CN108190926A - A kind of preparation method of desiliconization flyash - Google Patents
A kind of preparation method of desiliconization flyash Download PDFInfo
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Abstract
The present invention provides a kind of preparation method of desiliconization flyash, and aluminous fly-ash with solid base is mixed, mixture is refined by the preparation method, obtains refinement activating fly ash；Desiliconization processing is carried out using the refinement activating fly ash that aqueous slkali or water obtain, separation of solid and liquid obtains desiliconization flyash.The preparation method silica removal efficiency is high, side reaction generation is less, and process is simple, easy to operate, obtained desiliconization flyash has the characteristics that alumina silica ratio is high, sodium content is relatively low, production cost is low, do not generate secondary solid and liquid pollutant, realize that aluminous fly-ash minimizing, recycling efficiently utilize, economy and obvious environment benefit.
Description
Technical field
The invention belongs to field of inorganic chemical engineering, are related to a kind of preparation method of desiliconization flyash.
Background technology
Aluminous fly-ash is that the solid that generates gives up after middle of Inner Mongolia, the power generation of northern Shanxi characteristic high alumina coal burning
Gurry.About 30,000,000 tons of year yield at present, but comprehensive utilization ratio causes air, water resource, soil resource etc. less than 20%
Serious pollution.On the other hand, aluminous fly-ash potential resources is big, Al2O3 contents>40%, alumina silica ratio is about 1.2 left sides
The right side mainly exists in the form of mullite phase and amorphous phase aluminosilicate, is prepared available for Al-Si Refractory Materials and aluminium oxide carries
Industry is taken, it is exhausted that the high-quality bauxite in China can be alleviated.
Aluminous fly-ash prepares raising flyash alumina silica ratio in Al-Si composites and the research for extracting aluminum oxide technology
Its key application.The method for improving raw material alumina silica ratio at present focuses primarily upon removing amorphous silicon di-oxide, CN 104043639
A discloses a kind of preparation method of desiliconization flyash, using aluminous fly-ash as raw material, by high-temperature activation, pre-desiliconizing, secondary de-
The desiliconization powder that alumina silica ratio is 2.3-2.5 is prepared in the processes such as silicon, washing drying；Our unit is proposed based on early-stage study basis
Pre-desiliconizing, diluted acid activation, deep desilication technical thought, CN 102583411 A and CN 102583409 A discloses one kind
Using flyash production mullite method, using aluminous fly-ash as raw material, by pretreatment, pre-desiliconizing, acid activation, it is secondary take off
The processes such as silicon, sintering obtain high trade mark mullite；104671811 A of CN disclose a kind of utilize at two sections of acid of aluminous fly-ash
The method that reason prepares mullite, with the non-raw material of aluminous fly-ash, by pre-desiliconizing, hypo acid processing, the processing of two hypo acids, washing,
The processes such as roasting obtain high trade mark mullite；106220190 A of CN are disclosed a kind of prepares mullite using aluminous fly-ash
Method is activated, the method that desiliconization prepares mullite by mechanical-chemical, can obtain the product that alumina silica ratio is more than 2.55.It is above-mentioned
The thinking that research unit proposes realizes the efficient removal of amorphous aerosil, and solid phase alumina silica ratio can have 1 or so raising to 2.2
More than, alumina content can reach more than 60%, prepare Al-Si composites for aluminous fly-ash and extraction aluminium oxide provides
Key technology.
Invention content
For problems of the prior art, the present invention provides a kind of preparation method of desiliconization flyash, the preparation
Method can greatly improve the silica alumina ratio in flyash, realize the deep removal of silica, be prepared for high trade mark aluminium silicon materials
New technology is provided with alumina extraction process.
In order to achieve the above objectives, the present invention uses following technical scheme：
The present invention provides a kind of preparation method of desiliconization flyash, the described method comprises the following steps：
(1) aluminous fly-ash with solid base is mixed, mixture is refined, obtain refinement activating fly ash；
(2) the refinement activating fly ash progress desiliconization processing obtained using aqueous slkali or water to step (1), separation of solid and liquid,
Obtain desiliconization flyash.
