CN105540596A - Method for preparing silicon dioxide from high-silicon and high-iron fly ash - Google Patents
Method for preparing silicon dioxide from high-silicon and high-iron fly ash Download PDFInfo
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- CN105540596A CN105540596A CN201610014846.XA CN201610014846A CN105540596A CN 105540596 A CN105540596 A CN 105540596A CN 201610014846 A CN201610014846 A CN 201610014846A CN 105540596 A CN105540596 A CN 105540596A
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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
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/124—Preparation of adsorbing porous silica not in gel form and not finely divided, i.e. silicon skeletons, by acidic treatment of siliceous materials
Abstract
The invention discloses a method for preparing silicon dioxide from high-silicon and high-iron fly ash. The method for preparing silicon dioxide from the fly ash is conducted on the technological condition that the ratio of m<fly ash> to m<NaCO3> is 1 to 1.2, the calcination temperature is 800 DEG C, the calcination time is two hours, the gel-gel temperature is 94 DEG C, and the yield of silicon dioxide is 85.35%. According to the method for preparing silicon dioxide from the high-silicon and high-iron fly ash, the high-silicon and high-iron fly ash serves as the raw material, silicon dioxide is prepared through the steps of fly-ash activation, hydrochloric acid leaching, sol obtaining and gel obtaining, the acid leaching decomposition rate of activated clinker and the yield of silicon dioxide are taken as evaluation indexes to study and analyze multiple factors which affect the silicon dioxide extraction process to seek a reasonable processing technology routine for preparing silicon dioxide from the fly ash, and therefore a technological support can be provided for industrial application of extracting silicon dioxide from the high-silicon and high-iron fly ash.
Description
Technical field
The invention belongs to technical field of chemistry and chemical engineering, particularly relate to a kind of method of high silicon high iron coal ash for manufacturing prepared silicon dioxide.
Background technology
Flyash receives in the flue gas after pulverized coal friring to catch the thin ash got off, and be one of primary solids refuse of coal-burning power plant's discharge, flyash contains abundant silicon-dioxide (23.1% ~ 62.4%), Al
2o
3(17.8% ~ 30%), Fe
2o
3oxide compounds such as (2.0% ~ 7.1%), can be used as the important source material that silicon-dioxide, aluminum oxide etc. extract.
At present, the document about silicon-dioxide in extract powder coal ash is a lot, but relates generally to the aspects such as the economic rationality of the purity of silicon-dioxide in flyash, quality, appearance structure and extraction process route, and the research for the productive rate of silicon in flyash is little.
Summary of the invention
The object of the present invention is to provide a kind of method of high silicon high iron coal ash for manufacturing prepared silicon dioxide, be intended to solve the problem that the low iron powder coal ash of existing high alumina only pays close attention to the extraction of aluminium and the inferior quality of silicon-dioxide.
The method of high silicon high iron coal ash for manufacturing prepared silicon dioxide of the present invention, the method for the method high silicon high iron coal ash for manufacturing prepared silicon dioxide of described high silicon high iron coal ash for manufacturing prepared silicon dioxide comprises:
By flyash and anhydrous sodium carbonate in the dry 24h of the dry case of the constant-temperature vacuum being placed in 105 DEG C, then take out and be placed in drying basin to be chilled to room temperature stand-by, m
flyash: m
sodium carbonate=1:1.2;
Take flyash and anhydrous sodium carbonate, be placed in 30mL porcelain crucible, be positioned over after stirring be warming up to 800 DEG C retort furnace in roasting 2h, after roasting terminates, take out and be placed in drying basin that to be chilled to room temperature stand-by;
Roasting grog is placed in 250mL beaker, after material is fully wetting with water, use glass stick to add hydrochloric acid soln while stirring, and proceed in ultrasonic cleaning machine ultrasonic;
After ultrasonic end, filter above-mentioned acidleach product, and wash filter cake with hydrochloric acid, collection filtrate is stand-by; Use tap water filter cake again until neutrality, after filter residue being placed in the constant-temperature vacuum dry case inner drying 24h of 105 DEG C, being chilled to room temperature and weighing;
Gained filtrate is proceeded in 250mL beaker, measure pH, put into thermostat water bath and carry out sol-gel, measuring pH<0.5 when there is colloidal sol, after collosol and gel terminates, measuring pH<0.5;
After sol-gel terminates, under the power of 240W, carry out ultrasonic 5min acidleach with the hydrochloric acid soln of the 1mol/L of 20mL to above-mentioned Silica hydrogel, carry out centrifugation after acidleach terminates, this step repeats 3 times;
Under the wet gel of gained being put into the power of 240W, wash to straight neutrality with the ultrasonic 5min of the tap water of 20mL, filter residue is placed in the dry case of constant-temperature vacuum dry, and weighs.
