CN105621490A - Method for separating iron oxide in coal ash of circulating fluidized bed - Google Patents
Method for separating iron oxide in coal ash of circulating fluidized bed Download PDFInfo
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- CN105621490A CN105621490A CN201610064575.9A CN201610064575A CN105621490A CN 105621490 A CN105621490 A CN 105621490A CN 201610064575 A CN201610064575 A CN 201610064575A CN 105621490 A CN105621490 A CN 105621490A
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- coal ash
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- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000010883 coal ash Substances 0.000 title claims abstract description 20
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title abstract description 28
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 87
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 70
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 17
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 8
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 8
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000010881 fly ash Substances 0.000 claims description 55
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 44
- 239000007788 liquid Substances 0.000 claims description 38
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 34
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 29
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 24
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 24
- 239000012065 filter cake Substances 0.000 claims description 24
- 239000000706 filtrate Substances 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 229960004756 ethanol Drugs 0.000 claims description 22
- 238000007885 magnetic separation Methods 0.000 claims description 19
- 238000000926 separation method Methods 0.000 claims description 15
- 229910021529 ammonia Inorganic materials 0.000 claims description 12
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 12
- LDHBWEYLDHLIBQ-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide;hydrate Chemical compound O.[OH-].[O-2].[Fe+3] LDHBWEYLDHLIBQ-UHFFFAOYSA-M 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000011324 bead Substances 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 9
- 239000002956 ash Substances 0.000 claims description 5
- 229910052681 coesite Inorganic materials 0.000 claims description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 229910052682 stishovite Inorganic materials 0.000 claims description 5
- 229910052905 tridymite Inorganic materials 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 3
- VWWHFOBVDHPEKJ-UHFFFAOYSA-N aluminum ethanol trinitrate Chemical compound C(C)O.[N+](=O)([O-])[O-].[Al+3].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] VWWHFOBVDHPEKJ-UHFFFAOYSA-N 0.000 claims description 2
- 230000006698 induction Effects 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 2
- 235000019441 ethanol Nutrition 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 11
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 8
- 238000000605 extraction Methods 0.000 description 6
- 239000000292 calcium oxide Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000005243 fluidization Methods 0.000 description 4
- 239000003245 coal Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 3
- 238000010248 power generation Methods 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 239000000469 ethanolic extract Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002481 ethanol extraction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- NOTVAPJNGZMVSD-UHFFFAOYSA-N potassium monoxide Inorganic materials [K]O[K] NOTVAPJNGZMVSD-UHFFFAOYSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- HUAUNKAZQWMVFY-UHFFFAOYSA-M sodium;oxocalcium;hydroxide Chemical compound [OH-].[Na+].[Ca]=O HUAUNKAZQWMVFY-UHFFFAOYSA-M 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/66—Nitrates, with or without other cations besides aluminium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Processing Of Solid Wastes (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention provides a method for separating iron oxide in coal ash of a circulating fluidized bed. The method includes dissolving out all Fe2O3 and FeO and partial non-crystalline Al2O3 in the coal ash by the aid of low-temperature hydrothermal reaction between nitric acid and the coal ash; separating and extracting the Fe2O3 and FeO in solution by the aid of ethyl alcohol to obtain the high-purity iron oxide. The method is free of special requirements on equipment, the low-temperature hydrothermal reaction can be carried out by the aid of the method, the iron oxide in the coal ash can be efficiently separated and extracted by the aid of the method, aluminum oxide in the coal ash can be dissolved out by 90%-96% by the aid of the method, and the iron oxide in the coal ash can be dissolved out by 98%-100% by the aid of the method. According to the technical scheme, the method has the advantages that coal ash resources can be sufficiently utilized, manufacturing processes are simple, and the method is low in production cost and suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of Ash Utilization Application way, separate the method for ferrum oxide in circulating fluid bed coal ash in particular to a kind of.
Background technology
Coal fired power generation is one of commonly used power generation mode in countries in the world, and effective utilization of the coal-fired a large amount of flyash produced has become world subject. At present, China's electric power more than 70% is produced by coal fired power generation, and the yield about 30% of whole nation coal is used for generating electricity, consequent flyash is if, with amount deficiency, not only occupy a large amount of soil, cause serious environmental pollution, be also the waste of a kind of resource.
The feature that fluidization bed fly ash sinters due to its cold cycle, Circulating Fluidized Bed Ash cannot form glassy phase and cause that activity is relatively low, in addition fluidized bed ash is in sintering process, it is added with excessive Calx, gel time and intensity to itself produce large effect, make fluidization bed fly ash activity relatively low, cannot be frozen into after aquation and there is some strength, it is impossible to be used for paving the way as conventional boiler ash, build, the field such as well cementation. So fluidization bed fly ash can only use the mode buried to process, bury the seed of trouble of environmentally undesirable impact. Therefore how effectively to process the problem that circulating fluid bed coal ash becomes extremely urgent.
