CN105600831A - Method for separating iron oxide in coal-powder boiler fly ash - Google Patents
Method for separating iron oxide in coal-powder boiler fly ash Download PDFInfo
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- CN105600831A CN105600831A CN201610066332.9A CN201610066332A CN105600831A CN 105600831 A CN105600831 A CN 105600831A CN 201610066332 A CN201610066332 A CN 201610066332A CN 105600831 A CN105600831 A CN 105600831A
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- aluminum phosphate
- iron oxide
- flyash
- filter cake
- coal
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000010881 fly ash Substances 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000000843 powder Substances 0.000 title claims abstract description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 108
- 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
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 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 10
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 5
- 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
- 239000000706 filtrate Substances 0.000 claims description 47
- 238000000967 suction filtration Methods 0.000 claims description 38
- 239000007788 liquid Substances 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000005955 Ferric phosphate Substances 0.000 claims description 24
- 229940032958 ferric phosphate Drugs 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
- 229910000399 iron(III) phosphate Inorganic materials 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 23
- 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
- 238000002360 preparation method Methods 0.000 claims description 16
- 238000000926 separation method Methods 0.000 claims description 15
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 14
- 235000014413 iron hydroxide Nutrition 0.000 claims description 14
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims description 14
- 238000011084 recovery Methods 0.000 claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 11
- 239000011324 bead Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 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
- 239000010883 coal ash Substances 0.000 claims description 4
- 238000003811 acetone extraction Methods 0.000 claims description 3
- 239000002956 ash Substances 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229910052682 stishovite Inorganic materials 0.000 claims description 3
- 229910052905 tridymite Inorganic materials 0.000 claims description 3
- 230000006698 induction Effects 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 1
- 238000000605 extraction Methods 0.000 description 6
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000010248 power generation Methods 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 239000003245 coal Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-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
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 229910001004 magnetic alloy Inorganic materials 0.000 description 1
- 239000006148 magnetic separator Substances 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
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 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
- 239000005060 rubber Substances 0.000 description 1
- 238000005245 sintering Methods 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
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Inorganic materials O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater 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
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/36—Aluminium phosphates
-
- 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)
- Compounds Of Iron (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention provides a method for separating iron oxide in coal-powder boiler fly ash. In the method, through a low-temperature hydrothermal reaction between phosphoric acid and fly ash, all Fe2O3 and FeO and some amorphous-state Al2O3 in the fly ash are dissolved out; and Fe2O3 and FeO in the solution are separated and extracted using acetone to obtain high-purity iron oxide. The method provided by the invention imposes no special requirements on equipment, adopts low-temperature reaction and can be used for efficiently separating and extracting iron oxide in fly ash. By adopting the method, 90-96% of aluminum oxide in the fly ash can be dissolved out, and 98-100% of iron oxide can be dissolved out; and the technical solution provided by the invention makes full use of the fly ash resource and has the advantages of simple production technology and low production cost and is suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of Ash Utilization and utilize method, specifically relate to a kind of separation in coal-powder boiler flyash and be oxidizedThe method of iron.
Background technology
Coal fired power generation is one of power generation mode of generally adopting of countries in the world, the coal-fired a large amount of flyash that produce effectivelyUtilize and become world subject. At present, China exceedes 70% electric power and is produced by coal fired power generation, national coalOutput about 30%, for generating, if consequent flyash utilization deficiency not only occupies a large amount of soils, causesSerious environmental pollution is also a kind of waste of resource.
From another angle, in flyash, be rich in many oxide, as Al2O3，SiO2，Fe2O3，FeO，CaO，MgO，SO3，Na2O，K2O etc., contain a small amount of rare earth element in addition. These oxides are divided from flyashFrom extracting and prepare corresponding high value-added product, not only can produce higher social economy's exploitation valueValue, also can alleviate the harm of flyash to environment.