Further, glass stick is used to add the hydrochloric acid soln 35mL of 3mol/L while stirring.
Further, ultrasonic 1min in the ultrasonic cleaning machine of 240W is proceeded to.
Further, with the hydrochloric acid 10mL of 3mol/L, filter cake is washed.
Further, filter residue is placed in the dry 24h of the dry case of constant-temperature vacuum of 105 DEG C.
The method of high silicon high iron coal ash for manufacturing prepared silicon dioxide provided by the invention, with high silicon high iron flyash for raw material, the method of flyash activating-hydrochloric acid acidleach-sol-gel is adopted to prepare silicon-dioxide, with acidleach rate of decomposition, silicon-dioxide productive rate for evaluation index, research and analysis are carried out on the factors affected in silicon-dioxide leaching process, the processing technology routine of the coal ash for manufacturing prepared silicon dioxide of reasonable, thinks that the industrial application of high silicon high iron flyash extraction silicon-dioxide provides technical support.
Accompanying drawing explanation
Fig. 1 is the method flow diagram of the high silicon high iron coal ash for manufacturing prepared silicon dioxide that the embodiment of the present invention provides.
What Fig. 2 was the material proportion that provides of the embodiment of the present invention on acidleach rate of decomposition and silicon-dioxide productive rate affects schematic diagram.
What Fig. 3 was the maturing temperature that provides of the embodiment of the present invention on acidleach rate of decomposition and silicon-dioxide productive rate affects schematic diagram.
What Fig. 4 was the roasting time that provides of the embodiment of the present invention on flyash rate of decomposition and silicon-dioxide productive rate affects schematic diagram.
What Fig. 5 was the hydrochloric acid consumption that provides of the embodiment of the present invention on acidleach rate of decomposition and silicon-dioxide productive rate affects schematic diagram.
What Fig. 6 was the pickling liquor concentration that provides of the embodiment of the present invention on flyash rate of decomposition and silicon-dioxide productive rate affects schematic diagram.
Fig. 7 is that under the identical rate of decomposition that provides of the embodiment of the present invention, sol-gel liquid starting point concentration affects schematic diagram to silicon-dioxide productive rate.
Fig. 8 is that under the identical rate of decomposition that provides of the embodiment of the present invention, Sol-gel transition temperatures affects schematic diagram to silicon-dioxide productive rate.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The present invention take sodium carbonate as activator activating fly ash, investigates composition of raw materials, roasting condition (temperature, time), acidleach condition (consumption, concentration), colloidal sol-gelation condition (starting point concentration, the temperature) impact on silicon-dioxide productive rate.Result shows: 1) flyash is not having to carry out high-temperature activation under auxiliary agent condition, and acidleach rate of decomposition is 24.13%, without silica product.2) concentration of hydrochloric acid and sol-gel liquid starting point concentration on the productive rate of silicon-dioxide substantially without impact.3) temperature is the remarkable factor affecting sol-gel.4) optimum process condition is: m
powder coal ash: m
sodium carbonate=1:1.2, maturing temperature 800 DEG C, roasting time 2h; Gel-gelling temp 94 DEG C, the productive rate of silicon-dioxide can reach 85.35%.
Below in conjunction with accompanying drawing, application principle of the present invention is explained in detail.