From another angle, rich in many oxide in flyash, such as Al2O3, SiO2, Fe2O3, FeO, CaO, MgO, SO3, Na2O, K2O etc., additionally contain a small amount of rare earth element. These oxides separation and Extraction from flyash out and is prepared corresponding high value-added product, higher social economy's value can not only be produced, it is possible to alleviate the flyash harm to environment.
The comprehensive utilizating research of flyash, the particularly research of separation and Extraction aluminium oxide from flyash, from the forties in last century so far, many experts both domestic and external, scholar study at this and have carried out extensive work and proposed multiple separating and extracting process. But when extracting separation aluminium oxide, ferrum oxide is fallen as impurity treatment, not by Fe in flyash2O3With FeO recycling, cause the serious waste of resource.
And ferrum oxide is as a kind of inorganic pigment, it is widely used in the fields such as paint, rubber, plastic cosmetic, building ground material, accurate five metals instrument, optical glass, enamel, school supply and stationery, leather, magnetic alloy and high-grade alloy steel.
At present, Chinese scholars proposes certain methods for separation and Extraction ferrum oxide from flyash, such as: calcium oxide sintering process, soda lime sintering process etc., but these methods due to process conditions limit, the reason such as the ferrum oxide response rate is low, power consumption is big, production cost is high, bed drain purge is big, cause separation and Extraction ferrum oxide implementation result poor.
It is an object of the invention to utilize dust technology to react with ordinary cycle fluidization bed fly ash low-temperature hydrothermal, make Fe whole in flyash2O3, FeO and part amorphous state Al2O3Dissolution, recycling separation of ethanol extracts the Fe in solution2O3, FeO, finally give the iron oxide product that purity is higher.
Summary of the invention
It is an object of the invention to provide and a kind of utilize the method for ferrum oxide in nitric acid and ethanol extraction flyash under cryogenic.
Technical scheme provided by the invention includes utilizing nitric acid to react with flyash low-temperature hydrothermal, makes Fe whole in flyash2O3, FeO and part amorphous state Al2O3Dissolution, recycling separation of ethanol extracts the Fe in solution2O3, FeO obtain highly purified ferrum oxide. Technical scheme processing technology provided by the invention is simple, reduce production cost, take full advantage of the resource of flyash, is suitable for large-scale production.
Realize the object of the invention technical scheme as follows:
A kind of separate the method for ferrum oxide in circulating fluid bed coal ash, it is characterised in that described preparation method comprises the steps:
1) magnetic bead in magnetic separation separation of fine coal ash;
2) acidleach: at 50 DEG C��80 DEG C, mixes flyash with the nitric acid that concentration is 1%��5% with the ratio that solid-to-liquid ratio is 1:3��1:6 of nitric acid in flyash, reacts 1��4h;
3) solid-liquid separation: after reactant is cooled to room temperature, sucking filtration, the filter cake water washing that solid-to-liquid ratio is 2:1��1:2 by flyash Yu water, obtain the solution of ferric nitrate and aluminum nitrate;
4) separation of ethanol aluminum nitrate and ferrum oxide: ethanol and step 3) in the described solution that obtains mix by 2:1��5:1 volume ratio, again by the mol ratio of aluminium oxide Yu ammonium nitrate be 1:3��1:4 add formulating ammonium nitrate mixed liquor, after stirring 1��2h, sucking filtration, obtain aluminum nitrate filter cake; Then by the absolute ethanol washing that solid-to-liquid ratio is 2:1��1:2 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed;
5) ferrum oxide reclaims: dropping ammonia, in described recovery filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Further, described flyash is following component by mass percentage:
Al2O3+SiO2+Fe2O3> 50%, CaO > 10%.
Further, described flyash is Peng Lai ash, following component by mass percentage: Al2O3, 19.25%; SiO2, 49.08%; Fe2O3, 3.6%; CaO, 16.34%; SO3, 4.27%; Loss on ignition, 5.68%.
Further, described step 1) in, carry out wet magnetic separation separation with wet type low-intensity (magnetic) separator.
Further, described wet type low-intensity (magnetic) separator magnetic induction 0.2T, pan feeding speed 500mL/min, material concentration 8%, magnetic separation 3��5 times.