By aluminous fly-ash and solid caustic soda mixing and ball milling, the heat generated using mechanical milling process promotes solid caustic soda medium to enter aluminium silicon
In hydrochlorate ore deposit phase, stable vitreous structure is destroyed, generates lattice defect, reduces the activation energy of its reaction, so as to reach activation
Purpose.It is further handled by diluted alkaline or aqueous solution, alkaline media can be excited to decompose the effect of silica, so as to fulfill dioxy
The efficient removal of SiClx.
Wherein, the aluminous fly-ash that the present invention uses is not less than 43% flyash for alumina content.
As currently preferred technical solution, the mass ratio of step (1) aluminous fly-ash and solid base is (0.5
~2.0):1, such as 0.5:1、0.6:1、0.7:1、0.8:1、0.9:1、1.0:1、1.1:1、1.2:1、1.3:1、1.4:1、1.5:1、
1.6:1、1.7:1、1.8:1、1.9:1 or 2:1 etc., it is not limited to cited numerical value, other are not arranged in the numerical value orientation
The numerical value of act is equally applicable.
As currently preferred technical solution, step (1) described solid base includes sodium hydroxide and/or potassium hydroxide.
As currently preferred technical solution, the method for step (1) described refinement is appointing in crushing, grinding or ball milling
It anticipates a kind of or at least two combinations, preferably ball milling.
As currently preferred technical solution, the mass ratio of mixture and abrading-ball is (1.0~2.5) in the ball milling:
1, such as 1.0:1、1.1:1、1.2:1、1.3:1、1.4:1、1.5:1、1.6:1、1.7:1、1.8:1、1.9:1、2.0:1、2.1:1、
2.2:1、2.3:1、2.4:1 or 2.5:1 etc., it is not limited to cited numerical value, other are unrequited in the numerical value orientation
Numerical value is equally applicable.
Preferably, the rotating speed of the ball milling be 150~350r/min, as 150r/min, 200r/min, 250r/min,
300r/min or 350r/min etc., it is not limited to cited numerical value, other unrequited numerical value are same in the numerical value orientation
Sample is applicable in.
Preferably, the time of the ball milling be 60~180min, as 60min, 70min, 80min, 90min, 100min,
110min, 120min, 130min, 140min, 150min, 160min, 170min or 180min etc., it is not limited to cited
Numerical value, other unrequited numerical value are equally applicable in the numerical value orientation.
As currently preferred technical solution, step (2) described aqueous slkali is sodium hydroxide and/or the water of potassium hydroxide
Solution；
Preferably, a concentration of 0~6.5mol/L of step (2) described aqueous slkali, not including 0, as 0.1mol/L,
0.2mol/L、0.5mol/L、1.0mol/L、1.5mol/L、2.0mol/L、2.5mol/L、3.0mol/L、3.5mol/L、
4.0mol/L, 4.5mol/L, 5.0mol/L, 5.5mol/L, 6.0mol/L or 6.5mol/L etc., it is not limited to cited
Numerical value, other unrequited numerical value are equally applicable in the numerical value orientation.
As currently preferred technical solution, step (2) aqueous slkali or water are consolidated with refining the liquid of activating fly ash
Than for (5~10):1, such as 5:1、6:1、7:1、8:1、9:1 or 10:1 etc., it is not limited to cited numerical value, the numerical value side
Other unrequited numerical value are equally applicable in position.
As currently preferred technical solution, the temperature of step (2) the desiliconization processing is 85~95 DEG C, such as 85 DEG C,
86 DEG C, 87 DEG C, 88 DEG C, 89 DEG C, 90 DEG C, 91 DEG C, 92 DEG C, 93 DEG C, 94 DEG C or 95 DEG C etc., it is not limited to cited number
It is worth, other unrequited numerical value are equally applicable in the numerical value orientation.