The comprehensive utilizating research of flyash, the particularly research of separation and Extraction aluminium oxide from flyash, from last century 40Many experts both domestic and external, scholar carried out extensive work and proposed multiple separation and Extraction in this research so far ageMethod. But in the time extracting separation of oxygenated aluminium, iron oxide is disposed as impurity, not by Fe in flyash2O3With FeO recycling, cause the serious waste of resource.
And iron oxide is as a kind of inorganic pigment, be widely used in paint, rubber, plastics cosmetics, building fine grinding material,The fields such as accurate five metals instrument, optical glass, enamel, school supply and stationery, leather, magnetic alloy and high-grade alloy steel.
At present, Chinese scholars has proposed certain methods for separation and Extraction iron oxide from flyash, for example: calcium oxideSintering process, soda lime sintering process etc., but these methods due to process conditions restrictions, the iron oxide rate of recovery is low, power consumption is large,The reasons such as production cost is high, bed drain purge is large, cause separation and Extraction iron oxide implementation result poor.
The object of the invention is to utilize phosphoric acid,diluted to react with common coal-powder boiler flyash low-temperature hydrothermal, make in flyash wholeFe2O3, FeO and part amorphous state Al2O3Stripping, recycling acetone separation is extracted the Fe in solution2O3、FeO，Finally obtain the iron oxide product that purity is higher.
Summary of the invention
The object of this invention is to provide a kind of side that utilizes iron oxide in phosphoric acid and acetone extraction flyash under cryogenic conditionsMethod.
Technical scheme provided by the invention comprises utilizes phosphoric acid to react with flyash low-temperature hydrothermal, makes in flyash wholeFe2O3, FeO and part amorphous state Al2O3Stripping, recycling acetone separation is extracted the Fe in solution2O3, FeO comesTo highly purified iron oxide. Technical scheme manufacture craft provided by the invention is simple, reduce production costs, take full advantage ofThe resource of flyash, is applicable to large-scale production.
Realize the object of the invention technical scheme as follows:
Separate a method for iron oxide in coal-powder boiler flyash, described preparation method comprises the steps:
1) magnetic bead in magnetic separation separation of fine coal ash;
2) acidleach: at 120 DEG C～150 DEG C, the ratio that is 1:1～1:5 in the solid-to-liquid ratio of flyash and phosphoric acid is by fine coalThe phosphoric acid that ash is 3%～10% with concentration mixes, reaction 3～8h;
3) Separation of Solid and Liquid: reactant is cooled to after room temperature, suction filtration, it is 2 that filter cake is used by the solid-to-liquid ratio of flyash and water:The water washing of 1～1:2, obtains the solution of ferric phosphate and aluminum phosphate;
4) acetone extraction aluminum phosphate: by acetone and step 3) in the ferric phosphate that obtains and the volume ratio of aluminum phosphate solution be 1:1～3:1 preparation adds acetone, stirs after 3～5min, and suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate;
5) process aluminum sulfate filter cake: add dense by the solid-to-liquid ratio 1:2 of aluminum phosphate filter cake and aqueous acetone solution～1:5 preparationDegree is 40%～70% aqueous acetone solution, stirs after 10～30min, and suction filtration, then obtain aluminum phosphate filter cake, and reclaim filterLiquid; Repeat this aqueous acetone solution washing procedure 4～6 times, separate to greatest extent ferric phosphate, the final iron-holder that obtainsExtremely low aluminum phosphate filter cake, and reclaim filtrate;
6) iron oxide reclaims: add for 1:1000～2:1000 prepares by hydrogen peroxide and above-mentioned whole recovery filtrate volumes ratiosEnter hydrogen peroxide, leave standstill after 3～5min, drip ammoniacal liquor to pH value of solution > 8, filter, obtain highly purified iron hydroxide.
Further, described flyash is following component by mass percentage:
Al2O3+SiO2+Fe2O3＞70％，CaO＞5％。
Further, described flyash following component by mass percentage: Al2O3，29.87％；19.25％，47.08％；Fe2O3，7.01％；CaO，6.98％；SO3, 1.2%; Loss on ignition, 7.68%.
