CN105776342A - Method for separating Fe2O3 in pulverized coal ash of circulating fluidized bed - Google Patents
Method for separating Fe2O3 in pulverized coal ash of circulating fluidized bed Download PDFInfo
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- CN105776342A CN105776342A CN201610064554.7A CN201610064554A CN105776342A CN 105776342 A CN105776342 A CN 105776342A CN 201610064554 A CN201610064554 A CN 201610064554A CN 105776342 A CN105776342 A CN 105776342A
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- aluminum phosphate
- coal ash
- filter cake
- solution
- flyash
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- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000010883 coal ash Substances 0.000 title claims abstract description 22
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title claims abstract description 13
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 154
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 18
- 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 16
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 9
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 9
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims description 72
- 239000012065 filter cake Substances 0.000 claims description 57
- 235000011187 glycerol Nutrition 0.000 claims description 57
- 239000010881 fly ash Substances 0.000 claims description 55
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 53
- 239000000706 filtrate Substances 0.000 claims description 48
- 238000001914 filtration Methods 0.000 claims description 38
- 239000007788 liquid Substances 0.000 claims description 34
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 30
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 26
- 229910000398 iron phosphate Inorganic materials 0.000 claims description 24
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 20
- 238000007885 magnetic separation Methods 0.000 claims description 19
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 18
- 229910021529 ammonia Inorganic materials 0.000 claims description 14
- LDHBWEYLDHLIBQ-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide;hydrate Chemical compound O.[OH-].[O-2].[Fe+3] LDHBWEYLDHLIBQ-UHFFFAOYSA-M 0.000 claims description 14
- 239000012530 fluid Substances 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000011324 bead Substances 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 9
- 230000003252 repetitive effect Effects 0.000 claims description 8
- 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
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 230000006698 induction Effects 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 16
- 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 1
- 239000000203 mixture Substances 0.000 description 16
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 8
- 239000000292 calcium oxide Substances 0.000 description 4
- 230000000694 effects Effects 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
- 238000005516 engineering process 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
- 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
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution 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
- C01G49/06—Ferric oxide [Fe2O3]
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
Abstract
The method provides a method for separating Fe2O3 in pulverized coal ash of a circulating fluidized bed.The method includes the steps that phosphoric acid and pulverized coal ash are subjected to a low-temperature hydrothermal reaction so that all Fe2O3 and FeO and part of amorphous Al2O3 in pulverized coal ash can be dissolved out; then, Fe2O3 and FeO in the solution are separated and extracted with glycerol to obtain high-purity Fe2O3.According to the method, no special requirement for equipment exists, only the low-temperature reaction is needed, and Fe2O3 in pulverized coal ash can be efficiently separated and extracted; Al2O3 in pulverized coal ash can be dissolved out by 90%-96%, and Fe2O3 in pulverized coal ash can be dissolved out by 98%-100%.By means of the technical scheme, the resource of pulverized coal ash is fully utilized, the manufacturing process is simple, the production cost is low, and the method is 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, and consequent flyash, if, with amount deficiency, not only occupies a large amount of soil, causes 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 phosphoric acid,diluted to react with ordinary cycle fluidization bed fly ash low-temperature hydrothermal, make Fe whole in flyash2O3, FeO and part amorphous state Al2O3Dissolution, recycling glycerol separate draw solution in Fe2O3, 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 phosphoric acid and glycerin extraction flyash under cryogenic.
Technical scheme provided by the invention includes utilizing phosphoric acid to react with flyash low-temperature hydrothermal, makes Fe whole in flyash2O3, FeO and part amorphous state Al2O3Dissolution, the Fe in recycling glycerol separate draw 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 separating the method for ferrum oxide in circulating fluid bed coal ash, described preparation method comprises the steps:
1) magnetic bead in magnetic separation separation of fine coal ash；
2) acidleach: at 100 DEG C～120 DEG C, mixes flyash with the phosphoric acid that concentration is 3%～10% with the ratio that solid-to-liquid ratio is 1:1～1:5 of phosphoric acid in flyash, reacts 3～8h；
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 iron phosphate and aluminum phosphate；
4) glycerin extraction aluminum phosphate: by glycerol and step 3) in the volume ratio of the iron phosphate that obtains and aluminum phosphate solution be that 1:1～2:1 prepares glycerol adding, after stirring 3～5min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；
5) process aluminum sulfate filter cake: adding concentration by solid-to-liquid ratio 1:2～1:5 preparation of aluminum phosphate filter cake with glycerine water solution is the glycerine water solution of 55%～70%, after stirring 10～30min, sucking filtration, then obtain aluminum phosphate filter cake, and reclaim filtrate；This glycerine water solution washing procedure of repetitive operation 4～6 times, separates iron phosphate to greatest extent, the aluminum phosphate filter cake that final iron-holder is extremely low, and reclaims filtrate；
6) ferrum oxide reclaims: add hydrogen peroxide with above-mentioned whole recovery filtrate volumes than for 1:1000～2:1000 preparation by hydrogen peroxide, and after standing 3～5min, dropping ammonia, to pH value of solution > 8, filters, obtains highly purified 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；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.
