 74
- 229910001200 Ferrotitanium Inorganic materials 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 58
- 239000003610 charcoal Substances 0.000 title claims abstract description 23
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 52
- 239000004917 carbon fiber Substances 0.000 claims abstract description 52
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000002002 slurry Substances 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000007787 solid Substances 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000002270 dispersing agent Substances 0.000 claims abstract description 8
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 5
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 5
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 42
- 238000000034 method Methods 0.000 claims description 39
- 230000008569 process Effects 0.000 claims description 28
- 229910052742 iron Inorganic materials 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 13
- 238000007885 magnetic separation Methods 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 13
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 12
- 239000003546 flue gas Substances 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 7
- 238000005188 flotation Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000004065 wastewater treatment Methods 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000003463 adsorbent Substances 0.000 claims description 5
- 229910001108 Charcoal iron Inorganic materials 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- -1 glycol Class compound Chemical class 0.000 claims description 4
- 229910001385 heavy metal Inorganic materials 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 238000004131 Bayer process Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000000197 pyrolysis Methods 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical group [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 238000011033 desalting Methods 0.000 claims description 2
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- 239000002440 industrial waste Substances 0.000 claims description 2
- 150000002505 iron Chemical class 0.000 claims description 2
- 150000007522 mineralic acids Chemical class 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 claims 1
- 229910052783 alkali metal Inorganic materials 0.000 claims 1
- 150000001340 alkali metals Chemical group 0.000 claims 1
- 239000003034 coal gas Substances 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 229940113116 polyethylene glycol 1000 Drugs 0.000 claims 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000000151 deposition Methods 0.000 description 31
- 230000008021 deposition Effects 0.000 description 23
- 238000001179 sorption measurement Methods 0.000 description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 8
- 239000005864 Sulphur Substances 0.000 description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 239000002351 wastewater Substances 0.000 description 7
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 6
- 229910052753 mercury Inorganic materials 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000008929 regeneration Effects 0.000 description 5
- 238000011069 regeneration method Methods 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000003213 activating effect Effects 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000002955 isolation Methods 0.000 description 4
- 238000003701 mechanical milling Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 239000004071 soot Substances 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000008246 gaseous mixture Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- IQXJCCZJOIKIAD-UHFFFAOYSA-N 1-(2-methoxyethoxy)hexadecane Chemical compound CCCCCCCCCCCCCCCCOCCOC IQXJCCZJOIKIAD-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- KMWBBMXGHHLDKL-UHFFFAOYSA-N [AlH3].[Si] Chemical compound [AlH3].[Si] KMWBBMXGHHLDKL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 150000001399 aluminium compounds Chemical class 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229950009789 cetomacrogol 1000 Drugs 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002506 iron compounds Chemical class 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01J20/0211—Compounds of Ti, Zr, Hf
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- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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- 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
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- 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
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- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- Chemical & Material Sciences (AREA)
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- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention provides a kind of charcoal ferrotitanium sieve and silica-sesquioxide compound and its preparation method and application, and the preparation method of the charcoal ferrotitanium sieve and silica-sesquioxide compound is ground to obtain the first slurry the following steps are included: water is added into red mud；Acid for adjusting pH value is added into the first slurry to 2-4, surface dispersant is added, grinds the lower alkaline matter that is added and adjusts pH value to 5-10, obtain the second slurry；Second slurry is separated by solid-liquid separation, solid roasting is obtained into cladded type ferrotitanium sieve and silica-sesquioxide；Cladded type ferrotitanium sieve and silica-sesquioxide is restored under reducing gas atmosphere, the generation of carbon fiber is then carried out under hydrocarbon atmosphere, obtains the charcoal ferrotitanium sieve and silica-sesquioxide compound after cooling.The higher value application of red mud may be implemented in the present invention, has extremely strong commercial application potentiality.
Description
Technical field
The invention belongs to the processing of dangerous solid waste and application fields, are related to a kind of charcoal ferrotitanium sieve and silica-sesquioxide compound
And its preparation method and application.
