CN105692635A - Method for preparing water glass using fly ash of common circulating fluidized bed - Google Patents
Method for preparing water glass using fly ash of common circulating fluidized bed Download PDFInfo
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- CN105692635A CN105692635A CN201610065388.2A CN201610065388A CN105692635A CN 105692635 A CN105692635 A CN 105692635A CN 201610065388 A CN201610065388 A CN 201610065388A CN 105692635 A CN105692635 A CN 105692635A
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- fly ash
- waterglass
- solid
- flyash
- leaching residue
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- 239000010881 fly ash Substances 0.000 title claims abstract description 81
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 235000019353 potassium silicate Nutrition 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000002253 acid Substances 0.000 claims abstract description 41
- 238000002386 leaching Methods 0.000 claims abstract description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 31
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000377 silicon dioxide Substances 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 7
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 7
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 7
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 7
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 51
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 238000007885 magnetic separation Methods 0.000 claims description 20
- 238000000227 grinding Methods 0.000 claims description 18
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 15
- 239000001117 sulphuric acid Substances 0.000 claims description 15
- 235000011149 sulphuric acid Nutrition 0.000 claims description 15
- 239000002893 slag Substances 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 13
- 229910052710 silicon Inorganic materials 0.000 claims description 13
- 239000010703 silicon Substances 0.000 claims description 13
- 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 12
- 239000012065 filter cake Substances 0.000 claims description 12
- 229910000358 iron sulfate Inorganic materials 0.000 claims description 12
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 10
- 239000011324 bead Substances 0.000 claims description 8
- 239000010883 coal ash Substances 0.000 claims description 7
- 239000002956 ash Substances 0.000 claims description 4
- 235000013312 flour Nutrition 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000006698 induction Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 238000003672 processing method Methods 0.000 claims 1
- 239000000376 reactant Substances 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000003518 caustics Substances 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 28
- 238000006243 chemical reaction Methods 0.000 description 24
- 239000000843 powder Substances 0.000 description 21
- 239000000203 mixture Substances 0.000 description 12
- 238000010298 pulverizing process Methods 0.000 description 11
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000001354 calcination Methods 0.000 description 4
- 239000003245 coal Substances 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005243 fluidization Methods 0.000 description 4
- 238000010248 power generation Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000004115 Sodium Silicate Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 241001274660 Modulus Species 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000006148 magnetic separator Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- NOTVAPJNGZMVSD-UHFFFAOYSA-N potassium monoxide Inorganic materials [K]O[K] NOTVAPJNGZMVSD-UHFFFAOYSA-N 0.000 description 1
- 238000007780 powder milling Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Inorganic materials O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
-
- 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
- C01F7/68—Aluminium compounds containing sulfur
- C01F7/74—Sulfates
- C01F7/743—Preparation from silicoaluminious materials, e.g. clays or bauxite
-
- 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]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/14—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention provides a method for preparing water glass using the fly ash of a common circulating fluidized bed. The method comprises the following steps: enabling sulfuric acid and fly ash to react in a low-temperature roasting condition to dissolve out Al2O3, Fe2O3 and FeO from the fly ash; and performing high-temperature hydrothermal extraction of SiO2 from acid leaching residue using a caustic alkali solution to prepare water glass. The method provided by the invention imposes no special requirements on equipment, adopts low-temperature roasting and can make efficient use of SiO2 in the fly ash to prepare water glass; in the method provided by the invention, 90-96% of aluminum oxide and 98-100% of iron oxide in the fly ash can be dissolved out; and 70-78% of silicon dioxide in the acid leaching residue is converted into liquid-5 type water glass of which the modulus is greater than 2.2. In the technical scheme provided by the invention, the fly ash resource is fully utilized, the preparation technology is simple, the production cost is low, and the method is suitable for large-scale production.