As shown in Figure 1, the method for high silicon high iron coal ash for manufacturing prepared silicon dioxide of the present invention comprises the following steps:
S101: by flyash and anhydrous sodium carbonate in the dry 24h of the dry case of the constant-temperature vacuum being placed in 105 DEG C, then takes out and is placed in drying basin to be chilled to room temperature stand-by;
S102: accurately take above-mentioned over dry flyash 2.0000g and 2.4000g over dry anhydrous sodium carbonate, be placed in 30mL porcelain crucible, be positioned over after stirring be warming up to 800 DEG C retort furnace in roasting 2h, after roasting terminates, take out immediately and be placed in drying basin that to be chilled to room temperature stand-by;
S103: above-mentioned roasting grog is placed in 250mL beaker, after material is fully wetting by suitable quantity of water, use glass stick to add the hydrochloric acid soln 35mL of 3mol/L while stirring, and proceeds to rapidly ultrasonic 1min in the ultrasonic cleaning machine of 240W;
S104: after ultrasonic end, filters above-mentioned acidleach product, and washs filter cake with the hydrochloric acid 10mL of 3mol/L, and collection filtrate is stand-by; Use tap water filter cake again until neutrality, after filter residue being placed in the constant-temperature vacuum dry case inner drying 24h of 105 DEG C, being chilled to room temperature and weighing;
S105: proceed in 250mL beaker by above-mentioned gained filtrate, measures pH, puts into thermostat water bath and carry out sol-gel, measuring pH<0.5, after collosol and gel terminates, measuring pH<0.5 when there is colloidal sol;
S106: after sol-gel terminates, under the power of 240W, carry out ultrasonic 5min acidleach with the hydrochloric acid soln of the 1mol/L of 20mL to above-mentioned Silica hydrogel, carry out centrifugation after acidleach terminates, this step repeats 3 times;
S107: under the wet gel of gained being put into the power of 240W, washs to straight neutrality with the ultrasonic 5min of the tap water of 20mL, filter residue is placed in the dry 24h of the dry case of constant-temperature vacuum of 105 DEG C, and weighs.
Below in conjunction with experiment, application principle of the present invention is further described.
1. experimental section
1.1 experiment reagents and instrument
Reagent: flyash, six Pan Shui Qian Gui power plant; Anhydrous sodium carbonate (AR, Chongqing Mao Ye chemical reagent company limited); Hydrochloric acid (AR, Chongqing river and mountain Chemical Co., Ltd.); Dehydrated alcohol (AR, Tianjin Fu Yu Fine Chemical Co., Ltd).
Instrument: KQ-300DE numerical control supersonic cleaning machine, Kunshan Ultrasonic Instruments Co., Ltd.; TG1650-WS whizzer, Hunan Saite Xiang Yi whizzer Instrument Ltd.; The dry case of DZ-88 electric heating constant temperature vacuum, Shanghai leap medical apparatus and instruments factory; FA1004 analytical balance, the flat responsibility company limited in upper sea; HWSK-5 muffle furnace, Hebi City Hua Tong analytical instrument company; HH-S thermostat water bath, Hengfeng instrument plant of Jintan City.
1.2 experimental technique
Sodium carbonate activating fly ash mainly forms the product that silico-aluminate etc. is soluble in acid, for the stripping improving silicon, aluminium in flyash is active, take hydrochloric acid as pickling liquor, composition of raw materials, maturing temperature, roasting time and pickling liquor consumption and concentration are investigated to the impact of silicon, aluminium solubility rate, solubility rate higher then silicon-dioxide productive rate is also high, for research silicate solution colloidal sol-gelation condition is on the impact of productive rate, investigate the impact of sol solutions starting point concentration and temperature, under specific experiment step is shown in:
1. accurately take flyash (the meter m of 1:1.2 (mass ratio, lower same)
1) and sodium carbonate in the baking oven inner drying 24h of 105 DEG C, mix after being chilled to room temperature and be placed in roasting 2h in the inherent 800 DEG C of retort furnaces of porcelain crucible, roasting terminates rear taking-up, and to be placed in drying basin stand-by;
2. above-mentioned sample is placed in 250mL beaker, adds the hydrochloric acid soln of the 3mol/L of 35mL while stirring, after end to be dissolved, filter, wash to neutral, after filter residue being placed in the baking oven inner drying 24h of 105 DEG C, be chilled to room temperature weightometer m
2.