Background technique
Red mud is that aluminium industry extracts the pollution strong basicity waste residue being discharged when aluminium oxide, average 1 ton of oxidation of every production
Aluminium incidentally generates 1.0~2.0 tons of red muds.A large amount of red mud sufficiently effective cannot utilize, and can only rely on the stockyard heap of large area
It puts, occupies a large amount of soils, serious pollution also is caused to environment.Red mud is classified as dangerous waste by most of country
Object, the generation of red mud causes various influences directly or indirectly to the production of the mankind, life, so to greatest extent
Reduce red mud yield and harm, realize by all kinds of means, the recycling of quantity greatly it is extremely urgent.
Due to containing a large amount of iron oxide in red mud, into red, appearance is similar to redness of the skin or complexion soil, thus gains the name.Red mud
In not only contain iron oxide, go back the ingredients such as silica, aluminium oxide, sodium oxide molybdena.It how to be the height for realizing these ingredients in red mud
Value utilization is the research emphasis of this field, such as discloses in CN102234171A and CN101468866A red mud carrying out dealkalize
The then raw material as production cement；CN101891406A and CN1837121A is disclosed using red mud or after iron is selected in dealkalize
The method that red mud and desulfurized gypsum prepare cement；CN103373815A discloses porous by main material production of Bayer process red mud
Devitrified glass；CN103420359A discloses the method for red mud catalysis preparation carbon nanotube, and red mud passes through in the method
Baking 1-4h, which then crushed 200 meshes, at 101-109 DEG C can be used as catalyst production carbon nanotube；CN102757060A is disclosed
In such a way that lime disappears sodium, wherein aluminium and part ferriferous oxide are then separated, realizes the depth extraction of aluminium compound.However,
In these above-mentioned inventions, the dealkalize of red mud medium alkaline compound or other treatment processes obtain iron oxide therein
It utilizes well.And with red mud directly as carbon fiber catalyst, due to containing a large amount of alkaline matter and chlorine member in raw material
Element, and iron particle partial size is big, it is difficult to have the high activity and high carbon yield of carbon fiber preparation, because without having industrial application
Prospect.Pollution and Synthetical Utilization Situation in conjunction with red mud, it is seen that there are no feasible technologies to realize iron in red mud at this stage
Higher value application method and approach and the high-valued and big red mud application approach of amount.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of charcoal ferrotitanium sieve and silica-sesquioxide compound and its
Preparation method and application.This method prepares the charcoal ferrotitanium silicon-aluminium compound by red mud, which borrows magnetic after crushing
The initial gross separation of charcoal iron compound Yu other oxides may be implemented in separation；Or the compound can be crushed after can directly make
For the adsorbent of the agent of heavy metal in flue gas oxidation-adsorption and purification of waste water, and by Magneto separate, the multiple of the substance may be implemented
Using with regeneration.The method achieve the reasonable higher value applications of red mud, have extremely strong commercial application potentiality.
In order to achieve that object of the invention, the invention adopts the following technical scheme:
On the one hand, the present invention provides a kind of preparation method of charcoal ferrotitanium sieve and silica-sesquioxide compound, the method includes with
Lower step:
(1) water is added into red mud, it is ground to obtain the first slurry；
(2) acid for adjusting pH value is added in the first slurry obtained to step (1) to 2-4, surface dispersant is added, under grinding
Alkaline matter is added and adjusts pH value to 5-10, obtains the second slurry；
(3) the second slurry obtained by step (2) is separated by solid-liquid separation, solid roasting is obtained into the oxidation of cladded type ferrotitanium sial
Object；
(4) cladded type ferrotitanium sieve and silica-sesquioxide is restored under reducing gas atmosphere, then in hydrocarbon gas
The generation that carbon fiber is carried out under atmosphere, obtains the charcoal ferrotitanium sieve and silica-sesquioxide compound.
The present invention utilizes above-mentioned preparation method, prepares charcoal ferrotitanium sieve and silica-sesquioxide compound by red mud, realizes that carbon fiber exists
The growth on ferrotitanium sieve and silica-sesquioxide surface, the compound made have carbon fiber high activity and high carbon yield, may be implemented
The higher value application of red mud has extensive prospects for commercial application.
In preparation method of the present invention, step (1) red mud is Bayer process red mud, sub-molten salt red mud or sintering process
In red mud any one or at least two mixture.
