CN105753002A - Method for preparing sodium silicate by utilizing coal ash of common circulating fluidized bed - Google Patents
Method for preparing sodium silicate by utilizing coal ash of common circulating fluidized bed Download PDFInfo
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- CN105753002A CN105753002A CN201610065421.1A CN201610065421A CN105753002A CN 105753002 A CN105753002 A CN 105753002A CN 201610065421 A CN201610065421 A CN 201610065421A CN 105753002 A CN105753002 A CN 105753002A
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- waterglass
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- flyash
- water
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000010883 coal ash Substances 0.000 title claims abstract description 13
- 239000004115 Sodium Silicate Substances 0.000 title abstract description 7
- 229910052911 sodium silicate Inorganic materials 0.000 title abstract description 7
- 238000002386 leaching Methods 0.000 claims abstract description 41
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- 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 11
- 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
- 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 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 6
- 239000010881 fly ash Substances 0.000 claims description 74
- 239000007788 liquid Substances 0.000 claims description 58
- 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 43
- 235000019353 potassium silicate Nutrition 0.000 claims description 40
- 239000002253 acid Substances 0.000 claims description 39
- 239000000843 powder Substances 0.000 claims description 26
- 238000007885 magnetic separation Methods 0.000 claims description 20
- 238000000227 grinding Methods 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 17
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 15
- 239000002893 slag Substances 0.000 claims description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 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
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 12
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000000967 suction filtration Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 10
- 239000011324 bead Substances 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000002956 ash Substances 0.000 claims description 5
- 235000013312 flour Nutrition 0.000 claims description 3
- 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
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000003518 caustics Substances 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract 3
- 230000002378 acidificating effect Effects 0.000 abstract 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 239000001117 sulphuric acid Substances 0.000 abstract 1
- 235000011149 sulphuric acid Nutrition 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 29
- 238000006243 chemical reaction Methods 0.000 description 14
- 239000000203 mixture Substances 0.000 description 13
- 239000000428 dust Substances 0.000 description 11
- 239000003245 coal Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000005243 fluidization Methods 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
- 238000004090 dissolution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000010248 power generation Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 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
- 239000011521 glass Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000006148 magnetic separator Substances 0.000 description 2
- 235000019795 sodium metasilicate Nutrition 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 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
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000001816 cooling Methods 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
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000004571 lime Substances 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
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 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
- 239000010453 quartz Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000011084 recovery Methods 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
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention provides a method for preparing sodium silicate by utilizing coal ash of a common circulating fluidized bed. The method comprises the following steps: reacting sulphuric acid and coal ash under a low-temperature roasting condition; dissolving Al2O3, Fe2O3 and FeO out from the coal ash; extracting SiO2 from acidic leaching residues by using a caustic solution by a high-temperature hydrothermal method to prepare the sodium silicate. The method provided by the invention is the method which has no special requirement on equipment and is used for preparing the sodium silicate by roasting at a low temperature and effectively utilizing SiO2 in the coal ash. According to the method provided by the invention, 90 to 96 percent of aluminium oxide and 98 to 100 percent of iron oxide can be dissolved out from the coal ash; the 78 to 84 percent of silicon dioxide in the acidic leaching residues is converted into liquid-2 type sodium silicate with the modulus greater than 3.1. According to the technical scheme provided by the invention, the resources of the coal ash are fully utilized; the manufacturing process is simple; the production cost is low; the method is suitable for large-scale production.
Description
Technical field
The present invention relates to the preparation method of a kind of waterglass, in particular to one and utilize ordinary cycle fluidization bed fly ash
The method preparing waterglass.
Background technology
Coal fired power generation is one of commonly used power generation mode in countries in the world, having of the coal-fired a large amount of flyash produced
Effect utilizes has become world subject.At present, China's electric power more than 70% is produced by coal fired power generation, whole nation coal
The yield of charcoal about 30% is used for generating electricity, and consequent flyash, if, with amount deficiency, not only occupies a large amount of soil,
Cause serious environmental pollution, be also the waste of a kind of resource.
Fluidization bed fly ash sinters due to its low-temperature circulating, and Circulating Fluidized Bed Ash cannot form glass phase and cause
Activity is relatively low, and fluidized bed ash is in sintering process in addition, is added with the lime of excess, during to itself gel
Between and intensity produce large effect, make fluidization bed fly ash activity relatively low, cannot be frozen into after aquation have certain strong
Degree, 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 make
Process by the mode buried, bury the seed of trouble of environmentally undesirable impact.Therefore the most effectively processing cycle fluidization bed fly ash becomes
For extremely urgent problem.