3. above-mentioned gained filtrate is put into thermostat water bath and carry out sol-gel, after sol-gel terminates, adopt the hydrochloric acid soln of the 1mol/L of 20mL to carry out secondary pickling and centrifugation, product is placed in the dry 24h of the dry case of constant-temperature vacuum of 105 DEG C, meter m
3.
1.3 evaluation index
The optimization of processing condition is evaluated with the productive rate of the acidleach rate of decomposition of roasting grog and silica product, and flyash activating effect is better, and acidleach rate of decomposition is higher, and its productive rate is also high.The calculating formula of rate of decomposition is shown in formula (1-1), and the calculating formula of productive rate is shown in formula (2-2).
In formula, η
1, η
2-flyash rate of decomposition, silicon-dioxide productive rate, %;
M
0-silicon-dioxide Theoretical Mass, g; m
1-flyash quality, g;
M
2-acidleach mass of residue, g; m
3-silicon-dioxide experimental yield, g;
2 results and discussion
The impact of 2.1 flyash and sodium carbonate quality proportioning
Flyash and sodium carbonate amount by 1:0,1:0.6,1:0.8,1:1.0,1:1.2,1:1.4,1:1.6,1.8,1:2.0 carries out proportioning, except quality proportioning, all the other processes are all tested by the carrying out of 1.2, the results are shown in Figure 2.
As seen from Figure 2, when sodium carbonate amount is 0, the acidleach rate of decomposition of roasting grog is 24.13%, but there is no silica product, illustrate in pickling liquor substantially do not have silicon compound, only high-temperature activation flyash can not change the structure of silicon in flyash and makes it to react with hydrochloric acid to enter solution system; Along with Na
2cO
3the increase of consumption, rate of decomposition and the silicon-dioxide productive rate of flyash increase gradually, work as m
flyash: m
sodium carbonateduring=1:1.4, acidleach rate of decomposition is 95.61%, and silicon-dioxide productive rate is 86.40%, works as m
flyash: m
sodium carbonateduring=1:1.6, acidleach rate of decomposition and silicon-dioxide productive rate slightly decline, and work as m
flyash: m
sodium carbonateduring>=1:1.8, because sample generation sintering cannot take out acidleach from crucible, and cause acidleach rate of decomposition and productive rate reduces to zero rapidly.
Sodium carbonate amount is in the scope of 0.6 ~ 1.4; acidleach rate of decomposition and productive rate slightly increase; but increasing degree is more slow; loft, the complexity of taking out from crucible of roasting grog in Binding experiment process; and reducing the angle of raw materials cost and protective roast equipment, the quality proportioning of suggestion flyash and sodium carbonate adopts 1:1.2 comparatively suitable.Now, the acidleach rate of decomposition of roasting grog is 95.58%, and silicon-dioxide productive rate is 85.89%.
The impact of 2.2 maturing temperatures
Investigate maturing temperature at room temperature (~ 25 DEG C), the acidleach rate of decomposition of 650 DEG C, 700 DEG C, 750 DEG C, 800 DEG C, 850 DEG C, 900 DEG C flyash and the variation relation of silicon-dioxide productive rate, except maturing temperature, all the other processes are all tested by 1.2, the results are shown in Figure 3.
As seen from Figure 3: in the scope of 25 DEG C ~ 800 DEG C, acidleach rate of decomposition and the silicon-dioxide productive rate of roasting grog increase along with the increase of maturing temperature, when maturing temperature >=850 DEG C, because sample generation sintering cannot take out acidleach from crucible, and cause acidleach rate of decomposition and productive rate reduces to zero rapidly.After 800 DEG C of roastings, the acidleach rate of decomposition of roasting grog can reach 96.28%, and silicon-dioxide productive rate is 86.03%.
In conjunction with the experimental data of 1.1, by powdered coal ash acidleach and direct acidleach of not roasting after roasting 2h in the retort furnace of 800 DEG C, the former 24.13% the latter of its acidleach rate of decomposition is 65.52%, but all without silica product.After powdered coal ash direct roasting is described, is only that mineral crystal formation develops more stable, considerable change is not occurred for the weave construction between the chemical element in flyash.