Preferably, the mass ratio of step (1) red mud and the water of addition is 1:(1-5), such as 1:1,1:2,1:3,1:4
Or 1:5.
Preferably, step (1) it is described grinding so that grain diameter be less than or equal to 100nm, such as 100nm, 90nm, 80nm,
70nm, 60nm, 50nm, 40nm, 30nm, 20nm, 10nm, 8nm, 5nm, 3nm or 1nm.
Preferably, the grinding can be ball milling.
Preferably, the time of the grinding be 10-36h, such as 10h, 12h, 14h, 16h, 18h, 20h, 22h, for 24 hours,
26h, 28h, 30h, 32h, 34h or 36h.
Preferably, the solid content of step (1) first slurry be 10-50%, such as 10%, 13%, 15%, 18%,
20%, 25%, 28%, 30%, 35%, 38%, 40%, 45%, 48% or 50%.
Preferably, step (2) acid is inorganic acid or organic acid, it is preferable that the acid can be industrial waste acid.
Preferably, acid for adjusting pH value is added in step (2) into the first slurry to 2-4, for example, 2,2.3,2.5,2.8,3,
3.2,3.5,3.8 or 4.
Preferably, step (2) surface dispersant is polyethylene glycols compound and/or fatty alcohol polyethenoxy ether class
Compound, preferably cetomacrogol 1000.
Preferably, the additive amount of step (2) described surface dispersant is the 0.1-1% of the first slurry gross mass, such as
0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9% or
1%.
Preferably, step (2) described alkaline matter can in alkali metal hydroxide or carbonate any one or
At least two combination, preferably sodium hydroxide and/or sodium carbonate.
Preferably, alkaline matter is added in step (2) and adjusts pH value to 5-10, for example, 5,5.5,6,6.5,7,7.5,8,
8.5,9,9.5 or 10.
When alkaline matter being added in the step (2) adjusting pH value to 5-10, silicoaluminate forms colloidal sol, iron oxygen in solution
Compound nano particle is coated to silicoaluminate surface, realizes the precipitating again of main substance in red mud.
Preferably, the temperature of step (3) described roasting be 400-800 DEG C, such as 400 DEG C, 430 DEG C, 450 DEG C, 480 DEG C,
510℃、530℃、550℃、570℃、600℃、620℃、640℃、660℃、680℃、700℃、720℃、750℃、780℃
Or 800 DEG C.
Preferably, the time of step (3) described roasting be 1-20h, such as 1h, 2h, 3h, 5h, 7h, 9h, 10h, 12h,
14h, 16h, 18h, 19h or 20h.
Preferably, after step (3) is separated by solid-liquid separation obtained water phase carry out desalting processing and it is up to standard after discharged.
Preferably, step (4) reducing gas atmosphere is hydrogen atmosphere.
Preferably, step (4) it is described reduction carried out at 500-800 DEG C, such as 500 DEG C, 530 DEG C, 550 DEG C, 580 DEG C,
600 DEG C, 630 DEG C, 650 DEG C, 680 DEG C, 700 DEG C, 720 DEG C, 750 DEG C, 780 DEG C or 800 DEG C.
Preferably, the time of step (4) described reduction be 2-10h, such as 2h, 2.3h, 2.5h, 2.8h, 3h, 3.3h,
3.5h, 3.8h, 4h, 4.3h, 4.5h, 4.8h, 5h, 6h, 6.5h, 7h, 7.5h, 8h, 8.5h, 9h, 9.5h or 10h.
The oxide of iron is reduced to iron under the reducing gas atmosphere of step of the present invention (4), obtains Fe-TiO2/SiO2-
Al2O3Compound.In the present invention, Fe-TiO2/SiO2-Al2O3Compound indicates there is iron by the load of carrier of sieve and silica-sesquioxide
With the compound of titanium oxide.
