CN108455637A - A kind of method of pre-desiliconizing with high alumina fly ash - Google Patents

A kind of method of pre-desiliconizing with high alumina fly ash Download PDF

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CN108455637A
CN108455637A CN201810074364.2A CN201810074364A CN108455637A CN 108455637 A CN108455637 A CN 108455637A CN 201810074364 A CN201810074364 A CN 201810074364A CN 108455637 A CN108455637 A CN 108455637A
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ash
fly
desiliconizing
acidizer
activation
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公彦兵
孙俊民
洪景南
许学斌
杨会宾
王娜
李运改
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High Aluminum Coal Resources Development and Utilization R&D Center of Datang International Power Generation Co Ltd
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High Aluminum Coal Resources Development and Utilization R&D Center of Datang International Power Generation Co Ltd
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Priority to CN201810074364.2A priority Critical patent/CN108455637A/en
Publication of CN108455637A publication Critical patent/CN108455637A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/04Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
    • C01F7/06Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom by treating aluminous minerals or waste-like raw materials with alkali hydroxide, e.g. leaching of bauxite according to the Bayer process
    • C01F7/0693Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom by treating aluminous minerals or waste-like raw materials with alkali hydroxide, e.g. leaching of bauxite according to the Bayer process from waste-like raw materials, e.g. fly ash or Bayer calcination dust

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The present invention provides a kind of method of pre-desiliconizing with high alumina fly ash, includes the following steps:1) activation process is carried out to the aluminous fly-ash, obtains activation aluminous fly-ash;2) the activation aluminous fly-ash is mixed with sodium hydroxide solution and carries out pre-desiliconizing processing, filtering obtains desiliconization aluminous fly-ash;Wherein, the alumina silica ratio of the desiliconization aluminous fly-ash is 2.5 3.8, and the mass fraction of the sodium oxide molybdena in the desiliconization aluminous fly-ash is 0.5 3.0%.This method can effectively improve the desilication efficiency to aluminous fly-ash, be obviously improved the alumina silica ratio of flyash after desiliconization.

Description

A kind of method of pre-desiliconizing with high alumina fly ash
Technical field
The present invention relates to a kind of methods of pre-desiliconizing with high alumina fly ash, belong to flyash pre-desiliconizing processing technology field.
Background technology
Since China's bauxite resource is relatively deficient, 7% or so of the worlds alumina ore reserves Jin Zhan gross reserves, and be mostly hardly possible The diaspore ore of processing, resource problem have become the main bottleneck of China's sustainable development of alumina industry.And China The aluminous fly-ash rich reserves generated after the coal power generation in the area such as Middle-west Inner Mongolia and North of Shanxi, the only quasi- Ge Er in Inner Mongol The potential aluminous fly-ash resource reserves in coalfield just up to 15,000,000,000 tons, be equivalent to 8 times of the current bauxite reserves in China with On, and alumina content can reach 40%-50% in the aluminous fly-ash of part.
In recent years, major universities and colleges of China and R&D institution had actively developed aluminous fly-ash extraction aluminium oxide new process and had ground Study carefully, major processes are:Pre-desiliconizing-soda lime sintering process, a step acid extracting, ammonium sulfate sintering-Bayer process, lime stone are burnt Knot-low temperature Bayer process etc..In these methods, the alumina silica ratio of flyash is effectively improved by pre-desiliconizing means, on the one hand not The grade of flyash is improved only, and then improves the economy of alumina producing system, is on the other hand even more that silicon resource is efficient Cooperate with the requisite measure utilized.
Then current technology can only improve flyash alumina silica ratio to 2.0 or so, and desilication efficiency is relatively low, cause follow-up The problems such as internal circulating load of alumina producing is big, the quantity of slag is big, lime consumption is high, therefore how a kind of new pre-desiliconizing production work is provided Skill, the alumina silica ratio for further increasing desiliconization flyash are current urgent problems to be solved.
Invention content
The present invention provides a kind of method of pre-desiliconizing with high alumina fly ash, can effectively improve the desiliconization effect to aluminous fly-ash Rate is obviously improved the alumina silica ratio of flyash after desiliconization, and the recovery rate to improve aluminium oxide in aluminous fly-ash is laid a good foundation.
