CN105776236A - Method for preparing sodium silicate by means of ordinary pulverized coal ash of pulverized coal furnace - Google Patents
Method for preparing sodium silicate by means of ordinary pulverized coal ash of pulverized coal furnace Download PDFInfo
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- CN105776236A CN105776236A CN201610066903.9A CN201610066903A CN105776236A CN 105776236 A CN105776236 A CN 105776236A CN 201610066903 A CN201610066903 A CN 201610066903A CN 105776236 A CN105776236 A CN 105776236A
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- 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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Abstract
The invention provides a method for preparing sodium silicate by means of ordinary pulverized coal ash of a pulverized coal furnace.The method comprises the steps that sulfuric acid is reacted with the pulverized coal ash under the low temperature roasting condition, Al2O3, Fe2O3 and FeO in the pulverized coal ash are dissolved out, and a caustic alkali solution is used for hydrothermally extracting SiO2 in acid leaching slag at high temperature to prepare sodium silicate.The method has no special requirement on equipment, low temperature roasting is achieved, and SiO2 in the pulverized coal ash can be efficiently utilized for preparing sodium silicate; by means of the method, 90%-96% of aluminum oxide in the pulverized coal ash can be dissolved out, and 98%-100% of iron oxide in the pulverized coal ash can be dissolved out; 74%-80% of silicon dioxide in the acid leaching slag is converted into liquid-3-type sodium silicate of which the modulus is larger than 2.6.According to the method for preparing sodium silicate by means of the ordinary pulverized coal ash of the pulverized coal furnace, the pulverized coal 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 present invention relates to the preparation method of a kind of waterglass, a kind of utilize common coal-powder boiler coal ash for manufacturing for the method for waterglass.
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.
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.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 metasilicate, 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 be quartz sand and soda ash are mixed by a certain percentage after in reverberatory furnace, be heated to about 1400 DEG C, generate molten sodium metasilicate, be 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 in autoclave heat directly generate 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 the new technology of waterglass.Additionally, the content of silica is higher in flyash, in flyash, content is between 34%～65% for it, and the 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 a kind of roasting under cryogenic and can efficiently utilize the SiO in ordinary cycle fluidization bed fly 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 most Al in flyash2O3、Fe2O3, FeO dissolution, recycling caustic solution high temperature hydro-thermal extracts the SiO in acid leaching residue2Preparing waterglass, the technical scheme manufacture craft that the present invention provides 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 common coal-powder boiler coal ash for manufacturing 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 flyash；
2) mechanical grinding: powder milling coal ash, improves its fineness and specific surface area；
3) acid dipping separation: at 260 DEG C～320 DEG C, is mixed flyash with the sulfuric acid that concentration is 90%～98% with the ratio that solid-to-liquid ratio is 4:1～1:1 of sulfuric acid in flyash, reacts 4～8h；
4) separation of solid and liquid: 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 suction filtration obtains filter cake, again with the water that solid-to-liquid ratio is 2:1～the 1:2 washing of flyash with water, obtain 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 Yu solution be 1:1～1:2 adds the soda lye that concentration is 14%～18%, 6～8h are heated in autoclave, reaction temperature 160～180 DEG C, after being cooled to room temperature, filter and with a small amount of water washing solid slag.
Further, by mass percentage, its chemical composition is Al to described flyash2O3+SiO2+Fe2O3＞ 70%, CaO ＞ 5%.By mass percentage, its chemical composition is as follows: Al for described flyash2O3, 29.87%；19.25%, 47.08%；Fe2O3, 7.01%；CaO, 6.98%；SO3, 1.2%；Loss on ignition, 7.68%.
Further, described step 1) in, using magnetic bead in wet magnetic separation separation flyash, use wet type low-intensity (magnetic) separator, magnetic separator magnetic separation condition is magnetic induction intensity 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 uses dry method grinding, uses roller to grind formula flour mill；Grinding machine controlled 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, iron oxide dissolution 98%～100%；Described step 5) in, 74%～80% silica in acid leaching residue is converted into waterglass.
Further, described step 5) can be selected for another technical scheme replacement, acid leaching residue carries out calcining at 1300～1500 DEG C 2～5h, ratio according still further to acid leaching residue with the solid-to-liquid ratio of solution is 1:1～1:2 adds the sodium hydroxide solution that concentration is 14%～18%, 1～3h is heated in autoclave, reaction temperature 160～180 DEG C, after being cooled to room temperature, filter and with a small amount of water washing solid slag.
Further, above-mentioned preparation method obtains modulus is liquid-3 type waterglass more than 2.6.
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 is liquid-3 type waterglass more than 2.6.