Preferably, the time of desiliconization processing is 50~120min, as 50min, 60min, 70min, 80min,
90min, 100min, 110min or 120min etc., it is not limited to cited numerical value, other are unrequited in the numerical value orientation
Numerical value it is equally applicable.
As currently preferred technical solution, the desiliconization flyash obtained to step (2) is washed, separation of solid and liquid and
It is dry.
Preferably, the temperature of the slurry be 60~90 DEG C, such as 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C or
90 DEG C etc., it is not limited to cited numerical value, other unrequited numerical value are equally applicable in the numerical value orientation.
Preferably, the liquid-solid ratio of the washing is (1~3):1, such as 1:1、1.2:1、1.5:1、1.8:1、2:1、2.2:1、
2.5:1、2.8:1 or 3:1 etc., it is not limited to cited numerical value, other unrequited numerical value are similary in the numerical value orientation
It is applicable in.
As currently preferred technical solution, the described method comprises the following steps：
(1) by aluminous fly-ash and solid base according to mass ratio (0.5~2):1 mixing, mixture ball milling is refined, and is mixed
The mass ratio of material and abrading-ball is (1.0~2.5):1, the rotating speed of ball milling is 150~350r/min, time of ball milling for 50~
120min obtains refinement activating fly ash；
(2) using the aqueous slkali of 0~6.5mol/L (not including 0) or water according to liquid-solid ratio (5~10):1 pair of step (1) obtains
The refinement activating fly ash arrived carries out desiliconization at 85~95 DEG C and handles 50~120min, and separation of solid and liquid obtains desiliconization flyash,
And the desiliconization flyash is washed, separation of solid and liquid and drying.
Compared with prior art, the present invention at least has the advantages that：
(1) present invention provides a kind of preparation method of desiliconization flyash, and the preparation method realizes the depth of silica
Removing, can obtain the product that alumina silica ratio is more than 2.55, and simultaneous oxidation aluminium content is high trade mark aluminium silicon materials system up to more than 61%
Standby and alumina extraction industry provides technical support, and it is exhausted to alleviate the high-quality bauxite resource in China；
(2) present invention provides a kind of preparation method of desiliconization flyash, and the preparation method is handled only with a step diluted alkaline
The deep removal of silica can be realized, operating process is simple, and operating flexibility is big, and desiliconization lye is recycled after causticization to be made
With non-secondary pollution object generates, and realizes economy and environmental benefit joint development.
Description of the drawings
Fig. 1 is a kind of flow diagram of desiliconization coal ash for manufacturing Preparation Method provided by the invention.
Specific embodiment
Technical solution to further illustrate the present invention below with reference to the accompanying drawings and specific embodiments.
For the present invention is better described, technical scheme of the present invention is easy to understand, of the invention is typical but non-limiting
Embodiment is as follows：
Embodiment 1
The present embodiment provides a kind of preparation methods of desiliconization flyash, the described method comprises the following steps：
(1) by aluminous fly-ash and sodium hydroxide according to mass ratio 2:1 mixing, mixture ball milling is refined, mixture with
The mass ratio of abrading-ball is 1:1, the rotating speed of ball milling is 350r/min, and the time of ball milling is 60min, obtains refinement activating fly ash；
(2) using the sodium hydrate aqueous solution of 6.5mol/L according to liquid-solid ratio 8:The refinement activation powder that 1 pair of step (1) obtains
Coal ash carries out desiliconization processing 75min at 95 DEG C, and separation of solid and liquid obtains desiliconization flyash, and the desiliconization flyash is carried out
Washing, separation of solid and liquid and drying.
Embodiment 2
The present embodiment provides a kind of preparation methods of desiliconization flyash, the described method comprises the following steps：
(1) by aluminous fly-ash and sodium hydroxide according to mass ratio 0.5:1 mixing, mixture ball milling is refined, mixture
Mass ratio with abrading-ball is 1:1, the rotating speed of ball milling is 200r/min, and the time of ball milling is 75min, obtains refinement activation fine coal
Ash；
(2) using the sodium hydrate aqueous solution of 2.5mol/L according to liquid-solid ratio 5:The refinement activation powder that 1 pair of step (1) obtains
Coal ash carries out desiliconization processing 90min at 90 DEG C, and separation of solid and liquid obtains desiliconization flyash, and the desiliconization flyash is carried out
Washing, separation of solid and liquid and drying.