Preferably, step (4) hydrocarbon atmosphere is dry distillation gas, organic exhaust gas, low-carbon alkanes or water-gas
In atmosphere any one or at least two combination；
Preferably, the generation temperature of step (4) described carbon fiber be 500-800 DEG C, such as 500 DEG C, 530 DEG C, 550 DEG C,
580 DEG C, 600 DEG C, 630 DEG C, 650 DEG C, 680 DEG C, 700 DEG C, 720 DEG C, 750 DEG C, 780 DEG C or 800 DEG C.
Preferably, the generation of step (4) described carbon fiber carries out in external-heating rotary kiln, particle residence time 0.5-
2.5h, such as 0.5h, 0.8h, 1h, 1.2h, 1.4h, 1.6h, 1.8h, 2h, 2.1h, 2.3h, 2.4h or 2.5h.
Preferably, step (4) grinding uses wet ball-milling.
Preferably, after step (4), it is compound that the mode by flotation or magnetic separation obtains the relatively high charcoal iron of iron content
Object.
On the other hand, the present invention provides the charcoal ferrotitanium sial oxidations that the preparation method as described in first aspect is prepared
Object compound, the compound are represented by Fe-TiO2/SiO2-Al2O3Compound.
On the other hand, the present invention provides the charcoal ferrotitanium sieve and silica-sesquioxide compounds in Nanoscale Iron catalyst preparation
Using.The compound can obtain the relatively high charcoal iron complexes of iron content by way of flotation or magnetic separation, and then can incite somebody to action
It is as nanometer iron catalyst.
On the other hand, the suction the present invention provides the charcoal ferrotitanium sieve and silica-sesquioxide compound in preparation for wastewater treatment
Application in attached dose.The compound can have ammonia nitrogen waste water and phenols wastewater directly as the adsorbent for wastewater treatment
There is good clean-up effect.
On the other hand, the present invention provides the charcoal ferrotitanium sieve and silica-sesquioxide compounds to prepare coal-fired flue-gas heavy metal de-
Except the application in adsorbent.Charcoal ferrotitanium sieve and silica-sesquioxide compound of the present invention can be used as coal-fired flue-gas after vulcanizing treatment
The adsorbent of heavy metal removing, mercury adsorbance reach 10mg/g or more, fully meet actual industrial requirement.
Compared with prior art, the invention has the following beneficial effects:
The present invention can prepare cladding nanometer iron material using red mud by plain mode, and be used for the catalysis of carbon fiber
The higher value application of red mud is realized in agent；Nano iron particles and other are realized in growth using carbon fiber on nano iron particles surface
The physical separation of substance realizes dividing for iron and titanium sial and other impurities in red mud in conjunction with ball mill crushing and Magnetic Separation Technology
From.
Detailed description of the invention
Fig. 1 is the ferrotitanium sieve and silica-sesquioxide compound of present invention preparation deposition carbon fiber and carries out magnetic separation to the compound
Isolated process flow chart；
Fig. 2 is the ferrotitanium sieve and silica-sesquioxide compound of present invention preparation deposition carbon fiber and carries out cigarette using the compound
Qi exhaustion mercury and the process flow chart recycled；
Fig. 3 is the ferrotitanium sieve and silica-sesquioxide compound of present invention preparation deposition carbon fiber and is carried out using the compound useless
Water process and the process flow chart recycled.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.Those skilled in the art should be bright
, the described embodiments are merely helpful in understanding the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
A kind of preparation method for the ferrotitanium sieve and silica-sesquioxide compound depositing carbon fiber, includes the following steps:
(1) after the water of 1kg is added into the red mud of 1kg, it is added into ball milling 12h in ball grinder, so that grain diameter is small
In being equal to 100nm, the first slurry is obtained, the solid content of the first slurry is 30%；
(2) after dilute nitric acid solution (10% concentration) 1kg is gradually added dropwise into the first slurry, solution ph is about 2, system at
For pulpous state；After ammonium hydroxide (10% concentration) 0.5kg is gradually added dropwise in pulpous state red mud in mechanical milling process, solution ph is about 6, and sial is molten
Glue precipitates again, and system viscosity becomes smaller, and obtains the second slurry；
(3) it after the second slurry being separated by solid-liquid separation and washed, is dried under the conditions of 120 DEG C, and then under the conditions of 400 DEG C
Roasting 6h obtains solid matter, i.e. cladded type ferrotitanium sieve and silica-sesquioxide；
(4) cladded type ferrotitanium sieve and silica-sesquioxide is restored into 10h under the conditions of 500 DEG C of atmosphere of hydrogen, then switches to de- CO2
Dry distillation gas (main component: CH4、CO、H2、C2H6、H2S), 2h is reacted at 600 DEG C, obtains the ferrotitanium silicon of deposition carbon fiber
Aluminum oxide compound.