Say 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.By these oxides from flyash
Separation and Extraction out and prepares corresponding high value-added product, can not only produce higher social economy and utilize
It is worth, it is possible to alleviate the flyash harm to environment.
The aqueous solution common name waterglass of sodium metasilicate, waterglass is that a kind of purposes compares inorganic chemical product widely.Water glass
The production method of glass divides dry method (solid phase method) and wet method (liquid phase method) two kinds.Dry production is by quartz sand and soda ash
Being heated to about 1400 DEG C in reverberatory furnace after mixing by a certain percentage, generate molten sodium metasilicate, being characterized in can
Require to prepare waterglass according to different moduluses, but power consumption is bigger；Wet production is by caustic-soda aqueous solution and quartz
Powder is total to heat in autoclave and directly generates waterglass, is concentrated to give product water glass through filtering, though its power consumption is less 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 waterglass
New technology.Additionally, the content of silica is higher in flyash, its in flyash content between 34%～65%,
Silica 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 one roasting under cryogenic and can efficiently utilize ordinary cycle fluid bed powder coal
SiO in ash2The method preparing waterglass.
The technical scheme that the present invention provides is reacted under the conditions of including utilizing sulfuric acid and flyash low-temperature bake, makes in flyash
Most Al2O3、Fe2O3, FeO dissolution, recycling caustic solution high temperature hydro-thermal extracts the SiO in acid leaching residue2
Preparing waterglass, the technical scheme manufacture craft that the present invention provides is simple, reduce production cost, take full advantage of powder
The resource of coal ash, is suitable for large-scale production.
Realize the object of the invention technical scheme as follows:
A kind of ordinary cycle fluid-bed fly ash is utilized to comprise the steps: for the method for waterglass, preparation method
1) magnetic separation separates: this process is for the magnetic bead in magnetic separation separation flyash；
2) mechanical grinding: powder milling coal ash, improves its fineness and specific surface area；
3) acid dipping separation: the flyash after magnetic separation, grinding is mixed with the sulfuric acid that concentration is 80%～98%, control
Powder process coal ash is 2:1～1:1 with the solid-to-liquid ratio of sulfuric acid, adds thermal response 4～6h, and reaction temperature is 150 DEG C～220 DEG C；
4) separation of solid and liquid: after acid dipping separation reaction end is cooled to room temperature, be 1 according to the solid-to-liquid ratio of flyash Yu water:
2～1:6 preparations, heats 75～95 DEG C, stirring 1～3h, and suction filtration obtains filter cake, then consolidating with flyash and water
Liquor ratio is the water washing of 2:1～1:2, obtains ferric sulfate and the solution of 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 with solution be 1:1～1:2 addition concentration is
The soda lye of 11%～15%, heating 6～8h in autoclave, reaction temperature 160～200 DEG C, cooling
To room temperature, filter and wash solid slag with a small amount of water.
Further, by mass percentage, its chemical composition is Al to described flyash2O3+SiO2+Fe2O3＞ 50%,
CaO ＞ 10%.Described flyash uses 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, use magnetic bead in wet magnetic separation separation flyash, use wet type low-intensity magnetic field
Magnetic separator, magnetic separator magnetic separation condition is magnetic induction intensity 0.2T, pan feeding speed 500mL/min, material concentration 8%,
And carry out 3～5 magnetic separation.
Further, described step 2) in, machinery fine coal uses dry method grinding, uses roller to grind formula flour mill；Grinding machine
Control as mill speed 1000r/min～1200r/min, abrasive dust time 3～5min.
Further, described step 4) in separation of solid and liquid, the alumina leaching 90%～96% in flyash, oxidation
Iron dissolution 98%～100%；Described step 5) in, 78%～84% silica 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 1300～1500 DEG C
Lower calcining 2～5h, the ratio according still further to acid leaching residue with the solid-to-liquid ratio of solution be 1:1～1:2 add concentration be 11%～
The sodium hydroxide solution of 15%, in autoclave, heating 1～3h, reaction temperature 160～200 DEG C, be cooled to room
Wen Hou, filters and washs solid slag with a small amount of water.
Further, above-mentioned preparation method obtains modulus is liquid-2 type waterglass more than 3.1.
With immediate prior art ratio, the technical scheme that the present invention provides has a following excellent effect:
1, the technical scheme that the present invention provides, can the most efficiently utilize the silica in flyash to prepare modulus
For liquid-2 type waterglass more than 3.1.
2, the technical scheme that the present invention provides, utilizes the method treated coal ash of sulfuric acid low temperature roasting, to equipment without spy
Different requirement.
3, the technical scheme that the present invention provides, can be by the alumina leaching 90%～96% in flyash, and iron oxide is molten
Go out 98%～100%.