The present invention provides a kind of method of pre-desiliconizing with high alumina fly ash, includes the following steps:
1) activation process is carried out to the aluminous fly-ash, obtains activation aluminous fly-ash;
2) the activation aluminous fly-ash is mixed with sodium hydroxide solution and carries out pre-desiliconizing processing, filtering obtains desiliconization Aluminous fly-ash;
Wherein, the alumina silica ratio of the desiliconization aluminous fly-ash is 2.5-3.8, the sodium oxide molybdena in the desiliconization aluminous fly-ash Mass fraction be 0.5-3.0%.
The method of pre-desiliconizing with high alumina fly ash as described above, wherein the activation process includes the following steps:
A. the aluminous fly-ash is mixed with acidizer solution, obtains mixture;
B. physically activated processing is carried out to the mixture using ball mill or disc mill, filtering obtains the activation Aluminous fly-ash;
Wherein, the acidizer solution is the aqueous solution of acidizer, and the acidizer is selected from sulfuric acid, hydrochloric acid, nitre It is one or more in acid and phosphoric acid;In the acidizer solution, the mass fraction of the acidizer is 3-30%.
The method of pre-desiliconizing with high alumina fly ash as described above, wherein the activation process includes the following steps:
C. physically activated processing is carried out to the aluminous fly-ash using ball mill or disc mill, it is high obtains intermediate activation Aluminium powder coal ash;
D. the intermediate aluminous fly-ash that activates is mixed into progress chemical activation processing with acidizer solution, filtering obtains To the activation aluminous fly-ash;
Wherein, the acidizer solution is the aqueous solution of acidizer, and the acidizer is selected from sulfuric acid, hydrochloric acid, nitre It is one or more in acid and phosphoric acid;In the acidizer solution, the mass fraction of the acidizer is 3-30%.
The method of pre-desiliconizing with high alumina fly ash as described above, wherein further include to the mixture before step B It is heated to 50-100 DEG C.
The method of pre-desiliconizing with high alumina fly ash as described above, wherein in the mixture, the acidizer solution with The mass ratio of the aluminous fly-ash is 2~10.
The method of pre-desiliconizing with high alumina fly ash as described above, wherein the time of the physically activated processing is 0.5min ~60min.
The method of pre-desiliconizing with high alumina fly ash as described above, wherein the acidizer solution and intermediate activation high alumina The mass ratio of flyash is 2~10.
The method of pre-desiliconizing with high alumina fly ash as described above, wherein control the treatment temperature of the chemical activation processing It it is 50 DEG C -100 DEG C, the processing time for controlling the chemical activation processing is 30min~120min.
The method of pre-desiliconizing with high alumina fly ash as described above, wherein the mass fraction of the sodium hydroxide solution is 5% ~20%, the mass ratio of the sodium hydroxide solution and the activation aluminous fly-ash is 2~10.
The method of pre-desiliconizing with high alumina fly ash as described above, wherein controlling the treatment temperature that the pre-desiliconizing is handled is 50 DEG C -120 DEG C, the processing time for controlling the pre-desiliconizing processing is 0.5-2h.
The present invention is using aluminous fly-ash as raw material, and by carrying out a series of processing to raw material, it is 2.5-3.8 to obtain alumina silica ratio Desiliconization flyash, meanwhile, when the sodium oxide molybdena in desiliconization aluminous fly-ash mass fraction be 0.5-3.0%, not only facilitate The extraction work of desiliconization aluminous fly-ash subsequent oxidation aluminium, additionally it is possible to ensure repetition of the sodium hydroxide mother liquor in desiliconization pretreatment It utilizes.Wherein, aluminous fly-ash of the invention refers in aluminous fly-ash, and the mass content of aluminium oxide is not less than 40%.
The main component of aluminous fly-ash is mullite and amorphous silicon di-oxide, and the basic ideas of pre-desiliconizing processing are exactly It is reacted with amorphous silicon di-oxide by lye and generates sodium silicate solution, and mullite does not react with lye.However according to grinding Study carefully display, by the aluminous fly-ash that high-temp combustion is formed, part mullite crystal and amorphous silicon di-oxide are mutually wrapped up, made Inert amorphous silicon di-oxide is difficult to react with lye in terms of at there are problems that physics and chemistry two, to cause Pre-desilicification process desilication efficiency is low, desiliconization alumina silica ratio is not high problem.The technical thought of the present invention is based on this point, right Aluminous fly-ash carries out activation process, to improve the activity of amorphous silicon di-oxide in flyash, promotes amorphous state titanium dioxide Silicon reacts with lye, regulates and controls the dynamics of desilication reaction, and then improve pre-desiliconizing efficiency, improves the aluminium silicon of desiliconization flyash Than.