Further, the other method of described process aluminum sulfate filter cake includes: add water with water solid-to-liquid ratio 3:1～1:1 preparation by aluminum phosphate filter cake, aluminum phosphate is made to dissolve, again by the volume ratio of glycerol Yu solution be 3:1～12:1 prepare glycerol adding, after stirring 3～5min, sucking filtration, obtains aluminum phosphate filter cake, and reclaims filtrate.
Further, described ferrum oxide reclaims other method and includes: in reclaiming dropping ammonia in filtrate, to pH value of solution > 10, filters, obtains highly purified hydrated ferric oxide..
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 4 magnetic separation, then with 5% phosphoric acid mix by solid-to-liquid ratio 1:2, and at 110 DEG C, react 5h；Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 1:1 of flyash Yu water, obtains the solution of iron phosphate and aluminum phosphate after being cooled to room temperature；It is that 1:1 prepares glycerol adding by the volume ratio of glycerol with iron phosphate and aluminum phosphate solution, after stirring 5min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；Mix with the ratio of 1:3 with the glycerine water solution that concentration is 70% in aluminum phosphate filter cake, after stirring 15min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；This glycerine water solution washing procedure of repetitive operation 6 times, and reclaim filtrate；Hydrogen peroxide mixes by the volume ratio of 1:1000 with reclaiming filtrate, and after standing 5min, dropping ammonia, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 2, flyash through 3 magnetic separation, then with 8% phosphoric acid mix by solid-to-liquid ratio 1:3, and at 120 DEG C, react 6h；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 iron phosphate and aluminum phosphate after being cooled to room temperature；It is that 1:1 prepares glycerol adding by the volume ratio of glycerol with iron phosphate and aluminum phosphate solution, after stirring 3min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；Mix with the ratio of 1:5 with the glycerine water solution that concentration is 60% in aluminum phosphate filter cake, after stirring 30min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；This glycerine water solution washing procedure of repetitive operation 4 times, and reclaim filtrate；Hydrogen peroxide mixes by the volume ratio of 1:1000 with reclaiming filtrate, and after standing 3min, dropping ammonia, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 3, flyash through 3 magnetic separation, then with 3% phosphoric acid mix by solid-to-liquid ratio 1:2, and at 100 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 iron phosphate and aluminum phosphate after being cooled to room temperature；It is that 2:1 prepares glycerol adding by the volume ratio of glycerol with iron phosphate and aluminum phosphate solution, after stirring 5min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；Mix with the ratio of 1:2 with the glycerine water solution that concentration is 60% in aluminum phosphate filter cake, after stirring 10min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；This glycerine water solution washing procedure of repetitive operation 6 times, and reclaim filtrate；Hydrogen peroxide mixes by the volume ratio of 2:1000 with reclaiming filtrate, and after standing 3min, dropping ammonia, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 4, flyash through 5 magnetic separation, then with 9% phosphoric acid mix by solid-to-liquid ratio 1:4, and at 100 DEG C, react 5h；Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 4:5 of flyash Yu water, obtains the solution of iron phosphate and aluminum phosphate after being cooled to room temperature；It is that 2:1 prepares glycerol adding by the volume ratio of glycerol with iron phosphate and aluminum phosphate solution, after stirring 5min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；Mix with the ratio of 1:4 with the glycerine water solution that concentration is 55% in aluminum phosphate filter cake, after stirring 25min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；This glycerine water solution washing procedure of repetitive operation 5 times, and reclaim filtrate；Hydrogen peroxide mixes by the volume ratio of 1:1000 with reclaiming filtrate, and after standing 4min, dropping ammonia, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 5, flyash through 5 magnetic separation, then with 7% phosphoric acid mix by solid-to-liquid ratio 1:4, and at 110 DEG C, react 7h；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 iron phosphate and aluminum phosphate after being cooled to room temperature；It is that 2:1 prepares glycerol adding by the volume ratio of glycerol with iron phosphate and aluminum phosphate solution, after stirring 5min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；Mix with the ratio of 1:3 with the glycerine water solution that concentration is 65% in aluminum phosphate filter cake, after stirring 20min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；This glycerine water solution washing procedure of repetitive operation 6 times, and reclaim filtrate；Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 10, filters, obtains hydrated ferric oxide..
Embodiment 6, flyash through 3 magnetic separation, then with 6% phosphoric acid mix by solid-to-liquid ratio 1:3, and at 120 DEG C, react 6h；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 iron phosphate and aluminum phosphate after being cooled to room temperature；It is that 1:1 prepares glycerol adding by the volume ratio of glycerol with iron phosphate and aluminum phosphate solution, after stirring 5min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；Mix with the ratio of 1:2 with the glycerine water solution that concentration is 60% in aluminum phosphate filter cake, after stirring 10min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；This glycerine water solution washing procedure of repetitive operation 6 times, and reclaim filtrate；Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 10, filters, obtains hydrated ferric oxide..