Further, described step 1) purpose of magnetic separation is to isolate magnetic bead, that isolates magnetic bead in flyash is mainly composed of Fe3O4. Because of Fe3O4Stable chemical nature, not easily react with strong acid and strong base, therefore for make the ferrum oxide in flyash be totally separated extraction, it is necessary to add magnetic separation step.
With immediate prior art ratio, technical scheme provided by the invention has following excellent effect:
1, technical scheme provided by the invention, the ferrum oxide in energy fully high efficiency extraction flyash.
2, technical scheme provided by the invention, utilizes the method treated coal ash of low-temp reaction, to equipment without particular/special requirement.
3, technical scheme provided by the invention, can by the alumina leaching 90%��96% in flyash, ferrum oxide dissolution 98%��100%.
4, technical scheme provided by the invention, flyash is after magnetic separation, and the response rate of magnetic bead reaches more than 85%, and magnetic bead particle diameter is at 20��30um; From flyash, reclaim magnetic bead less costly, except nonmagnetic portion iron content is relatively low in the flyash after magnetic bead, be more beneficial for integrated application; With magnetic bead in conjunction with HGMS technology process waste water, can by effective for the tp removal rate in waste water, efficiency is high, treating capacity is big.
5, technical scheme provided by the invention, has widened the scope of total utilization of PCA.
Detailed description of the invention
Further technical scheme is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments. Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain, broadly fall into the scope of protection of the invention.
Embodiment 1, flyash through 3 magnetic separation, then with 5% nitric acid mix by solid-to-liquid ratio 1:3, and at 80 DEG C, react 4h; Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 2:1 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature; It is that 2:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:3 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 2h, sucking filtration, obtain aluminum nitrate filter cake; Then by the absolute ethanol washing that solid-to-liquid ratio is 2:1 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed; Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 2, flyash through 4 magnetic separation, then with 4% nitric acid mix by solid-to-liquid ratio 1:4, and at 70 DEG C, react 3h; Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 1:2 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature; It is that 3:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:4 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 1h, sucking filtration, obtain aluminum nitrate filter cake; Then by the absolute ethanol washing that solid-to-liquid ratio is 1:2 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed; Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 3, flyash through 5 magnetic separation, then with 3% nitric acid mix by solid-to-liquid ratio 1:5, and at 60 DEG C, react 3h; Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 2:1 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature; It is that 4:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:3 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 1.5h, sucking filtration, obtain aluminum nitrate filter cake; Then by the absolute ethanol washing that solid-to-liquid ratio is 2:3 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed; Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 4, flyash through 5 magnetic separation, then with 5% nitric acid mix by solid-to-liquid ratio 1:5, and at 50 DEG C, react 3h; Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 2:3 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature; It is that 5:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:3 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 2h, sucking filtration, obtain aluminum nitrate filter cake; Then by the absolute ethanol washing that solid-to-liquid ratio is 2:1 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed; Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 5, flyash through 5 magnetic separation, then with 2% nitric acid mix by solid-to-liquid ratio 1:6, and at 65 DEG C, react 4h; Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 4:3 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature; It is that 5:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:4 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 2h, sucking filtration, obtain aluminum nitrate filter cake; Then by the absolute ethanol washing that solid-to-liquid ratio is 2:1 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed; Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 6, flyash through 4 magnetic separation, then with 3% nitric acid mix by solid-to-liquid ratio 1:3, and at 75 DEG C, react 4h; Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 5:4 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature; It is that 3:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:4 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 1h, sucking filtration, obtain aluminum nitrate filter cake; Then by the absolute ethanol washing that solid-to-liquid ratio is 2:1 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed; Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 7, flyash through 5 magnetic separation, then with 5% nitric acid mix by solid-to-liquid ratio 1:4, and at 70 DEG C, react 2h; Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 2:1 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature; It is that 3:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:3 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 1h, sucking filtration, obtain aluminum nitrate filter cake; Then by the absolute ethanol washing that solid-to-liquid ratio is 1:2 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed; Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 8, flyash through 4 magnetic separation, then with 5% nitric acid mix by solid-to-liquid ratio 1:6, and at 55 DEG C, react 3h; Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 2:1 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature; It is that 4:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:4 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 2h, sucking filtration, obtain aluminum nitrate filter cake; Then by the absolute ethanol washing that solid-to-liquid ratio is 5:4 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed; Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 9, flyash through 3 magnetic separation, then with 1% nitric acid mix by solid-to-liquid ratio 1:3, and at 50 DEG C, react 4h; Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 4:1 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature; It is that 7:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:3 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 2h, sucking filtration, obtain aluminum nitrate filter cake; Then by the absolute ethanol washing that solid-to-liquid ratio is 2:1 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed; Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 10, flyash through 5 magnetic separation, then with 4% nitric acid mix by solid-to-liquid ratio 1:4, and at 80 DEG C, react 3h; Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 1:2 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature; It is that 2:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:3 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 1h, sucking filtration, obtain aluminum nitrate filter cake; Then by the absolute ethanol washing that solid-to-liquid ratio is 1:2 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed; Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Gained sample in above-described embodiment is carried out performance test respectively, obtains data as shown in table 1 below.