Compared with prior art, implementation of the invention has at least the following advantages:
1) the method desilication efficiency of pre-desiliconizing with high alumina fly ash of the invention is high, at the activation to aluminous fly-ash Reason improves the activity of silica in flyash, regulates and controls the dynamics of desilication reaction, by the alumina silica ratio of desiliconization flyash from present 2.0 or so improve to 2.5-3.8, to reduce the mass flow in aluminum oxide production process and the production quantity of slag;
2) compared with conventional desilication process, the desiliconization coal ash alkali content that the present invention obtains is reduced to 0.5- by 3.0~6.0% 3.0%, the loss of alkali is greatly reduced, system soda balance is maintained;
3) the method implementation condition of pre-desiliconizing with high alumina fly ash of the invention is mild, is easy to and existing pre-desiliconizing technique knot It closes, energy consumption is relatively low;
4) equipment that the method for pre-desiliconizing with high alumina fly ash of the invention uses has conventional equipment, is not required to additionally develop non- Marking device reduces equipment investment cost.
Description of the drawings
Fig. 1 is the flow chart of the embodiment of the method for pre-desiliconizing with high alumina fly ash of the present invention;
Fig. 2 is the flow chart of another embodiment of method of pre-desiliconizing with high alumina fly ash of the present invention;
Fig. 3 is the flow chart of the method another embodiment of pre-desiliconizing with high alumina fly ash of the present invention.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the attached drawing of the present invention, to this hair Technical solution in bright embodiment is clearly and completely described, it is clear that described embodiment is that a part of the invention is implemented Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creativeness The every other embodiment obtained under the premise of labour, shall fall within the protection scope of the present invention.
Fig. 1 is the flow chart of the embodiment of the method for pre-desiliconizing with high alumina fly ash of the present invention, as shown in Figure 1, the present embodiment The method of pre-desiliconizing with high alumina fly ash includes the following steps:
S101:Activation process is carried out to aluminous fly-ash, obtains activation aluminous fly-ash;
Above-mentioned activation process is vital processing step in the method for the present invention, and specifically, which is to be directed to Amorphous silicon di-oxide in aluminous fly-ash is activated, and avoids it by the mullite package in aluminous fly-ash and follow-up It can not react with lye and generate sodium silicate solution.
In other words, after aluminous fly-ash is carried out activation process, when aluminous fly-ash with lye when subsequently mixing, Amorphous silicon di-oxide in aluminous fly-ash will be positive react with lye and generate sodium silicate solution, to by high alumina Amorphous silicon di-oxide in flyash is converted into silicate ion and is dissolved in solution, and then improves the pre- of aluminous fly-ash Desilication efficiency reduces the silicone content in aluminous fly-ash, so as to make alumina silica ratio increase.
The method of the unlimited fixture body activation process of the present invention, if can reduce amorphous silicon di-oxide physical inertness and Chemical inertness promotees positive to react with lye.
S102:Activation aluminous fly-ash is mixed with sodium hydroxide solution and carries out pre-desiliconizing processing, filtering obtains desiliconization height Aluminium powder coal ash.
After S101 and S102, the alumina silica ratio of obtained desiliconization aluminous fly-ash is up to 2.5 or more, specifically, aluminium silicon Than for 2.5-3.8, the mass fraction of the sodium oxide molybdena in desiliconization aluminous fly-ash is 0.5-3.0%.
Above-mentioned pre-desiliconizing processing can be identical as conventional method, that is, by activation aluminous fly-ash and sodium hydroxide solution It after mixing, heats, stirring, so that the amorphous silicon di-oxide in activation aluminous fly-ash is reacted with sodium hydroxide solution and generate silicic acid Sodium improves the alumina silica ratio in desiliconization flyash to reduce the silicone content in aluminous fly-ash.
When activating aluminous fly-ash and sodium hydroxide solution after reaction, reaction system is filtered, and use tap water pair Filter cake is washed, dry cake, and the filter cake after drying is desiliconization aluminous fly-ash.