Further, described step 1) in, carry out wet magnetic separation separation with wet type low-intensity (magnetic) separator; A little less than described wet typeMagnetic field magnetic separator magnetic induction intensity 0.2T, pan feeding speed 500mL/min, material concentration 8%, magnetic separation 3～5 times.
Further, described step 1) object of magnetic separation is to isolate magnetic bead, isolates the main one-tenth of magnetic bead in flyashBe divided into Fe3O4. Because of Fe3O4Stable chemical nature, be difficult for reacting with strong acid and strong base, therefore be to make oxidation in flyashThe whole separation and Extraction of iron, must add magnetic separation step.
Further, the other method of described processing aluminum sulfate filter cake comprises: by aluminum phosphate filter cake and water solid-to-liquid ratio 3:1～1:1 preparation adds water, and aluminum phosphate is dissolved, then is that 3:1～12:1 preparation adds acetone by the volume ratio of acetone and solution,Stir after 3～5min, suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate.
Further, described iron oxide reclaims other method and comprises: in recovery filtrate, drip ammoniacal liquor, to pH value of solution >10, filter, obtain highly purified iron hydroxide.
With immediate prior art ratio, technical scheme provided by the invention has following excellent effect:
1, technical scheme provided by the invention, the fully iron oxide in 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 be by the alumina leaching in flyash 90%～96%, iron oxide stripping98％～100％。
4, technical scheme provided by the invention, flyash is after magnetic separation, and the rate of recovery of magnetic bead reaches more than 85%, magnetic bead grainFootpath is at 20～30um; From flyash, reclaim magnetic bead cost lower, except nonmagnetic portion iron in the flyash after magnetic bead containsMeasure lowlyer, be more conducive to integrated application; With magnetic bead in conjunction with High-gradient Magnetic isolation technics process waste water, can be by the phosphorus in waste waterClearance is effective, efficiency is high, treating capacity is large.
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, obviously, institute retouchesThe embodiment stating is only a part of embodiment of the present invention, instead of whole embodiment. Based on the enforcement in the present inventionExample, the every other embodiment that those of ordinary skill in the art obtain, belongs to the scope of protection of the invention.
Embodiment 1, flyash is through 4 magnetic separation, then mixes by solid-to-liquid ratio 1:2 with 5% phosphoric acid, and at 130 DEG CReaction 5h; Reaction finish be cooled to after room temperature, suction filtration obtains after filter cake, and with the solid-to-liquid ratio of flyash and water be 1:1Water washing, obtain the solution of ferric phosphate and aluminum phosphate; Be 3:1 by the volume ratio of acetone and ferric phosphate and aluminum phosphate solutionPreparation adds acetone, stirs after 5min, and suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate; Press aluminum phosphate filter cake and concentrationBe that 70% aqueous acetone solution mixes with the ratio of 1:3, stir after 15min, suction filtration, obtains aluminum phosphate filter cake, and returnsReceive filtrate; Repeat this aqueous acetone solution washing procedure 6 times, and reclaim filtrate; Hydrogen peroxide presses 1 with recovery filtrate:1000 volume ratio is mixed, and leaves standstill after 5min, drips ammoniacal liquor to pH value of solution > 8, filters, and obtains iron hydroxide.
Embodiment 2, flyash is through 3 magnetic separation, then mixes by solid-to-liquid ratio 1:3 with 8% phosphoric acid, and at 120 DEG CReaction 6h; Reaction finish be cooled to after room temperature, suction filtration obtains after filter cake, and with the solid-to-liquid ratio of flyash and water be 2:1Water washing, obtain the solution of ferric phosphate and aluminum phosphate; Be 2:1 by the volume ratio of acetone and ferric phosphate and aluminum phosphate solutionPreparation adds acetone, stirs after 3min, and suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate; Press aluminum phosphate filter cake and concentrationBe that 60% aqueous acetone solution mixes with the ratio of 1:5, stir after 30min, suction filtration, obtains aluminum phosphate filter cake, and returnsReceive filtrate; Repeat this aqueous acetone solution washing procedure 4 times, and reclaim filtrate; Hydrogen peroxide presses 1 with recovery filtrate:1000 volume ratio is mixed, and leaves standstill after 3min, drips ammoniacal liquor to pH value of solution > 8, filters, and obtains iron hydroxide.