Table 1
Above example is only in order to illustrate that technical scheme is not intended to limit; those of ordinary skill in the field are to be understood that; the specific embodiment of the present invention can being modified with reference to above-described embodiment or equivalent replacement, these are all being applied within the claims awaited the reply without departing from any amendment or equivalent replacement of spirit and scope of the invention.
Claims (5)
1. one kind separates the method for ferrum oxide in circulating fluid bed coal ash, it is characterised in that described preparation method comprises the steps:
1) magnetic bead in magnetic separation separation of fine coal ash;
2) acidleach: at 50 DEG C��80 DEG C, mixes flyash with the nitric acid that concentration is 1%��5% with the ratio that solid-to-liquid ratio is 1:3��1:6 of nitric acid in flyash, reacts 1��4h;
3) solid-liquid separation: after reactant is cooled to room temperature, sucking filtration, the filter cake water washing that solid-to-liquid ratio is 2:1��1:2 by flyash Yu water, obtain the solution of ferric nitrate and aluminum nitrate;
4) separation of ethanol aluminum nitrate and ferrum oxide: ethanol and step 3) in the described solution that obtains mix by 2:1��5:1 volume ratio, again by the mol ratio of aluminium oxide Yu ammonium nitrate be 1:3��1:4 add formulating ammonium nitrate mixed liquor, after stirring 1��2h, sucking filtration, obtain aluminum nitrate filter cake; Then by the absolute ethanol washing that solid-to-liquid ratio is 2:1��1:2 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed;
5) ferrum oxide reclaims: dropping ammonia, in described recovery filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
2. as claimed in claim 1 a kind of separate the method for ferrum oxide in circulating fluid bed coal ash, it is characterised in that described flyash is following component by mass percentage:
Al2O3+SiO2+Fe2O3> 50%, CaO > 10%.
3. as claimed in claim 2 a kind of separate the method for ferrum oxide in circulating fluid bed coal ash, it is characterised in that described flyash is Peng Lai ash, following component by mass percentage: Al2O3, 19.25%; SiO2, 49.08%; Fe2O3, 3.6%; CaO, 16.34%; SO3, 4.27%; Loss on ignition, 5.68%.
4. as claimed in claim 1 a kind of separate the method for ferrum oxide in circulating fluid bed coal ash, it is characterised in that described step 1) in, carry out wet magnetic separation separation with wet type low-intensity (magnetic) separator.
5. as claimed in claim 4 a kind of separate the method for ferrum oxide in circulating fluid bed coal ash, it is characterised in that described wet type low-intensity (magnetic) separator magnetic induction 0.2T, pan feeding speed 500mL/min, material concentration 8%, magnetic separation 3��5 times.
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| JPS6241721A (en) * | 1985-08-19 | 1987-02-23 | Nisshin Steel Co Ltd | Method of recovering iron oxide |
| CN101870489A (en) * | 2010-04-27 | 2010-10-27 | 中国神华能源股份有限公司 | Method for producing superfine aluminium hydroxide and aluminium oxide by using flyash |
| CN102101689A (en) * | 2010-12-23 | 2011-06-22 | 内蒙古昶泰资源循环再生利用科技开发有限责任公司 | Technological method for producing high-purity low-iron aluminum sulfate by using coal ash and comprehensively utilizing coal ash |
| CN104445212A (en) * | 2013-09-16 | 2015-03-25 | 贵阳铝镁设计研究院有限公司 | Method for processing fly ash used for circulating fluidized bed |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6241721A (en) * | 1985-08-19 | 1987-02-23 | Nisshin Steel Co Ltd | Method of recovering iron oxide |
| CN101870489A (en) * | 2010-04-27 | 2010-10-27 | 中国神华能源股份有限公司 | Method for producing superfine aluminium hydroxide and aluminium oxide by using flyash |
| CN102101689A (en) * | 2010-12-23 | 2011-06-22 | 内蒙古昶泰资源循环再生利用科技开发有限责任公司 | Technological method for producing high-purity low-iron aluminum sulfate by using coal ash and comprehensively utilizing coal ash |
| CN104445212A (en) * | 2013-09-16 | 2015-03-25 | 贵阳铝镁设计研究院有限公司 | Method for processing fly ash used for circulating fluidized bed |
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