Meanwhile filtrate can also recycle.On the one hand, filtrate can be used for preparing active silicic acid sodium, calcium silicates or Zeolite molecular sieve is prepared, another aspect filtrate can be concentrated to give sodium hydroxide solution and be re-used for activation aluminous fly-ash In pre-desiliconizing processing.
Specifically, in S102, the mass fraction of sodium hydroxide solution is 5%~20%, and works as sodium hydroxide solution When mass ratio with activation aluminous fly-ash is 2~10, all amorphous state titanium dioxides in activation aluminous fly-ash can either be met Silicon is completely converted into sodium metasilicate, and will not cause that reaction system is excessive, processing cost is excessively high.
Meanwhile after activation aluminous fly-ash is mixed with sodium hydroxide solution, the temperature of reaction system can be risen to 50 DEG C -120 DEG C, to promote reacting for amorphous silicon di-oxide and sodium hydroxide solution, in general, in autoclave (0.1- Activation aluminous fly-ash after heating body in 0.3Mpa) stirs 0.5-2h with sodium hydroxide solution, it will be able to it is high to stop activation Aluminium powder coal ash is reacted with sodium hydroxide solution, that is, terminates pre-desiliconizing processing.
Fig. 2 is the flow chart of another embodiment of method of pre-desiliconizing with high alumina fly ash of the present invention, in the base of above-described embodiment On plinth, S101 is specifically included:
S201:Aluminous fly-ash is mixed with acidizer solution, obtains mixture;
S202:Physically activated processing is carried out to mixture using ball mill or disc mill, filtering obtains activation high-alumina fly Coal ash.
That is, activation process can be that after mixing aluminous fly-ash with acidizer solution, mixture is placed in Physically activated processing is carried out in ball mill or disc mill, and when physically activated after treatment, reaction system is filtered, is washed It washs, filter cake is to activate aluminous fly-ash.
Wherein, the acidizer solution is the aqueous solution of acidizer, and the acidizer is selected from sulfuric acid, hydrochloric acid, nitre It is one or more in acid and phosphoric acid;In the acidizer solution, the mass fraction of the acidizer is 3-30%.Acid Inorganic agent can select common acid solution, such as sulfuric acid, hydrochloric acid, phosphoric acid and nitric acid, and the present invention is not intended to limit sour processing The quantity of agent type can be the aqueous solution of any one of above-mentioned acid solution, can also be two kinds in above-mentioned acid solution or two kinds The aqueous solution of the above mix acid liquor, for example, acidizer can be any one of hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, it can also It is the mixture of hydrochloric acid and sulfuric acid, can also be the mixture of hydrochloric acid, phosphoric acid, nitric acid.And when acidizer is a variety of acid solutions Mixture when, the present invention is not intended to limit the ratio between each acid solution.
It is to reduce amorphous state in aluminous fly-ash using acidizer by the purpose that aluminous fly-ash is mixed with acidizer The chemical inertness of silica, in order to further enhance the effect of chemical activation processing, at mixing aluminous fly-ash with acid When managing agent, the mass ratio that can control acidizer and aluminous fly-ash is 2~10.
Further, in order to enhance the sour treatment effect of acidizer, after aluminous fly-ash is mixed with acidizer, 50-100 DEG C can be heated the mixture to.
Then, mixture is placed in ball mill or disc mill and carries out physically activated processing, so-called physically activated processing It is exactly that ball milling or mill processing are carried out to the aluminous fly-ash in mixture, by aluminous fly-ash ball milling or mill to smaller grain Diameter (5-40 μm) reduces amorphous silicon di-oxide to increase the surface area of aluminous fly-ash (including amorphous silicon di-oxide) Physical inertness.
Further, the time for controlling physically activated processing is 0.5min~60min.
It is noted that in the present embodiment, when mixture is during carrying out physically activated processing, high alumina fine coal Ash can also react simultaneously with acidizer solution, i.e. the activation process of the present embodiment includes the physically activated place being carried out at the same time Reason and chemical activation processing.
After S202, in the processing for carrying out S101.
Fig. 3 is the flow chart of the method another embodiment of pre-desiliconizing with high alumina fly ash of the present invention, in the base of above-described embodiment On plinth, S101 is specifically included:
S301:Physically activated processing is carried out to aluminous fly-ash using ball mill or disc mill, it is high to obtain intermediate activation Aluminium powder coal ash;
S302:Centre activation aluminous fly-ash is mixed with acidizer solution and carries out chemical activation processing, filtering obtains Activate aluminous fly-ash.