Embodiment 3, flyash is through 3 magnetic separation, then mixes by solid-to-liquid ratio 1:2 with 3% phosphoric acid, and at 150 DEG CReaction 4h; Reaction finish be cooled to after room temperature, suction filtration obtains after filter cake, and with the solid-to-liquid ratio of flyash and water be 2:1Water washing, obtain the solution of ferric phosphate and aluminum phosphate; Be 1:1 by the volume ratio of acetone and ferric phosphate and aluminum phosphate solutionPreparation adds acetone, stirs after 5min, and suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate; Press aluminum phosphate filter cake and concentrationBe that 50% aqueous acetone solution mixes with the ratio of 1:2, stir after 10min, suction filtration, obtains aluminum phosphate filter cake, and returnsReceive filtrate; Repeat this aqueous acetone solution washing procedure 6 times, and reclaim filtrate; Hydrogen peroxide presses 2 with recovery filtrate:1000 volume ratio is mixed, and leaves standstill after 3min, drips ammoniacal liquor to pH value of solution > 8, filters, and obtains iron hydroxide.
Embodiment 4, flyash is through 5 magnetic separation, then mixes by solid-to-liquid ratio 1:4 with 9% phosphoric acid, and at 140 DEG CReaction 5h; Reaction finish be cooled to after room temperature, suction filtration obtains after filter cake, and with the solid-to-liquid ratio of flyash and water be 4:5Water washing, obtain the solution of ferric phosphate and aluminum phosphate; Be 2:1 by the volume ratio of acetone and ferric phosphate and aluminum phosphate solutionPreparation adds acetone, stirs after 5min, and suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate; Press aluminum phosphate filter cake and concentrationBe that 40% aqueous acetone solution mixes with the ratio of 1:4, stir after 25min, suction filtration, obtains aluminum phosphate filter cake, and returnsReceive filtrate; Repeat this aqueous acetone solution washing procedure 5 times, and reclaim filtrate; Hydrogen peroxide presses 1 with recovery filtrate:1000 volume ratio is mixed, and leaves standstill after 4min, drips ammoniacal liquor to pH value of solution > 8, filters, and obtains iron hydroxide.
Embodiment 5, flyash is through 5 magnetic separation, then mixes by solid-to-liquid ratio 1:4 with 7% phosphoric acid, and at 135 DEG CReaction 7h; Reaction finish be cooled to after room temperature, suction filtration obtains after filter cake, and with the solid-to-liquid ratio of flyash and water be 2:1Water washing, obtain the solution of ferric phosphate and aluminum phosphate; Be 3:1 by the volume ratio of acetone and ferric phosphate and aluminum phosphate solutionPreparation adds acetone, stirs after 5min, and suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate; Press aluminum phosphate filter cake and concentrationBe that 70% aqueous acetone solution mixes with the ratio of 1:3, stir after 20min, suction filtration, obtains aluminum phosphate filter cake, and returnsReceive filtrate; Repeat this aqueous acetone solution washing procedure 6 times, and reclaim filtrate; Drip ammoniacal liquor in reclaiming filtrate,To pH value of solution > 10, filter, obtain iron hydroxide.
Embodiment 6, flyash is through 3 magnetic separation, then mixes by solid-to-liquid ratio 1:3 with 6% phosphoric acid, and at 125 DEG CReaction 6h; Reaction finish be cooled to after room temperature, suction filtration obtains after filter cake, and with the solid-to-liquid ratio of flyash and water be 2:1Water washing, obtain the solution of ferric phosphate and aluminum phosphate; Be 2:1 by the volume ratio of acetone and ferric phosphate and aluminum phosphate solutionPreparation adds acetone, stirs after 5min, and suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate; Press aluminum phosphate filter cake and concentrationBe that 50% aqueous acetone solution mixes with the ratio of 1:2, stir after 10min, suction filtration, obtains aluminum phosphate filter cake, and returnsReceive filtrate; Repeat this aqueous acetone solution washing procedure 6 times, and reclaim filtrate; Drip ammoniacal liquor in reclaiming filtrate,To pH value of solution > 10, filter, obtain iron hydroxide.