Embodiment 3
The present embodiment provides a kind of preparation methods of desiliconization flyash, the described method comprises the following steps：
(1) by aluminous fly-ash and sodium hydroxide according to mass ratio 1:1 mixing, mixture ball milling is refined, mixture with
The mass ratio of abrading-ball is 1:1, the rotating speed of ball milling is 200r/min, and the time of ball milling is 75min, obtains refinement activating fly ash；
(2) using the sodium hydrate aqueous solution of 5mol/L according to liquid-solid ratio 6:The refinement activation fine coal that 1 pair of step (1) obtains
Ash carries out desiliconization processing 80min at 92 DEG C, and separation of solid and liquid obtains desiliconization flyash, and the desiliconization flyash is washed
It washs, separation of solid and liquid and drying.
Embodiment 4
The present embodiment provides a kind of preparation methods of desiliconization flyash, the described method comprises the following steps：
(1) by aluminous fly-ash and sodium hydroxide according to mass ratio 4:3 mixing, mixture ball milling is refined, mixture with
The mass ratio of abrading-ball is 1:1.5, the rotating speed of ball milling is 300r/min, and the time of ball milling is 120min, obtains refinement activation fine coal
Ash；
(2) using the sodium hydrate aqueous solution of 4mol/L according to liquid-solid ratio 7:The refinement activation fine coal that 1 pair of step (1) obtains
Ash carries out desiliconization processing 80min at 95 DEG C, and separation of solid and liquid obtains desiliconization flyash, and the desiliconization flyash is washed
It washs, separation of solid and liquid and drying.
Embodiment 5
The present embodiment provides a kind of preparation methods of desiliconization flyash, the described method comprises the following steps：
(1) by aluminous fly-ash and sodium hydroxide according to mass ratio 5:3 mixing, mixture ball milling is refined, mixture with
The mass ratio of abrading-ball is 1:2, the rotating speed of ball milling is 250r/min, and the time of ball milling is 120min, obtains refinement activating fly ash；
(2) using the sodium hydrate aqueous solution of 4.5mol/L according to liquid-solid ratio 7.5:The refinement activation that 1 pair of step (1) obtains
Flyash carries out desiliconization processing 100min at 90 DEG C, and separation of solid and liquid obtains desiliconization flyash, and to the desiliconization flyash into
Row washing, separation of solid and liquid and drying.
Embodiment 6
The present embodiment provides a kind of preparation methods of desiliconization flyash, the described method comprises the following steps：
(1) by aluminous fly-ash and sodium hydroxide according to mass ratio 3:4 mixing, mixture ball milling is refined, mixture with
The mass ratio of abrading-ball is 1:2.5, the rotating speed of ball milling is 150r/min, and the time of ball milling is 180min, obtains refinement activation fine coal
Ash；
(2) using the sodium hydrate aqueous solution of 4.5mol/L according to liquid-solid ratio 6:The refinement activation powder that 1 pair of step (1) obtains
Coal ash carries out desiliconization processing 110min at 90 DEG C, and separation of solid and liquid obtains desiliconization flyash, and the desiliconization flyash is carried out
Washing, separation of solid and liquid and drying.
Embodiment 7
The present embodiment provides a kind of preparation methods of desiliconization flyash, the described method comprises the following steps：
(1) by aluminous fly-ash and potassium hydroxide according to mass ratio 3:5 mixing, mixture ball milling is refined, mixture with
The mass ratio of abrading-ball is 1:1, the rotating speed of ball milling is 300r/min, and the time of ball milling is 100min, obtains refinement activating fly ash；
(2) using the potassium hydroxide aqueous solution of 3.0mol/L according to liquid-solid ratio 5.5:The refinement activation that 1 pair of step (1) obtains
Flyash carries out desiliconization processing 80min at 95 DEG C, and separation of solid and liquid obtains desiliconization flyash, and to the desiliconization flyash into
Row washing, separation of solid and liquid and drying.