2, the technical scheme that the present invention provides, utilizes the method treated coal ash of sulfuric acid low temperature roasting, to equipment without particular/special requirement.
3, the technical scheme that the present invention provides, can be by the alumina leaching 90%～96% in flyash, iron oxide dissolution 98%～100%.
4, the technical scheme that the present invention provides, can be converted into waterglass by the silica of in acid leaching residue 74%～80%.
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%, and magnetic bead particle diameter is 20～30um；From flyash, reclaim magnetic bead cost relatively low, except nonmagnetic portion iron content is relatively low in the flyash after magnetic bead, be more beneficial for integrated application；With magnetic bead combine HGMS technology process waste water, can by effective for the tp removal rate in waste water, 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 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 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, the fine powder powder obtained after abrasive dust 4min, then with 90% sulfuric acid mix by solid-to-liquid ratio 9:4, and at 280 DEG C react 5h；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 90 DEG C, stir 2h, after suction filtration obtains filter cake, and be that 1:1 washs by the solid-to-liquid ratio of flyash with water, obtain ferric sulfate and the solution of 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 8h, 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, then through mechanical grinding, mill speed is 1100r/min, the fine powder powder obtained after abrasive dust 4min, then with 98% sulfuric acid mix by solid-to-liquid ratio 9:5, and at 280 DEG C react 6h；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 85 DEG C, stir 2h, after suction filtration obtains filter cake, and be that 3:2 washs by the solid-to-liquid ratio of flyash with water, obtain ferric sulfate and the solution of 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 14%, and put into autoclave heat 7h, 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, then through mechanical grinding, mill speed is 1000r/min, the fine powder powder obtained after abrasive dust 4min, then with 94% sulfuric acid mix by solid-to-liquid ratio 3:1, and at 300 DEG C react 6h；After reaction end is 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 be that 3:2 washs by the solid-to-liquid ratio of flyash with water, obtain ferric sulfate and the solution of 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 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 4, flyash is through 3 magnetic separation, then through mechanical grinding, mill speed is 1200r/min, the fine powder powder obtained after abrasive dust 5min, then with 94% sulfuric acid mix by solid-to-liquid ratio 4:1, and at 290 DEG C react 7h；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, stir 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 and the solution of 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 7h, 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, then through mechanical grinding, mill speed is 1100r/min, the fine powder powder obtained after abrasive dust 4min, then with 96% sulfuric acid mix by solid-to-liquid ratio 2:1, and at 310 DEG C react 7h；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, stir 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 and the solution of 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 15%, 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, then through mechanical grinding, mill speed is 1000r/min, the fine powder powder obtained after abrasive dust 3min, then with 92% sulfuric acid mix by solid-to-liquid ratio 2:1, and at 260 DEG C react 6h；After reaction end is 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 be that 2:1 washs by the solid-to-liquid ratio of flyash with water, obtain ferric sulfate and the solution of 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 14%, 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 7, flyash is through 3 magnetic separation, then through mechanical grinding, mill speed is 1200r/min, the fine powder powder obtained after abrasive dust 3min, then with 94% sulfuric acid mix by solid-to-liquid ratio 1:1, and at 270 DEG C react 6h；After reaction end is 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 be that 1:2 washs by the solid-to-liquid ratio of flyash with water, obtain ferric sulfate and the solution of 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 8h, 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, then through mechanical grinding, mill speed is 1200r/min, the fine powder powder obtained after abrasive dust 3min, then with 96% sulfuric acid mix by solid-to-liquid ratio 3:1, and at 280 DEG C react 6h；After reaction end is 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 be that 1:2 washs by the solid-to-liquid ratio of flyash with water, obtain ferric sulfate and the solution of aluminum sulfate and high silicon acid leaching residue；Acid leaching residue carries out calcining at 1300 DEG C 4h, 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 14%, in autoclave heat 3h, reaction temperature 180 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, the fine powder powder obtained after abrasive dust 4min, then with 93% sulfuric acid mix by solid-to-liquid ratio 7:4, and at 290 DEG C react 8h；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 90 DEG C, stir 2h, after suction filtration obtains filter cake, and be that 1:1 washs by the solid-to-liquid ratio of flyash with water, obtain ferric sulfate and the solution of aluminum sulfate and high silicon acid leaching residue；Acid leaching residue carries out calcining at 1400 DEG C 5h, is that to add concentration be the sodium hydroxide solution of 15% 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, then through mechanical grinding, mill speed is 1200r/min, the fine powder powder obtained after abrasive dust 5min, then with 94% sulfuric acid mix by solid-to-liquid ratio 7:3, and at 270 DEG C react 6h；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, stir 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 and the solution of aluminum sulfate and high silicon acid leaching residue；Acid leaching residue carries out calcining at 1300 DEG C 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 detailed description of the invention of the present invention can be modified or equivalent with reference to above-described embodiment, these without departing from any amendment of spirit and scope of the invention or equivalent all within the claims that application is awaited the reply.