4, the technical scheme that the present invention provides, can be converted into waterglass by the silica of in acid leaching residue 78%～84%.
5, the technical scheme that the present invention provides, flyash is after magnetic separation, and the rate of recovery of magnetic bead reaches more than 85%, magnetic bead
Particle diameter is 20～30um；Magnetic bead cost is reclaimed relatively low, except nonmagnetic portion in the flyash after magnetic bead from flyash
Iron content is relatively low, is more beneficial for integrated application；Combine HGMS technology with magnetic bead and process waste water, can be by waste water
In tp removal rate effective, efficiency is high, treating capacity is big.
6, the technical scheme that the present invention provides, 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 institute
The embodiment described is only a part of embodiment of the present invention rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained, broadly fall into the scope of protection of the invention.
Embodiment 1, flyash is through 4 magnetic separation, then through mechanical grinding, mill speed is 1200r/min, abrasive dust 4min
After the fine powder powder that obtains, then with 82% sulfuric acid mix by solid-to-liquid ratio 5:4, and at 200 DEG C, react 4h；Instead
After should terminating to be cooled to room temperature, it is that 1:3 adds water by the solid-to-liquid ratio of flyash with water, is heated to 90 DEG C, stir 2h,
After suction filtration obtains filter cake, and it is that 1:1 washs by the solid-to-liquid ratio of flyash with water, obtains ferric sulfate and aluminum sulfate
Solution 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 caustic soda of 12.5%
Solution, and put into autoclave heating 8h, 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 2, flyash is through 5 magnetic separation, then through mechanical grinding, mill speed is 1100r/min, abrasive dust 4min
After the fine powder powder that obtains, then with 85% sulfuric acid mix by solid-to-liquid ratio 6:5, and at 200 DEG C, react 5h；Instead
After should terminating to be cooled to room temperature, it is that 1:3 adds water by the solid-to-liquid ratio of flyash with water, is heated to 85 DEG C, stir 2h,
After suction filtration obtains filter cake, and it is that 3:2 washs by the solid-to-liquid ratio of flyash with water, obtains ferric sulfate and aluminum sulfate
Solution and high silicon acid leaching residue；By acid leaching residue and the solid-to-liquid ratio of solution be 4:5 add concentration be 12% caustic soda molten
Liquid, and put into autoclave heating 7h, reaction temperature 180 DEG C；After being cooled to room temperature, filter and with a small amount of
Water washing solid slag, obtains waterglass.
Embodiment 3, flyash is through 4 magnetic separation, then through mechanical grinding, mill speed is 1000r/min, abrasive dust 4min
After the fine powder powder that obtains, then with 85% sulfuric acid mix by solid-to-liquid ratio 6:5, and at 200 DEG C, react 5h；Instead
After should terminating to be cooled to room temperature, it is that 1:4 adds water by the solid-to-liquid ratio of flyash with water, is heated to 80 DEG C, stir 2h,
After suction filtration obtains filter cake, and it is that 3:2 washs by the solid-to-liquid ratio of flyash with water, obtains ferric sulfate and aluminum sulfate
Solution and high silicon acid leaching residue；By acid leaching residue and the solid-to-liquid ratio of solution be 2:3 add concentration be 13% caustic soda molten
Liquid, and put into autoclave heating 6h, reaction temperature 200 DEG C；After being cooled to room temperature, filter and with a small amount of
Water washing solid slag, obtains waterglass.
Embodiment 4, flyash is through 3 magnetic separation, then through mechanical grinding, mill speed is 1200r/min, abrasive dust 5min
After the fine powder powder that obtains, then with 90% sulfuric acid mix by solid-to-liquid ratio 5:3, and at 220 DEG C, react 4h；Instead
After should terminating to be cooled to room temperature, it is that 1:3 adds water by the solid-to-liquid ratio of flyash with water, is heated to 95 DEG C, stir 3h,
After suction filtration obtains filter cake, and it is that 6:5 washs by the solid-to-liquid ratio of flyash with water, obtains ferric sulfate and aluminum sulfate
Solution and high silicon acid leaching residue；By acid leaching residue and the solid-to-liquid ratio of solution be 1:1 add concentration be 11% caustic soda molten
Liquid, and put into autoclave heating 7h, reaction temperature 180 DEG C；After being cooled to room temperature, filter and with a small amount of
Water washing solid slag, obtains waterglass.