Embodiment 8
(1) by aluminous fly-ash and sodium hydroxide according to mass ratio 1:2 mixing, mixture ball milling is refined, mixture with
The mass ratio of abrading-ball is 1:1, the rotating speed of ball milling is 300r/min, and the time of ball milling is 100min, obtains refinement activating fly ash；
(2) using water according to liquid-solid ratio 7:The refinement activating fly ash that 1 pair of step (1) obtains is carried out at 95 DEG C at desiliconization
90min is managed, separation of solid and liquid obtains desiliconization flyash, and the desiliconization flyash is washed, separation of solid and liquid and drying.
Comparative example 1
In this comparative example, other than the ball milling relevant operation without step (1), other conditions are same as Example 3.
Comparative example 2
In this comparative example, in addition to the mass ratio of step (1) aluminous fly-ash and solid base is 1:Outside 5, other conditions
It is same as Example 3.
Comparative example 3
In this comparative example, in addition to the mass ratio of step (1) aluminous fly-ash and solid base is 5:Outside 1, other conditions
It is same as Example 3.
Alumina-silica amount ratio, alumina content in the desiliconization flyash that embodiment 1-8 and comparative example 1-3 are prepared
It is tested with sodium content, the results are shown in Table 1.
Table 1
| Project | Alumina silica ratio | Alumina content/% | Sodium/potassium content/% |
| Embodiment 1 | 2.58 | 62.03 | 1.25 |
| Embodiment 2 | 2.62 | 63.28 | 1.43 |
| Embodiment 3 | 2.54 | 61.82 | 1.87 |
| Embodiment 4 | 2.57 | 61.97 | 1.76 |
| Embodiment 5 | 2.60 | 62.66 | 1.37 |
| Embodiment 6 | 2.54 | 61.47 | 1.72 |
| Embodiment 7 | 2.59 | 62.63 | 1.46 |
| Embodiment 8 | 2.52 | 61.38 | 1.94 |
| Comparative example 1 | 1.82 | 53.32 | 1.32 |
| Comparative example 2 | 2.64 | 64.03 | 2.37 |
| Comparative example 3 | 2.26 | 58.72 | 1.74 |
As it can be seen from table 1 the silica alumina ratio of desiliconization flyash that embodiment 1-8 is prepared is more than 2.55, simultaneous oxidation
Aluminium content is up to more than 61%, and comparative example 1 does not activate aluminous fly-ash raw material using ball milling, the desiliconization flyash being prepared
Silica alumina ratio is 1.82, alumina content 53.32%, and the mass ratio of aluminous fly-ash and solid base is 1 in comparative example 2:5, though
Right alumina silica ratio and alumina content are higher, but sodium content rises to 2.37, affects the property of desiliconization flyash, comparative example 3
The mass ratio of middle aluminous fly-ash and solid base is 5:1, the obtained silica alumina ratio of desiliconization flyash is 2.26, and alumina content is
58.72%.The property of desiliconization flyash that visual contrast example 1-3 is prepared is worse than embodiment 1-8.
Applicant states that the present invention illustrates the detailed construction feature of the present invention by above-described embodiment, but the present invention is simultaneously
Above-mentioned detailed construction feature is not limited to, that is, does not mean that the present invention has to rely on above-mentioned detailed construction feature and could implement.Institute
Belong to those skilled in the art it will be clearly understood that any improvement in the present invention, to the equivalence replacement of component selected by the present invention
And the increase of accessory, selection of concrete mode etc., it all falls within protection scope of the present invention and the open scope.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail, within the scope of the technical concept of the present invention, a variety of simple variants can be carried out to technical scheme of the present invention, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (10)
1. a kind of preparation method of desiliconization flyash, which is characterized in that the described method comprises the following steps：
(1) aluminous fly-ash with solid base is mixed, mixture is refined, obtain refinement activating fly ash；
(2) desiliconization processing is carried out to the refinement activating fly ash that step (1) obtains using aqueous slkali or water, separation of solid and liquid obtains
Desiliconization flyash.