The ferrotitanium sieve and silica-sesquioxide compound for the deposition carbon fiber that the present embodiment can be prepared is added in ball mill,
A small amount of water is added, soot particles are crushed, after flotation or magnetic separation are carried out in water phase, obtain corresponding carbon fiber iron particle
And titanium sial system composite oxide.What the preparation and its magnetic separation for depositing the ferrotitanium sieve and silica-sesquioxide compound of carbon fiber separated
Process flow is as shown in Figure 1, the group that the embodiment passes through the raw material and product 1-3 before process flow as shown in Figure 1 processing
At and its percentage composition it is as shown in table 1.
Table 1
The ferrotitanium sieve and silica-sesquioxide compound progress sulphur deposition for the deposition carbon fiber that the present embodiment is prepared is modified,
The H of 1% concentration is passed through under the conditions of 400 DEG C2S obtains sulphur modification compound after being handled, mercury list is carried out in simulated flue gas
Matter adsorbing and removing, adsorption capacity reach 10mg/g；It can be used for multiple times in the actual process in conjunction with Magnetic Isolation, deposit carbon fiber
The preparation of the ferrotitanium sieve and silica-sesquioxide compound of dimension and its flue gas demercuration and the process flow recycled are as shown in Figure 2.
The ferrotitanium sieve and silica-sesquioxide compound for the deposition carbon fiber that the present embodiment is prepared can be used for phenol wastewater
It is removed, using phenol as benchmark object, saturated extent of adsorption reaches 10mg/g；Under ultraviolet light auxiliary, degradation adsorbance reaches
100mg/g.After adsorption saturation in high temperature inert atmosphere regeneration activating, may be implemented to be recycled, deposit the ferrotitanium of carbon fiber
The preparation of sieve and silica-sesquioxide compound and to carry out wastewater treatment with it as shown in Figure 3 with the process flow that recycles.
Embodiment 2
A kind of preparation method for the ferrotitanium sieve and silica-sesquioxide compound depositing carbon fiber, includes the following steps:
(1) after the water of 2kg is added into the red mud of 1kg, it is added into ball milling 10h in ball grinder, so that grain diameter is small
In being equal to 100nm, the first slurry is obtained, the first slurry solid content is 20%；
(2) after dilute hydrochloric acid solution (5%) 1kg is gradually added dropwise into the first slurry, solution ph is about 4, and system becomes slurry
Shape；After sodium hydroxide (10% concentration) 0.5kg is gradually added dropwise in pulpous state red mud in mechanical milling process, solution ph is about 6, and sial is molten
Glue precipitates again, and system viscosity becomes smaller, and obtains the second slurry；
(3) it after the second slurry being separated by solid-liquid separation and washed, is dried under the conditions of 100 DEG C, and then under the conditions of 600 DEG C
Roasting 5h obtains solid matter, i.e. cladded type ferrotitanium sieve and silica-sesquioxide；
(4) cladded type ferrotitanium sieve and silica-sesquioxide is restored into 10h under the conditions of 700 DEG C of atmosphere of hydrogen, then switched to organic
Exhaust gas (ingredient is acetone, toluene etc.), reacts 1h at 700 DEG C, obtains the ferrotitanium sieve and silica-sesquioxide compound of deposition carbon fiber.
The ferrotitanium sieve and silica-sesquioxide compound for the deposition carbon fiber that the present embodiment can be prepared is added in ball mill,
A small amount of water is added, soot particles are crushed, after flotation or magnetic separation are carried out in water phase, obtain corresponding carbon fiber iron particle
And titanium sial system composite oxide.What the preparation and its magnetic separation for depositing the ferrotitanium sieve and silica-sesquioxide compound of carbon fiber separated
Process flow is as shown in Figure 1, the group that the embodiment passes through the raw material and product 1-3 before process flow as shown in Figure 1 processing
At and its percentage composition it is as shown in table 2.