Embodiment 5, flyash is through 5 magnetic separation, then through mechanical grinding, mill speed is 1100r/min, abrasive dust 4min
After the fine powder powder that obtains, then with 92% sulfuric acid mix by solid-to-liquid ratio 5:3, and at 180 DEG C, react 5h；Instead
After should terminating to be cooled to room temperature, it is that 1:3 adds water by the solid-to-liquid ratio of flyash with water, is heated to 95 DEG C, stir 3h,
After suction filtration obtains filter cake, and it is that 6:5 washs by the solid-to-liquid ratio of flyash with water, obtains ferric sulfate and aluminum sulfate
Solution and high silicon acid leaching residue；By acid leaching residue and the solid-to-liquid ratio of solution be 1:2 add concentration be 11% caustic soda molten
Liquid, and put into autoclave heating 6h, reaction temperature 190 DEG C；After being cooled to room temperature, filter and with a small amount of
Water washing solid slag, obtains waterglass.
Embodiment 6, flyash is through 5 magnetic separation, then through mechanical grinding, mill speed is 1000r/min, abrasive dust 3min
After the fine powder powder that obtains, then with 92% sulfuric acid mix by solid-to-liquid ratio 2:1, and at 150 DEG C, react 6h；Instead
After should terminating to be cooled to room temperature, it is that 1:6 adds water by the solid-to-liquid ratio of flyash with water, is heated to 75 DEG C, stir 1h,
After suction filtration obtains filter cake, and it is that 2:1 washs by the solid-to-liquid ratio of flyash with water, obtains ferric sulfate and aluminum sulfate
Solution and high silicon acid leaching residue；By acid leaching residue and the solid-to-liquid ratio of solution be 1:1 add concentration be 15% caustic soda molten
Liquid, and put into autoclave heating 6h, reaction temperature 200 DEG C；After being cooled to room temperature, filter and with a small amount of
Water washing solid slag, obtains waterglass.
Embodiment 7, flyash is through 3 magnetic separation, then through mechanical grinding, mill speed is 1200r/min, abrasive dust 3min
After the fine powder powder that obtains, then with 80% sulfuric acid mix by solid-to-liquid ratio 1:1, and at 220 DEG C, react 4h；Instead
After should terminating to be cooled to room temperature, it is that 1:2 adds water by the solid-to-liquid ratio of flyash with water, is heated to 95 DEG C, stir 3h,
After suction filtration obtains filter cake, and it is that 1:2 washs by the solid-to-liquid ratio of flyash with water, obtains ferric sulfate and aluminum sulfate
Solution and high silicon acid leaching residue；By acid leaching residue and the solid-to-liquid ratio of solution be 1:2 add concentration be 14% caustic soda molten
Liquid, and put into autoclave heating 8h, reaction temperature 160 DEG C；After being cooled to room temperature, filter and with a small amount of
Water washing solid slag, obtains waterglass.
Embodiment 8, flyash is through 3 magnetic separation, then through mechanical grinding, mill speed is 1200r/min, abrasive dust 3min
After the fine powder powder that obtains, then with 80% sulfuric acid mix by solid-to-liquid ratio 1:1, and at 220 DEG C, react 4h；Instead
After should terminating to be cooled to room temperature, it is that 1:2 adds water by the solid-to-liquid ratio of flyash with water, is heated to 95 DEG C, stir 3h,
After suction filtration obtains filter cake, and it is that 1:2 washs by the solid-to-liquid ratio of flyash with water, obtains ferric sulfate and aluminum sulfate
Solution and high silicon acid leaching residue；Acid leaching residue carries out calcining at 1300 DEG C 4h, then presses the solid-to-liquid ratio of acid leaching residue and solution
Ratio be 1:1 add concentration be the sodium hydroxide solution of 14%, in autoclave heat 3h, reaction temperature
200 DEG C, after being cooled to room temperature, filter and i.e. obtain waterglass with a small amount of water washing solid slag.