Claims (8)
1. one kind utilizes common coal-powder boiler coal ash for manufacturing for the method for waterglass, it is characterised in that described preparation method
Comprise the steps:
1) magnetic bead in magnetic separation separation flyash；
2) mechanical grinding；
3) acidleach: at 260 DEG C～320 DEG C, in the ratio that solid-to-liquid ratio is 4:1～1:1 of flyash and sulfuric acid by powder
Coal ash mixes with the sulfuric acid that concentration is 90%～98%, reacts 4～8h；
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: by acid leaching residue and 14%～18% soda lye by solid-to-liquid ratio be 1:1～
The proportions mixed liquor of 1:2, after heating 6～8h, is cooled to room temperature, mistake at 160～180 DEG C in reactor
Filter and wash solid slag with water.
The most as claimed in claim 1 a kind of utilize common coal-powder boiler coal ash for manufacturing for the method for waterglass, its feature
Being, described flyash is following component by mass percentage:
Al2O3+SiO2+Fe2O3＞ 70%, CaO ＞ 5%.
The most as claimed in claim 2 a kind of common coal-powder boiler coal ash for manufacturing is utilized to exist for the method for waterglass, its feature
In, described flyash is following component by mass percentage: Al2O3, 29.87%；19.25%, 47.08%；
Fe2O3, 7.01%；CaO, 6.98%；SO3, 1.2%；Loss on ignition, 7.68%.
The most as claimed in claim 1 a kind of common coal-powder boiler coal ash for manufacturing is utilized to exist for the method for waterglass, its feature
In, described step 1) in, carry out wet magnetic separation separation with wet type low-intensity (magnetic) separator.
The most as claimed in claim 4 a kind of utilize common coal-powder boiler coal ash for manufacturing for the method for waterglass, its feature
It is, 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.
The most as claimed in claim 1 a kind of utilize common coal-powder boiler coal ash for manufacturing for the method for waterglass, its feature
It is, described step 2) in, described mechanical grinding is that roller grinds formula flour mill dry method grinding.
The most as claimed in claim 6 a kind of utilize common coal-powder boiler coal ash for manufacturing for the method for waterglass, its feature
Being, described roller grinds formula flour mill mill speed 1000r/min～1200r/min, grinding 3～5min.
The most as claimed in claim 1 a kind of utilize common coal-powder boiler coal ash for manufacturing for the method for waterglass, its feature
Being, described acid leaching residue is prepared another processing method of waterglass and is included: at 1300～1500 DEG C calcine acid leaching residue
After 2～5h, then by acid leaching residue and 14%～18% sodium hydroxide solution in the ratio that solid-to-liquid ratio is 1:1～1:2
Preparation mixed liquor, at 160～180 DEG C, heating 1～3h in reactor, is cooled to room temperature, filters and wash solid with water
Slag i.e. obtains waterglass.
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| CN105621428A (en) * | 2016-01-29 | 2016-06-01 | 卓达新材料科技集团有限公司 | Method for preparing sodium silicate by using common pulverized fuel ash from pulverized coal furnace |
| CN109665534A (en) * | 2018-11-22 | 2019-04-23 | 山西大学 | A method of mesopore silicon oxide is prepared using flyash acid leaching residue |
| CN111302350A (en) * | 2020-03-05 | 2020-06-19 | 武汉理工大学 | Nanocrystal core suspension based on industrial solid waste and preparation method thereof |
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| CN105621428A (en) * | 2016-01-29 | 2016-06-01 | 卓达新材料科技集团有限公司 | Method for preparing sodium silicate by using common pulverized fuel ash from pulverized coal furnace |
| CN109665534A (en) * | 2018-11-22 | 2019-04-23 | 山西大学 | A method of mesopore silicon oxide is prepared using flyash acid leaching residue |
| CN109665534B (en) * | 2018-11-22 | 2022-05-20 | 山西大学 | Method for preparing mesoporous silicon oxide by using fly ash acid leaching residue |
| CN111302350A (en) * | 2020-03-05 | 2020-06-19 | 武汉理工大学 | Nanocrystal core suspension based on industrial solid waste and preparation method thereof |
| CN111302350B (en) * | 2020-03-05 | 2021-09-10 | 武汉理工大学 | Nanocrystal core suspension based on industrial solid waste and preparation method thereof |
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