Table 2
The ferrotitanium sieve and silica-sesquioxide compound progress sulphur deposition for the deposition carbon fiber that the present embodiment is prepared is modified,
The H of 1% concentration is passed through under the conditions of 400 DEG C2S obtains sulphur modification compound after being handled, mercury list is carried out in simulated flue gas
Matter adsorbing and removing, adsorption capacity reach 13mg/g；It can be used for multiple times in the actual process in conjunction with Magnetic Isolation, deposit carbon fiber
The preparation of the ferrotitanium sieve and silica-sesquioxide compound of dimension and its flue gas demercuration and the process flow recycled are as shown in Figure 2.
The ferrotitanium sieve and silica-sesquioxide compound for the deposition carbon fiber that the present embodiment is prepared can be used for phenol wastewater
It is removed, using phenol as benchmark object, saturated extent of adsorption reaches 15mg/g；Under ultraviolet light auxiliary, degradation adsorbance reaches
110mg/g.After adsorption saturation in high temperature inert atmosphere regeneration activating, may be implemented to be recycled, deposit the ferrotitanium of carbon fiber
The preparation of sieve and silica-sesquioxide compound and to carry out wastewater treatment with it as shown in Figure 3 with the process flow that recycles.
Embodiment 3
A kind of preparation method for the ferrotitanium sieve and silica-sesquioxide compound depositing carbon fiber, includes the following steps:
(1) after the water of 1kg is added into the red mud of 1kg, ball milling is added into ball grinder for 24 hours, so that grain diameter is small
In being equal to 100nm, the first slurry is obtained, the first slurry solid content is 50%；
(2) after sulfuric acid solution (50%) 0.2kg is gradually added dropwise into the first slurry, solution ph is about 3, and system becomes slurry
Shape；After aqueous sodium carbonate (5% concentration) 1kg is gradually added dropwise in pulpous state red mud in mechanical milling process, solution ph is about 7, sial
Colloidal sol precipitates again, and system viscosity becomes smaller, and obtains the second slurry；
(3) it after the second slurry being separated by solid-liquid separation and washed, is dried under the conditions of 100 DEG C, and then under the conditions of 800 DEG C
Roasting 3h obtains solid matter, i.e. cladded type ferrotitanium sieve and silica-sesquioxide；
(4) by cladded type ferrotitanium sieve and silica-sesquioxide under the conditions of 700 DEG C of atmosphere of hydrogen reductase 12 h, then switch to coal gasification
Gaseous mixture (CO, H2), 2.5h is reacted at 700 DEG C, obtains the ferrotitanium sieve and silica-sesquioxide compound of deposition carbon fiber.
The ferrotitanium sieve and silica-sesquioxide compound for the deposition carbon fiber that the present embodiment can be prepared is added in ball mill,
A small amount of water is added, soot particles are crushed, after flotation or magnetic separation are carried out in water phase, obtain corresponding carbon fiber iron particle
And titanium sial system composite oxide.What the preparation and its magnetic separation for depositing the ferrotitanium sieve and silica-sesquioxide compound of carbon fiber separated
Process flow is as shown in Figure 1, the group that the embodiment passes through the raw material and product 1-3 before process flow as shown in Figure 1 processing
At and its percentage composition it is as shown in table 3.
Table 3
The ferrotitanium sieve and silica-sesquioxide compound progress sulphur deposition for the deposition carbon fiber that the present embodiment is prepared is modified,
The H of 1% concentration is passed through under the conditions of 400 DEG C2S obtains sulphur modification compound after being handled, mercury list is carried out in simulated flue gas
Matter adsorbing and removing, adsorption capacity reach 15mg/g；It can be used for multiple times in the actual process in conjunction with Magnetic Isolation, deposit carbon fiber
The preparation of the ferrotitanium sieve and silica-sesquioxide compound of dimension and its flue gas demercuration and the process flow recycled are as shown in Figure 2.
The ferrotitanium sieve and silica-sesquioxide compound for the deposition carbon fiber that the present embodiment is prepared can be used for phenol wastewater
It is removed, using phenol as benchmark object, saturated extent of adsorption reaches 12mg/g；Under ultraviolet light auxiliary, degradation adsorbance reaches
108mg/g.After adsorption saturation in high temperature inert atmosphere regeneration activating, may be implemented to be recycled, deposit the ferrotitanium of carbon fiber
The preparation of sieve and silica-sesquioxide compound and to carry out wastewater treatment with it as shown in Figure 3 with the process flow that recycles.