That is, in the present embodiment, first carrying out physically activated processing (ball-milling treatment or mill to aluminous fly-ash Processing) intermediate activation aluminous fly-ash is obtained, centre activation aluminous fly-ash is being mixed into progress chemistry with acidizer solution Activation process obtains activation aluminous fly-ash.
First, aluminous fly-ash is placed in ball mill or disc mill and carries out physically activated processing, it is so-called physically activated Processing is exactly to carry out ball milling or mill to aluminous fly-ash to handle, by aluminous fly-ash ball milling or mill to smaller grain size (5- 40 μm), to increase the surface area of aluminous fly-ash (including amorphous silicon di-oxide), reduce the physics of amorphous silicon di-oxide Inertia.
Further, the time for controlling physically activated processing is 0.5min~60min.
Then, progress chemistry will be mixed with acidizer by the physically activated obtained intermediate activation aluminous fly-ash that handles Activation process finally obtains activation to reduce the chemical inertness of amorphous silicon di-oxide in aluminous fly-ash using acidizer Aluminous fly-ash.
It, can be with when mixing aluminous fly-ash and acidizer in order to further enhance the effect of chemical activation processing The mass ratio for controlling acidizer and aluminous fly-ash is 2~10, and the treatment temperature of control chemical activation processing is 50 DEG C -100 DEG C, the processing time of control chemical activation processing is 30min~120min.
Wherein, the acidizer solution is the aqueous solution of acidizer, and the acidizer is selected from sulfuric acid, hydrochloric acid, nitre It is one or more in acid and phosphoric acid;In the acidizer solution, the mass fraction of the acidizer is 3-30%.Acid Inorganic agent can select common acid solution, such as sulfuric acid, hydrochloric acid, phosphoric acid and nitric acid, and the present invention is not intended to limit sour processing The quantity of agent type can be the aqueous solution of any one of above-mentioned acid solution, can also be two kinds in above-mentioned acid solution or two kinds The aqueous solution of the above mix acid liquor, for example, acidizer can be any one of hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, it can also It is the mixture of hydrochloric acid and sulfuric acid, can also be the mixture of hydrochloric acid, phosphoric acid, nitric acid.And when acidizer is a variety of acid solutions Mixture when, the present invention is not intended to limit the ratio between each acid solution.
That is, in the present embodiment, activation process includes at the physically activated processing sequentially completed and chemical activation Reason.
After S302, in the processing for carrying out S101.
Hereinafter, the method for introducing the pre-desiliconizing with high alumina fly ash of the present invention by four specific embodiments.
Embodiment 1
The method of the pre-desiliconizing with high alumina fly ash of the present embodiment includes the following steps:
1) 100g aluminous fly-ash is taken, using disc mill polishing 0.5min, generates intermediate activation aluminous fly-ash;
Wherein, the mass fraction of the aluminium oxide in aluminous fly-ash is 47.21%, and the mass fraction of silica is 39.72%;
2) the above-mentioned intermediate aluminous fly-ash that activates is mixed with mass fraction for 14.5% sulfuric acid, wherein sulfuric acid solution Mass ratio with intermediate activation aluminous fly-ash is 3, is heated to 90 DEG C and stirs 120min, filter, rinses filter cake, must activate height Aluminium powder coal ash;
3) sodium hydroxide solution by above-mentioned activation aluminous fly-ash with mass concentration for 12% 280ml mixes, 115 Enter in autoclave under the conditions of DEG C and react 1h, is then filtered by vacuum to obtain the desiliconization liquid of liquid phase and the flyash of solid phase Filter cake;In 105 DEG C of temperature drying as desiliconization flyash manufactured in the present embodiment after Washing of Filter Cake.
After testing, the alumina silica ratio of the desiliconization flyash of the present embodiment is 2.67, Na2O percentage compositions are 1.67%.