Description
Technical field
The preparation method that the present invention relates to a kind of waterglass, utilizes ordinary cycle fluid-bed fly ash for the method for waterglass 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 aqueous solution common name waterglass of sodium silicate, waterglass is that a kind of purposes compares inorganic chemical product widely。The production method of waterglass divides dry method (solid phase method) and wet method (liquid phase method) two kinds。Dry production is to be heated to about 1400 DEG C in reverberatory furnace after quartz sand and soda being mixed by a certain percentage, generates molten sodium silicate, is characterized in require to prepare waterglass according to different moduluses, but power consumption is bigger；Wet production is caustic-soda aqueous solution and silica flour to be total to heat in autoclave directly generate waterglass, obtains product water glass through filtering and concentrating, though its power consumption is lower than dry method, but the SiO of the crystal state in silica flour2Dissolution rate is low, alkaline consumption is high。
For making full use of resource, reducing production cost, many researchs are developing different silicon sources to prepare the new technique of waterglass。Additionally, the content of silicon dioxide is higher in flyash, in flyash, content is between 34%～65% for it, and the silicon dioxide in extract powder coal ash prepares waterglass, effectively raises the comprehensive utilization value of flyash。
Summary of the invention
It is an object of the invention to provide a kind of roasting under cryogenic and can efficiently utilize the SiO in ordinary cycle fluidization bed fly ash2The method preparing waterglass。
Technical scheme provided by the invention includes utilizing when sulphuric acid and flyash low-temperature bake reacts, and makes most Al in flyash2O3、Fe2O3, FeO dissolution, recycling caustic solution high temperature hydro-thermal extracts the SiO in acid leaching residue2Preparing waterglass, 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 utilizing ordinary cycle fluid-bed fly ash for the method for waterglass, preparation method comprises the steps:
1) magnetic separation separates: this process is for the magnetic bead in magnetic separation separation of fine coal ash；
2) mechanical grinding: powder milling coal ash, improves its fineness and specific surface area；
3) acid dipping separation: mixed with the sulphuric acid that concentration is 80%～98% by the flyash after magnetic separation, grinding, the solid-to-liquid ratio controlling flyash and sulphuric acid is 2:1～1:1, and reacting by heating 4～6h, reaction temperature is 150 DEG C～220 DEG C；
4) solid-liquid separation: after acid dipping separation reaction end is cooled to room temperature, it is 1:2～1:6 preparation according to the solid-to-liquid ratio of flyash Yu water, heat 75～95 DEG C, stirring 1～3h, and sucking filtration obtains filter cake, again with the water washing that solid-to-liquid ratio is 2:1～1:2 of flyash Yu water, obtain the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue；
5) acid leaching residue prepares waterglass: according to the solid-to-liquid ratio of acid leaching residue Yu solution be 1:1～1:2 add concentration be the soda lye of 18%～20%, 4～6h is heated in autoclave, reaction temperature 160～180 DEG C, after being cooled to room temperature, filters and with a small amount of water washing solid slag。
Further, by mass percentage, its chemical composition is Al to described flyash2O3+SiO2+Fe2O3> 50%, CaO > 10%。Described flyash adopts Peng Lai ash, and by mass percentage, its chemical composition is as follows: 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, adopting magnetic bead in wet magnetic separation separation of fine coal ash, use wet type low-intensity (magnetic) separator, magnetic separator magnetic separation condition is magnetic induction 0.2T, pan feeding speed 500mL/min, material concentration 8%, and carries out 3～5 magnetic separation。
Further, described step 2) in, machinery fine coal adopts dry method grinding, uses roller to grind formula flour mill；Grinding machine controls as mill speed 1000r/min～1200r/min, pulverizing time 3～5min。
Further, described step 4) in solid-liquid separation, the alumina leaching 90%～96% in flyash, ferrum oxide dissolution 98%～100%；Described step 5) in, 70%～78% silicon dioxide in acid leaching residue is converted into waterglass。