Embodiment 4
A kind of preparation method for the ferrotitanium sieve and silica-sesquioxide compound depositing carbon fiber, includes the following steps:
(1) after the water of 5kg is added into the red mud of 1kg, it is added into ball milling 36h in ball grinder, so that grain diameter is small
In being equal to 100nm, the first slurry is obtained, the first slurry solid content is 40%；
(2) after sulfuric acid solution (50%) 0.5kg is gradually added dropwise into the first slurry, solution ph is about 4, and system becomes slurry
Shape；After aqueous sodium carbonate (5% concentration) 1.5kg is gradually added dropwise in pulpous state red mud in mechanical milling process, solution ph is about 10, silicon
Aluminum sol precipitates again, and system viscosity becomes smaller, and obtains the second slurry；
(3) it after the second slurry being separated by solid-liquid separation and washed, is dried under the conditions of 100 DEG C, and then under the conditions of 800 DEG C
Roasting 10h obtains solid matter, i.e. cladded type ferrotitanium sieve and silica-sesquioxide；
(4) cladded type ferrotitanium sieve and silica-sesquioxide is restored into 5h under the conditions of 700 DEG C of atmosphere of hydrogen, then switches to coal gasification
Gaseous mixture (CO, H2), 0.5h is reacted at 700 DEG C, obtains the ferrotitanium sieve and silica-sesquioxide compound of deposition carbon fiber.
The ferrotitanium sieve and silica-sesquioxide compound for the deposition carbon fiber that the present embodiment can be prepared is added in ball mill,
A small amount of water is added, soot particles are crushed, after flotation or magnetic separation are carried out in water phase, obtain corresponding carbon fiber iron particle
And titanium sial system composite oxide.What the preparation and its magnetic separation for depositing the ferrotitanium sieve and silica-sesquioxide compound of carbon fiber separated
Process flow is as shown in Figure 1, the group that the embodiment passes through the raw material and product 1-3 before process flow as shown in Figure 1 processing
At and its percentage composition it is as shown in table 4.
Table 4
The ferrotitanium sieve and silica-sesquioxide compound progress sulphur deposition for the deposition carbon fiber that the present embodiment is prepared is modified,
The H of 1% concentration is passed through under the conditions of 400 DEG C2S obtains sulphur modification compound after being handled, mercury list is carried out in simulated flue gas
Matter adsorbing and removing, adsorption capacity reach 10mg/g；It can be used for multiple times in the actual process in conjunction with Magnetic Isolation, deposit carbon fiber
The preparation of the ferrotitanium sieve and silica-sesquioxide compound of dimension and its flue gas demercuration and the process flow recycled are as shown in Figure 2.
The ferrotitanium sieve and silica-sesquioxide compound for the deposition carbon fiber that the present embodiment is prepared can be used for phenol wastewater
It is removed, using phenol as benchmark object, saturated extent of adsorption reaches 13mg/g；Under ultraviolet light auxiliary, degradation adsorbance reaches
105mg/g.After adsorption saturation in high temperature inert atmosphere regeneration activating, may be implemented to be recycled, deposit the ferrotitanium of carbon fiber
The preparation of sieve and silica-sesquioxide compound and to carry out wastewater treatment with it as shown in Figure 3 with the process flow that recycles.
The Applicant declares that the present invention illustrates the process method of the present invention through the above embodiments, but the present invention not office
It is limited to above-mentioned processing step, that is, does not mean that the present invention must rely on the above process steps to be carried out.Technical field
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to raw material selected by the present invention
Addition, selection of concrete mode etc., all of which fall within the scope of protection and disclosure of the present invention.