Embodiment 7, flyash through 5 magnetic separation, then with 6% phosphoric acid mix by solid-to-liquid ratio 1:3, and at 100 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 iron phosphate and aluminum phosphate after being cooled to room temperature；It is that 1:1 prepares glycerol adding by the volume ratio of glycerol with iron phosphate and aluminum phosphate solution, after stirring 5min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；Add water with water solid-to-liquid ratio 3:1 preparation by aluminum phosphate filter cake, make aluminum phosphate dissolve, then be that 8:1 prepares glycerol adding by the volume ratio of glycerol Yu solution, after stirring 4min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；Hydrogen peroxide mixes by the volume ratio of 1:1000 with reclaiming filtrate, and after standing 3～5min, dropping ammonia, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 8, flyash through 4 magnetic separation, then with 8% phosphoric acid mix by solid-to-liquid ratio 1:5, and at 110 DEG C, react 5h；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 iron phosphate and aluminum phosphate after being cooled to room temperature；It is that 2:1 prepares glycerol adding by the volume ratio of glycerol with iron phosphate and aluminum phosphate solution, after stirring 4min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；Add water with water solid-to-liquid ratio 1:1 preparation by aluminum phosphate filter cake, make aluminum phosphate dissolve, then be that 7:1 prepares glycerol adding by the volume ratio of glycerol Yu solution, after stirring 5min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；Hydrogen peroxide mixes by the volume ratio of 2:1000 with reclaiming filtrate, and after standing 5min, dropping ammonia, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 9, flyash through 5 magnetic separation, then with 6% phosphoric acid mix by solid-to-liquid ratio 1:1, and at 100 DEG C, react 5h；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 iron phosphate and aluminum phosphate after being cooled to room temperature；It is that 2:1 prepares glycerol adding by the volume ratio of glycerol with iron phosphate and aluminum phosphate solution, after stirring 5min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；Add water with water solid-to-liquid ratio 3:1 preparation by aluminum phosphate filter cake, make aluminum phosphate dissolve, then be that 12:1 prepares glycerol adding by the volume ratio of glycerol Yu solution, after stirring 5min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 10, filters, obtains hydrated ferric oxide..
Embodiment 10, flyash through 4 magnetic separation, then with 8% phosphoric acid mix by solid-to-liquid ratio 1:2, and at 100 DEG C, react 8h；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 iron phosphate and aluminum phosphate after being cooled to room temperature；It is that 1:1 prepares glycerol adding by the volume ratio of glycerol with iron phosphate and aluminum phosphate solution, after stirring 4min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；Add water with water solid-to-liquid ratio 1:1 preparation by aluminum phosphate filter cake, make aluminum phosphate dissolve, then be that 7:1 prepares glycerol adding by the volume ratio of glycerol Yu solution, after stirring 5min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 10, 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 (7)
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 100 DEG C～120 DEG C, mixes flyash with the phosphoric acid that concentration is 3%～10% with the ratio that solid-to-liquid ratio is 1:1～1:5 of phosphoric acid in flyash, reacts 3～8h；
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 iron phosphate and aluminum phosphate；
4) glycerin extraction aluminum phosphate: glycerol and step 3) in the described solution that obtains mix by 1:1～2:1 volume ratio, after stirring 3～5min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；
5) aluminum sulfate filter cake is processed: mix with the ratio that solid-to-liquid ratio is 1:2～1:5 with the glycerine water solution that concentration is 55%～70% in aluminum phosphate filter cake, after stirring 10～30min, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate；This glycerine water solution washing procedure of repetitive operation 4～6 times, and reclaim filtrate；
6) ferrum oxide reclaims: hydrogen peroxide mixes by the volume ratio of 1:1000～2:1000 with described recovery filtrate, and after standing 3～5min, dropping ammonia, 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 characterized in that, the other method of described process aluminum sulfate filter cake includes: add water with water solid-to-liquid ratio 3:1～1:1 preparation by aluminum phosphate filter cake, aluminum phosphate is made to dissolve, again by the volume ratio of glycerol Yu solution be 3:1～12:1 prepare glycerol adding, stirring 3～5min after, sucking filtration, obtain aluminum phosphate filter cake, and reclaim filtrate.
3. as claimed in claim 1 a kind of separate the method for ferrum oxide in circulating fluid bed coal ash, it is characterized in that, described ferrum oxide reclaims other method and includes: dropping ammonia is in described recovery filtrate, to pH value of solution > 10, filter, obtain hydrated ferric oxide..
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 flyash is following component by mass percentage:
Al2O3+SiO2+Fe2O3> 50%, CaO > 10%.
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 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%.
6. 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.
7. as claimed in claim 6 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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