CN105692636A - 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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- CN105692636A CN105692636A CN201610065399.0A CN201610065399A CN105692636A CN 105692636 A CN105692636 A CN 105692636A CN 201610065399 A CN201610065399 A CN 201610065399A CN 105692636 A CN105692636 A CN 105692636A
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- 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
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- 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
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- 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)
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- 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
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- 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
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-4 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 12%～18%, 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 12%～18% 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-4 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-4 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 15%, 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 12%, 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 17%, 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 12%, 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 13%, 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 16%, 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 18%, 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 13%, 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 16% 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 18% 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 12%～18% 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 12%～18% 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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| 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 |
| CN109336123A (en) * | 2018-11-22 | 2019-02-15 | 山西大学 | A method of using coal ash for manufacturing for soluble glass of high modulus |
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| CN109336123A (en) * | 2018-11-22 | 2019-02-15 | 山西大学 | A method of using coal ash for manufacturing for soluble glass of high modulus |
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