Embodiment 7, flyash is through 5 magnetic separation, then mixes by solid-to-liquid ratio 1:3 with 6% phosphoric acid, and at 145 DEG CReaction 4h; Reaction finish be cooled to after room temperature, suction filtration obtains after filter cake, and with the solid-to-liquid ratio of flyash and water be 2:1Water washing, obtain the solution of ferric phosphate and aluminum phosphate; Be 3:1 by the volume ratio of acetone and ferric phosphate and aluminum phosphate solutionPreparation adds acetone, stirs after 5min, and suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate; Press aluminum phosphate filter cake and water solidLiquor ratio 3:1 preparation adds water, and aluminum phosphate is dissolved, then is that 8:1 preparation adds acetone by the volume ratio of acetone and solution, stirsMix after 4min, suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate; Hydrogen peroxide and recovery filtrate are pressed the volume of 1:1000Than mixing, leave standstill after 3～5min, drip ammoniacal liquor to pH value of solution > 8, filter, obtain iron hydroxide.
Embodiment 8, flyash is through 4 magnetic separation, then mixes by solid-to-liquid ratio 1:5 with 8% phosphoric acid, and at 130 DEG CReaction 5h; Reaction finish be cooled to after room temperature, suction filtration obtains after filter cake, and with the solid-to-liquid ratio of flyash and water be 1:2Water washing, obtain the solution of ferric phosphate and aluminum phosphate; Be 1:1 by the volume ratio of acetone and ferric phosphate and aluminum phosphate solutionPreparation adds acetone, stirs after 4min, and suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate; Press aluminum phosphate filter cake and water solidLiquor ratio 1:1 preparation adds water, and aluminum phosphate is dissolved, then is that 7:1 preparation adds acetone by the volume ratio of acetone and solution, stirsMix after 5min, suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate; Hydrogen peroxide and recovery filtrate are pressed the volume of 2:1000Than mixing, leave standstill after 5min, drip ammoniacal liquor to pH value of solution > 8, filter, obtain iron hydroxide.
Embodiment 9, flyash is through 5 magnetic separation, then mixes by solid-to-liquid ratio 1:1 with 6% phosphoric acid, and at 140 DEG CReaction 5h; Reaction finish be cooled to after room temperature, suction filtration obtains after filter cake, and with the solid-to-liquid ratio of flyash and water be 1:2Water washing, obtain the solution of ferric phosphate and aluminum phosphate; Be 2:1 by the volume ratio of acetone and ferric phosphate and aluminum phosphate solutionPreparation adds acetone, stirs after 5min, and suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate; Press aluminum phosphate filter cake and water solidLiquor ratio 3:1 preparation adds water, and aluminum phosphate is dissolved, then is that 12:1 preparation adds acetone by the volume ratio of acetone and solution,Stir after 5min, suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate; Drip ammoniacal liquor in reclaiming filtrate, to pH value of solution> 10, filters, and obtains iron hydroxide.
Embodiment 10, flyash is through 4 magnetic separation, then mixes by solid-to-liquid ratio 1:2 with 8% phosphoric acid, and at 150 DEG CLower reaction 8h; Reaction finish be cooled to after room temperature, suction filtration obtains after filter cake, and with the solid-to-liquid ratio of flyash and water be 1:2 water washing, obtains the solution of ferric phosphate and aluminum phosphate; Be 3 by the volume ratio of acetone and ferric phosphate and aluminum phosphate solution:1 preparation adds acetone, stirs after 4min, and suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate; Press aluminum phosphate filter cake and waterSolid-to-liquid ratio 1:1 preparation adds water, and aluminum phosphate is dissolved, then is that 7:1 preparation adds acetone by the volume ratio of acetone and solution,Stir after 5min, suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate; Drip ammoniacal liquor in reclaiming filtrate, to pH value of solution> 10, filters, and obtains iron hydroxide.