The impact of 2.3 roasting time
After flyash and sodium carbonate are carried out proportioning according to the quality of 1:1.2, mix and be placed in difference roasting 0h, 0.5h, 1h, 1.5h, 2h, 2.5h, 3h in 800 DEG C of retort furnaces, all the other processes are tested according to 1.2, the results are shown in Figure 4.
As seen from Figure 4: along with the prolongation of roasting time, the acidleach rate of decomposition of roasting grog and silicon-dioxide productive rate also increase thereupon; When being upon firing 2h, rate of decomposition and silicon-dioxide productive rate can reach 95.87%, 85.52% respectively; More than after 2h upon firing, rate of decomposition and silicon-dioxide productive rate slightly reduce.In the time range of 0.5h ~ 3h, the acidleach rate of decomposition rangeability of roasting grog is little, but the rangeability of silicon-dioxide productive rate is more obvious, reason may be within the scope of this roasting time, react at the oxide compound such as iron, aluminium of roasting sodium carbonate in early stage more easily and in flyash, along with the carrying out of activation degree, the stable Si oxide of some structure comparison participates in reactivation process.
The impact of 2.4 pickling liquor consumptions
By 5 parts of m
flyash: m
sodium carbonatefor the mixture of 1:1.2 mix after in the retort furnace of 800 degrees Celsius, bake and bank up with earth 2 hours, roasting terminates hydrochloric acid soln 15ml, 20ml, 30ml, 35ml, 40ml of adding 3.0mol/l in backward roasting grog respectively, and its acidleach rate of decomposition and silicon-dioxide productive rate are as shown in Figure 5.
As seen from Figure 5: roasting grog in acidleach process, along with the increase acidleach rate of decomposition productive rate of hydrochloric acid consumption is all in first increasing the variation tendency reduced afterwards.Because of in flyash and sodium carbonate roasting process, the oxide compounds such as the silicon in flyash, aluminium, iron and sodium carbonate react and generate acid-soluble silicate, aluminate or silico-aluminate, when pickling liquor consumption is less than 35ml, acid-leaching reaction is not thorough, in roasting grog, a large amount of acid-soluble silicate or aluminate or silico-aluminate fully do not dissolve, and cause rate of decomposition low so that productive rate is also low; When pickling liquor consumption is 35ml, the acid-soluble compound of roasting grog terminates with primitive reaction, and the productive rate of rate of decomposition and silicon-dioxide is respectively 95.47%, 85.22%; When pickling liquor consumption is more than 35ml, H in acidleach system
+excessive, the formation being conducive to silicic acid gel enters acidleach residue, thus the productive rate of acidleach rate of decomposition and silicon-dioxide is all declined.
The impact of 2.5 concentration of hydrochloric acid
By 5 parts of m
flyash: m
sodium carbonatefor the mixture of 1:1.2 mix after in the retort furnace of 800 degrees Celsius, bake and bank up with earth 2 hours, roasting terminates the hydrochloric acid soln adding 0.105mol different concns 1.5mol/L, 2.0mol/L, 2.5mol/L, 3.0mol/L, 3.5mol/L in backward roasting grog, investigates H
+when mole number is identical, pickling liquor concentration is on the impact of rate of decomposition and productive rate, and experimental result is shown in Fig. 6.
As seen from Figure 6, at H
+when mole number is equal, change the concentration of pickling liquor, rate of decomposition and productive rate present increases the rear variation tendency reduced, but rangeability is very little, when concentration of hydrochloric acid is 2.62mol/L, and the Al in silica gel
2o
3content is more, affects silica product purity and granularity, owing to carrying out secondary pickling to gel products obtained therefrom in experimentation, therefore the concentration of pickling liquor can only affect the granularity of product in judgment experiment process, can ignore to the yield impact of product.In experimentation, for shortening the time of sol-gel and considering liquid measure, the hydrochloric acid of the bigger 3.0mol/L of concentration is selected to test.