Further, described step 5) can be selected for another technical scheme replacement, acid leaching residue is carried out calcining 2～5h at 1300～1500 DEG C, it is that to add concentration be the sodium hydroxide solution of 18%～20% to 1:1～1:2 according still further to the ratio of acid leaching residue with the solid-to-liquid ratio of solution, 1～3h is heated in autoclave, reaction temperature 160～180 DEG C, after being cooled to room temperature, filters and with a small amount of water washing solid slag。
Further, above-mentioned preparation method obtains modulus is liquid-5 type waterglass more than 2.2。
With immediate prior art ratio, technical scheme provided by the invention has following excellent effect:
1, technical scheme provided by the invention, can fully efficiently utilize the silicon dioxide in flyash to prepare modulus is liquid-5 type waterglass more than 2.2。
2, technical scheme provided by the invention, utilizes the method treated coal ash of sulfuric acid low temperature roasting, 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, can be converted into waterglass by the silicon dioxide of 70%～78% in acid leaching residue。
5, 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。
6, 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 is through 4 magnetic separation, and then through mechanical grinding, mill speed is 1200r/min, the fine powder powder obtained after pulverizing 4min, then with 82% sulphuric acid mix by solid-to-liquid ratio 5:4, and at 200 DEG C react 4h；Reaction end is that 1:3 adds water by the solid-to-liquid ratio of flyash Yu water, is heated to 90 DEG C after being cooled to room temperature, stirs 2h, after sucking filtration obtains filter cake, and is that 1:1 washs by the solid-to-liquid ratio of flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue；By the solid-to-liquid ratio of acid leaching residue Yu solution be 1:1 add concentration be the soda lye of 19%, and put into autoclave heat 6h, reaction temperature 170 DEG C；After being cooled to room temperature, filter and with a small amount of water washing solid slag, obtain waterglass。
Embodiment 2, flyash is through 5 magnetic separation, and then through mechanical grinding, mill speed is 1100r/min, the fine powder powder obtained after pulverizing 4min, then with 85% sulphuric acid mix by solid-to-liquid ratio 6:5, and at 200 DEG C react 5h；Reaction end is that 1:3 adds water by the solid-to-liquid ratio of flyash Yu water, is heated to 85 DEG C after being cooled to room temperature, stirs 2h, after sucking filtration obtains filter cake, and is that 3:2 washs by the solid-to-liquid ratio of flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue；By the solid-to-liquid ratio of acid leaching residue Yu solution be 4:5 add concentration be the soda lye of 18%, and put into autoclave heat 5h, reaction temperature 170 DEG C；After being cooled to room temperature, filter and with a small amount of water washing solid slag, obtain waterglass。
Embodiment 3, flyash is through 4 magnetic separation, and then through mechanical grinding, mill speed is 1000r/min, the fine powder powder obtained after pulverizing 4min, then with 85% sulphuric acid mix by solid-to-liquid ratio 6:5, and at 200 DEG C react 5h；Reaction end is that 1:4 adds water by the solid-to-liquid ratio of flyash Yu water, is heated to 80 DEG C after being cooled to room temperature, stirs 2h, after sucking filtration obtains filter cake, and is that 3:2 washs by the solid-to-liquid ratio of flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue；By the solid-to-liquid ratio of acid leaching residue Yu solution be 2:3 add concentration be the soda lye of 20%, and put into autoclave heat 4h, reaction temperature 160 DEG C；After being cooled to room temperature, filter and with a small amount of water washing solid slag, obtain waterglass。
Embodiment 4, flyash is through 3 magnetic separation, and then through mechanical grinding, mill speed is 1200r/min, the fine powder powder obtained after pulverizing 5min, then with 90% sulphuric acid mix by solid-to-liquid ratio 5:3, and at 220 DEG C react 4h；Reaction end is that 1:3 adds water by the solid-to-liquid ratio of flyash Yu water, is heated to 95 DEG C after being cooled to room temperature, stirs 3h, after sucking filtration obtains filter cake, and is that 6:5 washs by the solid-to-liquid ratio of flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue；By the solid-to-liquid ratio of acid leaching residue Yu solution be 1:1 add concentration be the soda lye of 18%, and put into autoclave heat 5h, reaction temperature 180 DEG C；After being cooled to room temperature, filter and with a small amount of water washing solid slag, obtain waterglass。