2. preparation method according to claim 1, which is characterized in that step (1) aluminous fly-ash and solid base
Mass ratio is (0.5~2):1.
3. preparation method according to claim 1 or 2, which is characterized in that step (1) described solid base includes sodium hydroxide
And/or potassium hydroxide.
4. according to claim 1-3 any one of them preparation methods, which is characterized in that the method for step (1) described refinement is
Crush, in grinding or ball milling any one or at least two combination, preferably ball milling.
5. preparation method according to claim 4, which is characterized in that the mass ratio of mixture and abrading-ball is in the ball milling
(1.0~2.5):1；
Preferably, the rotating speed of the ball milling is 150~350r/min；
Preferably, the time of the ball milling is 60~180min.
6. according to Claims 1 to 5 any one of them preparation method, which is characterized in that step (2) described aqueous slkali is hydrogen-oxygen
Change the aqueous solution of sodium and/or potassium hydroxide；
Preferably, a concentration of 0~6.5mol/L of step (2) described aqueous slkali, not including 0.
7. according to claim 1-6 any one of them preparation methods, which is characterized in that step (2) aqueous slkali or water with
The liquid-solid ratio for refining activating fly ash is (5~10):1.
8. according to claim 1-7 any one of them preparation methods, which is characterized in that the temperature of step (2) the desiliconization processing
Spend is 85~95 DEG C；
Preferably, the time of the desiliconization processing is 50~120min.
9. according to claim 1-8 any one of them preparation methods, which is characterized in that the desiliconization fine coal obtained to step (2)
Ash is washed, separation of solid and liquid and drying；
Preferably, the temperature of the slurry is 60~90 DEG C；
Preferably, the liquid-solid ratio of the washing is (1~3):1.
10. according to claim 1-9 any one of them preparation methods, which is characterized in that the described method comprises the following steps：
(1) by aluminous fly-ash and solid base according to mass ratio (0.5~2):1 mixing, mixture ball milling is refined, mixture with
The mass ratio of abrading-ball is (1.0~2.5):1, the rotating speed of ball milling is 150~350r/min, and the time of ball milling is 50~120min,
Obtain refinement activating fly ash；
(2) using the aqueous slkali of 0~6.5mol/L (not including 0) or water according to liquid-solid ratio (5~10):What 1 pair of step (1) obtained
Refinement activating fly ash carries out desiliconization at 85~95 DEG C and handles 50~120min, and separation of solid and liquid obtains desiliconization flyash, and right
The desiliconization flyash is washed, separation of solid and liquid and drying.
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| CN110734083A (en) * | 2019-11-20 | 2020-01-31 | 内蒙古日盛可再生资源有限公司 | Desiliconization method of high-alumina fly ash |
| CN110857250A (en) * | 2018-08-22 | 2020-03-03 | 中国科学院过程工程研究所 | Method for preparing ceramic tile by using fly ash as raw material |
| CN114772959A (en) * | 2022-04-29 | 2022-07-22 | 北京科技大学 | Preparation method of sodium aluminosilicate sol, product and application thereof |
| CN115703637A (en) * | 2021-08-10 | 2023-02-17 | 中国石油化工股份有限公司 | Porous silicon oxide and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110857250A (en) * | 2018-08-22 | 2020-03-03 | 中国科学院过程工程研究所 | Method for preparing ceramic tile by using fly ash as raw material |
| CN110734083A (en) * | 2019-11-20 | 2020-01-31 | 内蒙古日盛可再生资源有限公司 | Desiliconization method of high-alumina fly ash |
| CN115703637A (en) * | 2021-08-10 | 2023-02-17 | 中国石油化工股份有限公司 | Porous silicon oxide and preparation method and application thereof |
| CN114772959A (en) * | 2022-04-29 | 2022-07-22 | 北京科技大学 | Preparation method of sodium aluminosilicate sol, product and application thereof |
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