The impact of 2.6 sol-gel liquid liquid starting point concentrations is at 800 DEG C, roasting m flyash in the retort furnace of 2h: m sodium carbonate is 6 parts, the mixture of 1:1.2, the hydrochloric acid soln 35mL adding 3mol/L carries out acidleach, filter gained pickling liquor and be diluted with water to 50ml, 100m, 50ml, 200ml, 250ml, 300ml respectively, and be carry out sol-gel after the hydrochloric acid soln adjust ph <0.5 of 1mol/L by concentration, Fig. 7 is shown in the productive rate change of rate of decomposition and silicon-dioxide.
As seen from Figure 7, the variation tendency of rate of decomposition and the variation tendency of productive rate basically identical, and the productive rate of silicon-dioxide and its starting point concentration significantly do not contact, the time series analysis that in Binding experiment, sol-gel process terminates, the starting point concentration of gel-sol liquid is only relevant with the time forming gel, and the larger gel time of concentration is shorter, in experimentation, consider from energy consumption angle, select 3.5X10
-1mOL.L
-1the starting point concentration of (liquor capacity is 50ml) is tested.
The impact of 2.7 Sol-gel transition temperatures is at 800 DEG C, roasting m flyash in the retort furnace of 2h: m sodium carbonate is 6 parts, the mixture of 1:1.2, the hydrochloric acid soln 35mL adding 3mol/L carries out acidleach, filter gained pickling liquor and be diluted with water to 50ml, and be carry out sol-gel after the hydrochloric acid soln adjust ph <0.5 of 1mol/L by concentration, investigate room temperature (~ 25 DEG C), 45 DEG C, 65 DEG C, 75 DEG C, 85 DEG C, 94 DEG C, the productive rate variation relation of rate of decomposition and silicon-dioxide under totally 6 colloidal sol-gelling temps, the results are shown in Figure 8.As seen from Figure 8: in the process of sol-gel, there is no silica product under room temperature, Binding experiment process analysis, pickling liquor room temperature is placed 24h, 36h, within 1 week, is showed no solution sol-gel, and along with the prolongation of storage period, beaker bottom seemingly has microprecipitation to produce; When after raising pickling liquor Sol-gel transition temperatures, along with the raising of temperature, the productive rate of silicon-dioxide does not have noticeable change, but the time shorten that produces of colloidal sol and the time that gel formation terminates to gel also shorten.
For determining that sol-gel and temperature relation are significantly instead of concentration, at 800 DEG C, roasting m flyash in the retort furnace of 2h: m sodium carbonate is that the hydrochloric acid soln 35mL that the mixture of 1:1.2 adds 3mol/L carries out acidleach, filter gained filtrate water and be diluted to 50ml, and be place room temperature (~ 25 DEG C) after the hydrochloric acid soln adjust ph <0.5 of 1mol/L to carry out sol-gel by concentration, As time goes on 12h → 24h → 36h → 72h → 1 week, only observe beaker bottom and have microprecipitation, but do not observe the formation of sol-gel yet.As can be seen here, temperature is comparatively remarkable on the impact of system, and under the condition of 94 DEG C, sol-gel process only needs about 2h, and silicon-dioxide productive rate can reach 85.69%.
3 conclusions
1) flyash is not having to carry out high-temperature activation under auxiliary agent condition, and acidleach rate of decomposition is 24.13%, without silica product.
2) concentration of hydrochloric acid and sol-gel liquid starting point concentration on the productive rate of silicon-dioxide substantially without impact.
3) temperature is the remarkable factor affecting sol-gel.