Embodiment 5, flyash is through 5 magnetic separation, and then through mechanical grinding, mill speed is 1100r/min, the fine powder powder obtained after pulverizing 4min, then with 92% sulphuric acid mix by solid-to-liquid ratio 5:3, and at 180 DEG C react 5h；Reaction end is that 1:3 adds water by the solid-to-liquid ratio of flyash Yu water, is heated to 95 DEG C after being cooled to room temperature, stirs 3h, after sucking filtration obtains filter cake, and is that 6:5 washs by the solid-to-liquid ratio of flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue；By the solid-to-liquid ratio of acid leaching residue Yu solution be 1:2 add concentration be the soda lye of 18%, and put into autoclave heat 6h, reaction temperature 180 DEG C；After being cooled to room temperature, filter and with a small amount of water washing solid slag, obtain waterglass。
Embodiment 6, flyash is through 5 magnetic separation, and then through mechanical grinding, mill speed is 1000r/min, the fine powder powder obtained after pulverizing 3min, then with 92% sulphuric acid mix by solid-to-liquid ratio 2:1, and at 150 DEG C react 6h；Reaction end is that 1:6 adds water by the solid-to-liquid ratio of flyash Yu water, is heated to 75 DEG C after being cooled to room temperature, stirs 1h, after sucking filtration obtains filter cake, and is that 2:1 washs by the solid-to-liquid ratio of flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue；By the solid-to-liquid ratio of acid leaching residue Yu solution be 1:1 add concentration be the soda lye of 19%, and put into autoclave heat 5h, reaction temperature 170 DEG C；After being cooled to room temperature, filter and with a small amount of water washing solid slag, obtain waterglass。
Embodiment 7, flyash is through 3 magnetic separation, and then through mechanical grinding, mill speed is 1200r/min, the fine powder powder obtained after pulverizing 3min, then with 80% sulphuric acid mix by solid-to-liquid ratio 1:1, and at 220 DEG C react 4h；Reaction end is that 1:2 adds water by the solid-to-liquid ratio of flyash Yu water, is heated to 95 DEG C after being cooled to room temperature, stirs 3h, after sucking filtration obtains filter cake, and is that 1:2 washs by the solid-to-liquid ratio of flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue；By the solid-to-liquid ratio of acid leaching residue Yu solution be 1:2 add concentration be the soda lye of 20%, and put into autoclave heat 6h, reaction temperature 160 DEG C；After being cooled to room temperature, filter and with a small amount of water washing solid slag, obtain waterglass。
Embodiment 8, flyash is through 3 magnetic separation, and then through mechanical grinding, mill speed is 1200r/min, the fine powder powder obtained after pulverizing 3min, then with 80% sulphuric acid mix by solid-to-liquid ratio 1:1, and at 220 DEG C react 4h；Reaction end is that 1:2 adds water by the solid-to-liquid ratio of flyash Yu water, is heated to 95 DEG C after being cooled to room temperature, stirs 3h, after sucking filtration obtains filter cake, and is that 1:2 washs by the solid-to-liquid ratio of flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue；Acid leaching residue is carried out calcining 4h at 1300 DEG C, again by the ratio of acid leaching residue with the solid-to-liquid ratio of solution be 1:1 add concentration be the sodium hydroxide solution of 18%, in autoclave heat 3h, reaction temperature 180 DEG C, after being cooled to room temperature, filter and namely obtain waterglass with a small amount of water washing solid slag。
Embodiment 9, flyash is through 4 magnetic separation, and then through mechanical grinding, mill speed is 1200r/min, the fine powder powder obtained after pulverizing 4min, then with 82% sulphuric acid mix by solid-to-liquid ratio 5:4, and at 200 DEG C react 4h；Reaction end is that 1:3 adds water by the solid-to-liquid ratio of flyash Yu water, is heated to 90 DEG C after being cooled to room temperature, stirs 2h, after sucking filtration obtains filter cake, and is that 1:1 washs by the solid-to-liquid ratio of flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue；Acid leaching residue is carried out at 1400 DEG C calcining 5h, is that to add concentration be the sodium hydroxide solution of 19% to 1:2 according still further to the ratio of acid leaching residue with the solid-to-liquid ratio of solution, in autoclave, heats 2h, reaction temperature 170 DEG C, after being cooled to room temperature, filter and with a small amount of water washing solid slag, obtain waterglass。