Embodiment 9, flyash is through 4 magnetic separation, then through mechanical grinding, mill speed is 1200r/min, abrasive dust 4min
After the fine powder powder that obtains, then with 82% sulfuric acid mix by solid-to-liquid ratio 5:4, and at 200 DEG C, react 4h；Instead
After should terminating to be cooled to room temperature, it is that 1:3 adds water by the solid-to-liquid ratio of flyash with water, is heated to 90 DEG C, stir 2h,
After suction filtration obtains filter cake, and it is that 1:1 washs by the solid-to-liquid ratio of flyash with water, obtains ferric sulfate and aluminum sulfate
Solution and high silicon acid leaching residue；Acid leaching residue carries out calcining at 1400 DEG C 5h, according still further to the solid-liquid of acid leaching residue Yu solution
The ratio of ratio be 1:2 add concentration be the sodium hydroxide solution of 12%, in autoclave heat 2h, 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 10, flyash is through 3 magnetic separation, then through mechanical grinding, mill speed is 1200r/min, abrasive dust
The fine powder powder obtained after 5min, then with 90% sulfuric acid mix by solid-to-liquid ratio 5:3, and at 220 DEG C react
4h；After reaction end is cooled to room temperature, it is that 1:3 adds water by the solid-to-liquid ratio of flyash with water, is heated to 95 DEG C, stirs
Mix 3h, after suction filtration obtains filter cake, and be that 6:5 washs by the solid-to-liquid ratio of flyash with water, obtain ferric sulfate with
The solution of aluminum sulfate and high silicon acid leaching residue；Acid leaching residue carries out calcining at 1300 DEG C 3h, according still further to acid leaching residue and solution
The ratio of solid-to-liquid ratio be that to add concentration be the sodium hydroxide solution of 11% to 1:1, in autoclave, heat 1h, instead
Answer temperature 200 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 only in order to illustrate that technical scheme is not intended to limit, the ordinary skill people of art
Member should be appreciated that and can modify the detailed description of the invention of the present invention or equivalent with reference to above-described embodiment,
These claims all awaited the reply in application without departing from any amendment or the equivalent of spirit and scope of the invention are protected
Within the scope of protecting.
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 flyash；
2) mechanical grinding；
3) acidleach: at 150 DEG C～220 DEG C, in the ratio that solid-to-liquid ratio is 2:1～1:1 of flyash and sulfuric acid by powder
Coal ash mixes with the sulfuric acid that concentration is 80%～98%, reacts 4～6h；
4) separation of solid and liquid: after reactant is cooled to room temperature, is 1:2～1:6 by the solid-to-liquid ratio of flyash Yu water
Preparation adds water, at 75～95 DEG C, after stirring 1～3h, and suction filtration, filter cake is with being 2 by the solid-to-liquid ratio of flyash Yu water:
The water washing of 1～1:2, obtains ferric sulfate and the solution of aluminum sulfate and high silicon acid leaching residue；
5) acid leaching residue prepares waterglass: be 1:1～1 by the soda lye of acid leaching residue and 11%～15% by solid-to-liquid ratio:
The proportions mixed liquor of 2, after heating 6～8h, is cooled to room temperature, filters also at 160～200 DEG C in reactor
Wash solid slag with water.
A kind of utilize ordinary cycle fluid-bed fly ash for the method for waterglass, its
Being characterised by, described flyash is following component by mass percentage:
Al2O3+SiO2+Fe2O3＞ 50%, CaO ＞ 10%.
A kind of utilizing ordinary cycle fluid-bed fly ash for the method for waterglass, it is special
Levying and be, 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%.
A kind of utilize ordinary cycle fluid-bed fly ash for the method for waterglass, its
It is characterised by, described step 1) in, carry out wet magnetic separation separation with wet type low-intensity (magnetic) separator.
A kind of utilize ordinary cycle fluid-bed fly ash for the method for waterglass, its
It is characterised by, described wet type low-intensity (magnetic) separator magnetic induction intensity 0.2T, pan feeding speed 500mL/min, material concentration
8%, magnetic separation 3～5 times.
A kind of utilize ordinary cycle fluid-bed fly ash for the method for waterglass, its
It is characterised by, described step 2) in, described mechanical grinding is that roller grinds formula flour mill dry method grinding.
A kind of utilize ordinary cycle fluid-bed fly ash for the method for waterglass, its
Being characterised by, described roller grinds formula flour mill mill speed 1000r/min～1200r/min, grinding 3～5min.
A kind of utilize ordinary cycle fluid-bed fly ash for the method for waterglass, its
Being characterised by, described acid leaching residue is prepared another processing method of waterglass and is included: at 1300～1500 DEG C forge acid leaching residue
Burn after 2～5h, then by acid leaching residue and 11%～15% sodium hydroxide solution by the ratio that solid-to-liquid ratio is 1:1～1:2
Example preparation mixed liquor, at 160～200 DEG C, heating 1～3h in reactor, is cooled to room temperature, filters and wash with water solid
Body slag i.e. obtains waterglass.
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| CN105692635A (en) * | 2016-01-29 | 2016-06-22 | 卓达新材料科技集团有限公司 | Method for preparing water glass using fly ash of common circulating fluidized bed |
| CN109592693A (en) * | 2018-11-22 | 2019-04-09 | 中国神华能源股份有限公司 | A kind of method that acid leaching residue produces waterglass |
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| CN109592693A (en) * | 2018-11-22 | 2019-04-09 | 中国神华能源股份有限公司 | A kind of method that acid leaching residue produces waterglass |
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