Claims (26)
1. a kind of preparation method of charcoal ferrotitanium sieve and silica-sesquioxide compound, which is characterized in that the described method comprises the following steps:
(1) water is added into red mud, it is ground to obtain the first slurry；
(2) acid for adjusting pH value is added in the first slurry obtained to step (1) to 2-4, surface dispersant is added, grinds lower be added
Alkaline matter adjusts pH value to 5-10, obtains the second slurry；
(3) the second slurry obtained by step (2) is separated by solid-liquid separation, solid roasting is obtained into cladded type ferrotitanium sieve and silica-sesquioxide；
The temperature of the roasting is 400-800 DEG C；
(4) cladded type ferrotitanium sieve and silica-sesquioxide is restored under reducing gas atmosphere, then under hydrocarbon atmosphere
The generation for carrying out carbon fiber, obtains the charcoal ferrotitanium sieve and silica-sesquioxide compound.
2. preparation method according to claim 1, which is characterized in that step (1) red mud is Bayer process red mud, Asia is molten
In salt red mud or red mud from sintering process any one or at least two mixture.
3. preparation method according to claim 1, which is characterized in that the quality of step (1) red mud and the water of addition
Than for 1:(1-5).
4. preparation method according to claim 1, which is characterized in that step (1) grinding is so that grain diameter is less than
Equal to 100nm.
5. preparation method according to claim 1, which is characterized in that described to be ground to ball milling.
6. preparation method according to claim 1, which is characterized in that the time of the grinding is 10-36h.
7. preparation method according to claim 1, which is characterized in that the solid content of step (1) first slurry is 10-
50%.
8. preparation method according to claim 1 or 2, which is characterized in that step (2) acid is inorganic acid or organic
Acid.
9. preparation method according to claim 1, which is characterized in that step (2) acid is industrial waste acid.
10. preparation method according to claim 1, which is characterized in that step (2) surface dispersant is polyethylene glycol
Class compound and/or fatty alcohol polyethenoxy ether class compound.
11. preparation method according to claim 1, which is characterized in that step (2) surface dispersant is polyethylene glycol
1000。
12. preparation method according to claim 1, which is characterized in that the additive amount of step (2) described surface dispersant is
The 0.1-1% of first slurry gross mass.
13. preparation method according to claim 1, which is characterized in that step (2) alkaline matter is alkali metal hydrogen-oxygen
In compound or carbonate any one or at least two combination.
14. preparation method according to claim 1, which is characterized in that step (2) alkaline matter is sodium hydroxide
And/or sodium carbonate.
15. preparation method according to claim 1, which is characterized in that the time of step (3) described roasting is 1-20h.
16. preparation method according to claim 1, which is characterized in that the water phase that step (3) obtains after being separated by solid-liquid separation carries out
Desalting processing and it is up to standard after discharged.
17. preparation method according to claim 1, which is characterized in that step (4) reducing gas atmosphere is hydrogen gas
Atmosphere.
18. preparation method according to claim 1, which is characterized in that step (4) it is described reduction at 500-800 DEG C into
Row.
19. preparation method according to claim 1, which is characterized in that the time of step (4) described reduction is 2-10h.
20. preparation method according to claim 1, which is characterized in that step (4) hydrocarbon atmosphere is destructive distillation
In coal gas, organic exhaust gas, low-carbon alkanes or water gas atmosphere any one or at least two combination.
21. preparation method according to claim 1, which is characterized in that the generation temperature of step (4) described carbon fiber is
500-800℃。
22. preparation method according to claim 1, which is characterized in that the generation of step (4) described carbon fiber is in external-heat
It is carried out in rotary kiln, particle residence time 0.5-2.5h.
23. the charcoal ferrotitanium sieve and silica-sesquioxide that preparation method described in any one of -22 is prepared according to claim 1 is compound
Object.
24. application of the charcoal ferrotitanium sieve and silica-sesquioxide compound according to claim 23 in Nanoscale Iron catalyst preparation,
It is characterized in that, to obtain iron content by way of flotation or magnetic separation relatively high for the charcoal ferrotitanium sieve and silica-sesquioxide compound
Charcoal iron complexes, and then as nanometer iron catalyst.
25. charcoal ferrotitanium sieve and silica-sesquioxide compound according to claim 23 is in the adsorbent that preparation is used for wastewater treatment
Application.
26. charcoal ferrotitanium sieve and silica-sesquioxide compound according to claim 23 is preparing the absorption of coal-fired flue-gas heavy metal removing
Application in agent.
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