4) the optimal activation processing condition of flyash are: m flyash: m sodium carbonate is 1:1.2, maturing temperature 800 degrees Celsius, roasting time 2h, Sol-gel transition temperatures 94 DEG C of water-baths, and the productive rate of silicon-dioxide is 85.35%.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. a method for high silicon high iron coal ash for manufacturing prepared silicon dioxide, is characterized in that, the method for described high silicon high iron coal ash for manufacturing prepared silicon dioxide comprises:
By flyash and anhydrous sodium carbonate in the dry 24h of the dry case of the constant-temperature vacuum being placed in 105 DEG C, then take out and be placed in drying basin to be chilled to room temperature stand-by;
Take flyash and anhydrous sodium carbonate, be placed in 30mL porcelain crucible, be positioned over after stirring be warming up to 800 DEG C retort furnace in roasting 2h, after roasting terminates, take out and be placed in drying basin that to be chilled to room temperature stand-by;
Roasting grog is placed in 250mL beaker, after material is fully wetting with water, use glass stick to add hydrochloric acid soln while stirring, and proceed in ultrasonic cleaning machine ultrasonic;
After ultrasonic end, filter above-mentioned acidleach product, and wash filter cake with hydrochloric acid, collection filtrate is stand-by; Use tap water filter cake again until neutrality, after filter residue being placed in the constant-temperature vacuum dry case inner drying 24h of 105 DEG C, being chilled to room temperature and weighing;
Gained filtrate is proceeded in 250mL beaker, measure pH, put into thermostat water bath and carry out sol-gel, measuring pH<0.5 when there is colloidal sol, after collosol and gel terminates, measuring pH<0.5;
After sol-gel terminates, under the power of 240W, carry out ultrasonic acidleach 5min with the hydrochloric acid soln of the 1mol/L of 20mL to above-mentioned Silica hydrogel, carry out centrifugation after acidleach terminates, this step repeats 3 times;
Under the wet gel of gained being put into the power of 240W, with the ultrasonic 5min washing of the tap water of 20mL to neutrality, filter residue is placed in the dry case of constant-temperature vacuum dry, and weighs.
2. the method for high silicon high iron coal ash for manufacturing prepared silicon dioxide as claimed in claim 1, is characterized in that, flyash and anhydrous sodium carbonate need to dry, and flyash and anhydrous sodium carbonate mass ratio are 1:1.2; Glass stick is used to add the hydrochloric acid soln 35mL of 3mol/L while stirring.
3. the method for high silicon high iron coal ash for manufacturing prepared silicon dioxide as claimed in claim 1, is characterized in that, proceed to ultrasonic 1min in the ultrasonic cleaning machine of 240W.
4. the method for high silicon high iron coal ash for manufacturing prepared silicon dioxide as claimed in claim 1, is characterized in that, wash with the hydrochloric acid 10mL of 3mol/L to filter cake.
5. the method for high silicon high iron coal ash for manufacturing prepared silicon dioxide as claimed in claim 1, it is characterized in that, filter residue is placed in the dry 24h of the dry case of constant-temperature vacuum of 105 DEG C.
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| CN110963496A (en) * | 2019-12-18 | 2020-04-07 | 昆明理工大学 | Method for synthesizing ordered mesoporous silicon oxide by using fly ash |
| CN110975833A (en) * | 2019-12-18 | 2020-04-10 | 昆明理工大学 | Preparation method and application of silicon dioxide/cellulose composite porous material |
| CN112340744A (en) * | 2020-11-17 | 2021-02-09 | 临沂昊泉硅业科技有限公司 | Preparation method of silicon-aluminum composite aerogel |
| CN113548683A (en) * | 2021-07-22 | 2021-10-26 | 安徽大学绿色产业创新研究院 | Method for preparing magnesium-series and silicon-series materials by using serpentine without waste |
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| CN110040736A (en) * | 2019-05-15 | 2019-07-23 | 吉林唯圣能源科技开发有限公司 | A kind of preparation method of silica |
| CN110963496A (en) * | 2019-12-18 | 2020-04-07 | 昆明理工大学 | Method for synthesizing ordered mesoporous silicon oxide by using fly ash |
| CN110975833A (en) * | 2019-12-18 | 2020-04-10 | 昆明理工大学 | Preparation method and application of silicon dioxide/cellulose composite porous material |
| CN112340744A (en) * | 2020-11-17 | 2021-02-09 | 临沂昊泉硅业科技有限公司 | Preparation method of silicon-aluminum composite aerogel |
| CN113548683A (en) * | 2021-07-22 | 2021-10-26 | 安徽大学绿色产业创新研究院 | Method for preparing magnesium-series and silicon-series materials by using serpentine without waste |
| CN114735732A (en) * | 2022-05-06 | 2022-07-12 | 内蒙古工业大学 | Method for preparing alumina and silicon dioxide by using high-alumina fly ash |
| CN114735732B (en) * | 2022-05-06 | 2023-10-27 | 内蒙古工业大学 | Method for preparing alumina and silicon dioxide from high-alumina fly ash |
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