Gained sample in above-described embodiment is carried out respectively to performance test, obtain data as shown in table 1 below.
Table 1
Above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit, those of ordinary skill in the fieldShould be appreciated that with reference to above-described embodiment and can modify or be equal to replacement, these the specific embodiment of the present inventionDo not depart from any amendment of spirit and scope of the invention or be equal to and replace the claim protection domain all awaiting the reply in applicationWithin.
Claims (7)
1. a method that separates iron oxide in coal-powder boiler flyash, is characterized in that, described preparation method comprises the steps:
1) magnetic bead in magnetic separation separation of fine coal ash;
2) acidleach: at 120 DEG C～150 DEG C, the ratio that is 1:1～1:5 in the solid-to-liquid ratio of flyash and phosphoric acid by flyash withConcentration is 3%～10% phosphoric acid mixing, reaction 3～8h;
3) Separation of Solid and Liquid: reactant is cooled to after room temperature, suction filtration, it is 2:1～1 that filter cake is used by the solid-to-liquid ratio of flyash and water:2 water washing, obtains the solution of ferric phosphate and aluminum phosphate;
4) acetone extraction aluminum phosphate: acetone and step 3) in the described solution that obtains mix by 1:1～3:1 volume ratio, stirMix after 3～5min, suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate;
5) process aluminum sulfate filter cake: the aqueous acetone solution that is 40%～70% by aluminum phosphate filter cake and concentration taking solid-to-liquid ratio as 1:2～The ratio of 1:5 is mixed, and stirs after 10～30min, and suction filtration, obtains aluminum phosphate filter cake, and reclaims filtrate; Repeat this acetoneSolution washing operation 4～6 times, and reclaim filtrate;
6) iron oxide reclaims: hydrogen peroxide mixes by the volume ratio of 1:1000～2:1000 with described recovery filtrate, standing 3～After 5min, drip ammoniacal liquor to pH value of solution > 8, filter, obtain iron hydroxide.
2. a kind of method that separates iron oxide in coal-powder boiler flyash as claimed in claim 1, is characterized in that described processingThe other method of aluminum sulfate filter cake comprises: adds water by aluminum phosphate filter cake and water solid-to-liquid ratio 3:1～1:1 preparation, aluminum phosphate dissolved,Be that 3:1～12:1 preparation adds acetone by the volume ratio of acetone and solution again, stir after 3～5min, suction filtration, obtains aluminum phosphate filterCake, and reclaim filtrate.
3. a kind of method that separates iron oxide in coal-powder boiler flyash as claimed in claim 1, is characterized in that described oxidationIron reclaims other method and comprises: drip ammoniacal liquor in described recovery filtrate, to pH value of solution > 10, filter, obtain iron hydroxide.
4. a kind of method that separates iron oxide in coal-powder boiler flyash as claimed in claim 1, is characterized in that described fine coalAsh is following component by mass percentage:
Al2O3+SiO2+Fe2O3＞70％，CaO＞5％。
5. a kind of method that separates iron oxide in coal-powder boiler flyash as claimed in claim 4, is characterized in that described powderCoal ash following component by mass percentage: Al2O3，29.87％；19.25％，47.08％；Fe2O3，7.01％；CaO，6.98％；SO3, 1.2%; Loss on ignition, 7.68%.
6. a kind of method that separates iron oxide in coal-powder boiler flyash as claimed in claim 1, is characterized in that described step1), in, carry out wet magnetic separation separation with wet type low-intensity (magnetic) separator.
7. a kind of method that separates iron oxide in coal-powder boiler flyash as claimed in claim 6, is characterized in that described wet typeLow-intensity (magnetic) separator magnetic induction intensity 0.2T, pan feeding speed 500mL/min, material concentration 8%, magnetic separation 3～5 times.
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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 |
-
2016
- 2016-01-29 CN CN201610066332.9A patent/CN105600831A/en active Pending
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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Application publication date: 20160525 |