Embodiment 2
The method of the pre-desiliconizing with high alumina fly ash of the present embodiment includes the following steps:
1) 100g aluminous fly-ash is taken, using ball mill polishing 30min, generates intermediate activation aluminous fly-ash;
Wherein, the mass fraction of the aluminium oxide in aluminous fly-ash is 45.20%, and the mass fraction of silica is 41.55%;
2) will above-mentioned intermediate activation aluminous fly-ash be 10% with mass fraction mixed in hydrochloric acid, wherein hydrochloric acid solution with The mass ratio of centre activation aluminous fly-ash is 4, is heated to 93 DEG C and stirs 110min, filter, rinses filter cake, obtain activation high alumina Flyash;
3) sodium hydroxide solution by above-mentioned activation aluminous fly-ash with mass concentration for 11.5% 290ml mixes, Enter in autoclave under the conditions of 120 DEG C and react 1h, is then filtered by vacuum to obtain the desiliconization liquid of liquid phase and the powder of solid phase Coal ash filter cake;In 105 DEG C of temperature drying as desiliconization flyash manufactured in the present embodiment after Washing of Filter Cake.
After testing, the alumina silica ratio of the desiliconization flyash of the present embodiment is 2.61, Na2O percentage compositions are 1.73%.
Embodiment 3
The method of the pre-desiliconizing with high alumina fly ash of the present embodiment includes the following steps:
1) 100g aluminous fly-ash is taken, is mixed with the sulfuric acid that mass fraction is 15% and generates mixture, wherein sulfuric acid solution Mass ratio with aluminous fly-ash is 3;
In the aluminous fly-ash of the present embodiment, the mass fraction of aluminium oxide is 45.20%, and the mass fraction of silica is 41.55%;
2) after heating the mixture to 95 DEG C, it is placed in ball milling 100min in ball mill, is filtered, filter cake is rinsed, height must be activated Aluminium powder coal ash;
3) sodium hydroxide solution by above-mentioned activation aluminous fly-ash with mass concentration for 12.5% 280ml mixes, Enter in autoclave under the conditions of 120 DEG C and react 1h, is then filtered by vacuum to obtain the desiliconization liquid of liquid phase and the powder of solid phase Coal ash filter cake;In 105 DEG C of temperature drying as desiliconization flyash manufactured in the present embodiment after Washing of Filter Cake.
After testing, the alumina silica ratio of the desiliconization flyash of the present embodiment is 2.63, Na2O percentage compositions are 1.57%.
Embodiment 4
The method of the pre-desiliconizing with high alumina fly ash of the present embodiment includes the following steps:
1) 100g aluminous fly-ash is taken, the mixed in hydrochloric acid for being 15% with mass fraction generates mixture, wherein sulfuric acid solution Mass ratio with aluminous fly-ash is 4;
In the aluminous fly-ash of the present embodiment, the mass fraction of aluminium oxide is 49.20%, and the mass fraction of silica is 39.55%;
2) after heating the mixture to 95 DEG C, it is placed in ball milling 100min in ball mill, is filtered, filter cake is rinsed, height must be activated Aluminium powder coal ash;
3) sodium hydroxide solution by above-mentioned activation aluminous fly-ash with mass concentration for 12% 380ml mixes, 120 Enter in autoclave under the conditions of DEG C and react 1h, is then filtered by vacuum to obtain the desiliconization liquid of liquid phase and the flyash of solid phase Filter cake;In 105 DEG C of temperature drying as desiliconization flyash manufactured in the present embodiment after Washing of Filter Cake.
After testing, the alumina silica ratio of the desiliconization flyash of the present embodiment is 3.50, Na2O percentage compositions are 2.41%.
Embodiment 5
The method of the pre-desiliconizing with high alumina fly ash of the present embodiment includes the following steps:
1) 100g aluminous fly-ash is taken, the nitric acid and quality that the phosphoric acid and mass fraction for being 10% with mass fraction are 10% The mixed in hydrochloric acid of score 10% generates mixture, and (mass ratio of phosphoric acid, nitric acid and hydrochloric acid is 1:1:1), wherein acidizer is molten The mass ratio of the liquid mixture of nitric acid and hydrochloric acid (phosphoric acid) and aluminous fly-ash is 4.5;
In the aluminous fly-ash of the present embodiment, the mass fraction of aluminium oxide is 49.3%, and the mass fraction of silica is 38.6%;
2) after heating the mixture to 95 DEG C, it is placed in ball milling 100min in ball mill, is filtered, filter cake is rinsed, height must be activated Aluminium powder coal ash;
3) sodium hydroxide solution by above-mentioned activation aluminous fly-ash with mass concentration for 13% 400ml mixes, 115 Enter in autoclave under the conditions of DEG C and react 1h, is then filtered by vacuum to obtain the desiliconization liquid of liquid phase and the flyash of solid phase Filter cake;In 105 DEG C of temperature drying as desiliconization flyash manufactured in the present embodiment after Washing of Filter Cake.