Embodiment 10, flyash is through 3 magnetic separation, and then through mechanical grinding, mill speed is 1200r/min, the fine powder powder obtained after pulverizing 5min, then with 90% sulphuric acid mix by solid-to-liquid ratio 5:3, and at 220 DEG C react 4h；Reaction end is that 1:3 adds water by the solid-to-liquid ratio of flyash Yu water, is heated to 95 DEG C after being cooled to room temperature, stirs 3h, after sucking filtration obtains filter cake, and is that 6:5 washs by the solid-to-liquid ratio of flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue；Acid leaching residue is carried out at 1300 DEG C calcining 3h, is that to add concentration be the sodium hydroxide solution of 20% to 1:1 according still further to the ratio of acid leaching residue with the solid-to-liquid ratio of solution, in autoclave, heats 1h, reaction temperature 160 DEG C, after being cooled to room temperature, filter and with a small amount of water washing solid slag, obtain waterglass。
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 (8)
1. one kind utilizes ordinary cycle fluid-bed fly ash for the method for waterglass, it is characterised in that described preparation method comprises the steps:
1) magnetic bead in magnetic separation separation of fine coal ash；
2) mechanical grinding；
3) acidleach: at 150 DEG C～220 DEG C, mixes flyash with the sulphuric acid that concentration is 80%～98% with the ratio that solid-to-liquid ratio is 2:1～1:1 of sulphuric acid in flyash, reacts 4～6h；
4) solid-liquid separation: after reactant is cooled to room temperature, it is that 1:2～1:6 preparation adds water by the solid-to-liquid ratio of flyash Yu water, at 75～95 DEG C, after stirring 1～3h, sucking filtration, the filter cake water washing that solid-to-liquid ratio is 2:1～1:2 by flyash Yu water, obtains the solution of iron sulfate and aluminum sulfate and high silicon acid leaching residue；
5) acid leaching residue prepares waterglass: by acid leaching residue and 18%～20% soda lye by the proportions mixed liquor that solid-to-liquid ratio is 1:1～1:2, heat after 4～6h in reactor at 160～180 DEG C, be cooled to room temperature, filter and wash solid slag with water。
2. a kind of as claimed in claim 1 utilize ordinary cycle fluid-bed fly ash for the method for waterglass, it is characterised in that described flyash is following component by mass percentage:
Al2O3+SiO2+Fe2O3> 50%, CaO > 10%。
3. a kind of as claimed in claim 2 utilize ordinary cycle fluid-bed fly ash for the method for waterglass, 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. a kind of as claimed in claim 1 utilize ordinary cycle fluid-bed fly ash for the method for waterglass, it is characterised in that described step 1) in, carry out wet magnetic separation separation with wet type low-intensity (magnetic) separator。
5. a kind of as claimed in claim 4 utilize ordinary cycle fluid-bed fly ash for the method for waterglass, 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。
6. a kind of as claimed in claim 1 utilize ordinary cycle fluid-bed fly ash for the method for waterglass, it is characterised in that described step 2) in, described mechanical grinding is that roller grinds formula flour mill dry method grinding。
7. a kind of as claimed in claim 6 utilize ordinary cycle fluid-bed fly ash for the method for waterglass, it is characterised in that described roller grinds formula flour mill mill speed 1000r/min～1200r/min, grinding 3～5min。
8. a kind of as claimed in claim 1 utilize ordinary cycle fluid-bed fly ash for the method for waterglass, it is characterized in that, described acid leaching residue is prepared another processing method of waterglass and is included: after acid leaching residue being calcined 2～5h at 1300～1500 DEG C, again by acid leaching residue and 18%～20% sodium hydroxide solution by the proportions mixed liquor that solid-to-liquid ratio is 1:1～1:2, heating 1～3h in reactor at 160～180 DEG C, it is cooled to room temperature, filters and wash with water solid slag and namely obtain waterglass。
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