After testing, the alumina silica ratio of the desiliconization flyash of the present embodiment is 3.35, Na2O percentage compositions are 2.70%.
Finally it should be noted that:The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations;To the greatest extent Present invention has been described in detail with reference to the aforementioned embodiments for pipe, it will be understood by those of ordinary skill in the art that:Its according to So can with technical scheme described in the above embodiments is modified, either to which part or all technical features into Row equivalent replacement;And these modifications or replacements, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution The range of scheme.

Claims (10)

1. a kind of method of pre-desiliconizing with high alumina fly ash, which is characterized in that include the following steps:
1) activation process is carried out to the aluminous fly-ash, obtains activation aluminous fly-ash;
2) the activation aluminous fly-ash is mixed with sodium hydroxide solution and carries out pre-desiliconizing processing, filtering obtains desiliconization high alumina Flyash;
Wherein, the alumina silica ratio of the desiliconization aluminous fly-ash is 2.5-3.8, the matter of the sodium oxide molybdena in the desiliconization aluminous fly-ash Amount score is 0.5-3.0%.
2. the method for pre-desiliconizing with high alumina fly ash according to claim 1, which is characterized in that the activation process includes such as Lower step:
A. the aluminous fly-ash is mixed with acidizer solution, obtains mixture;
B. physically activated processing is carried out to the mixture using ball mill or disc mill, filtering obtains the activation high alumina Flyash;
Wherein, the acidizer solution be acidizer aqueous solution, the acidizer be selected from sulfuric acid, hydrochloric acid, nitric acid and It is one or more in phosphoric acid;In the acidizer solution, the mass fraction of the acidizer is 3-30%.
3. the method for pre-desiliconizing with high alumina fly ash according to claim 1, which is characterized in that the activation process includes such as Lower step:
C. physically activated processing is carried out to the aluminous fly-ash using ball mill or disc mill, obtains intermediate activation high-alumina fly Coal ash;
D. the intermediate aluminous fly-ash that activates is mixed into progress chemical activation processing with acidizer solution, filtering obtains institute State activation aluminous fly-ash;
Wherein, the acidizer solution be acidizer aqueous solution, the acidizer be selected from sulfuric acid, hydrochloric acid, nitric acid and It is one or more in phosphoric acid;In the acidizer solution, the mass fraction of the acidizer is 3-30%.
4. the method for pre-desiliconizing with high alumina fly ash according to claim 2, which is characterized in that before step B, further include 50-100 DEG C is heated to the mixture.
5. the method for pre-desiliconizing with high alumina fly ash according to claim 4, which is characterized in that described in the mixture The mass ratio of acidizer solution and the aluminous fly-ash is 2~10.
6. according to the method for any pre-desiliconizing with high alumina fly ash of claim 2-5, which is characterized in that described physically activated The time of processing is 0.5min~60min.
7. according to the method for the pre-desiliconizing with high alumina fly ash described in claim 3, which is characterized in that the acidizer solution is in Between activation aluminous fly-ash mass ratio be 2~10.
8. the method for pre-desiliconizing with high alumina fly ash according to claim 7, which is characterized in that control at the chemical activation The treatment temperature of reason is 50 DEG C -100 DEG C, and the processing time for controlling the chemical activation processing is 30min~120min.
9. the method for pre-desiliconizing with high alumina fly ash according to claim 1, which is characterized in that the sodium hydroxide solution Mass fraction is 5%~20%, and the mass ratio of the sodium hydroxide solution and the activation aluminous fly-ash is 2~10.
10. the method for pre-desiliconizing with high alumina fly ash according to claim 9, which is characterized in that control at the pre-desiliconizing The treatment temperature of reason is 50 DEG C -120 DEG C, and the processing time for controlling the pre-desiliconizing processing is 0.5-2h.
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CN114988422A (en) * 2022-08-05 2022-09-02 中国科学院过程工程研究所 High-modulus water glass obtained by utilizing gasified coarse slag and preparation method and application thereof
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