CN104671811B - A kind of method utilizing two sections of acid treatments of aluminous fly-ash to prepare mullite - Google Patents
A kind of method utilizing two sections of acid treatments of aluminous fly-ash to prepare mullite Download PDFInfo
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Abstract
The invention belongs to aluminous fly-ash comprehensive utilization, refractory material synthesis technical field, specifically disclose a kind of method that aluminous fly-ash prepares mullite through pre-desiliconizing, two sections of acid treatments.The present invention, with aluminous fly-ash as raw material, obtains mullite through pre-desiliconizing, two sections of acid treatments, washing, roastings.Wherein, two sections of acid treatment processes include that dilute acid pretreatment, concentrated acid process.Compared with the existing technology, the inventive method raw material sources are wide, add any aluminum source without extra, and the mullite obtained has the features such as aluminum content is high, impurity content is low, and production cost is low, does not produce secondary solid pollutant, economy and obvious environment benefit.
Description
Technical field
The invention belongs to field of inorganic chemical engineering, relate to the synthetic technology neck of solid waste comprehensive utilization, refractory material
Territory；In particular it relates to a kind of method utilizing two sections of acid treatments of aluminous fly-ash to prepare mullite.
Background technology
Aluminous fly-ash be middle of Inner Mongolia, northern Shanxi characteristic high alumina coal burning generating after produce solid
Garbage.Year generation amount about 30,000,000 tons at present, but comprehensive utilization ratio is less than 20%, causes serious environment dirty
Dye.On the other hand, aluminous fly-ash potential resources is big, its Al2O3Content > 40%, mainly mutually steady with mullite
Fixed existence, can be used for replacing the bauxite of worsening shortages to prepare mullite refractory.
At present by the research of flyash mullite synthesizing mainly for the purpose of improving alumina silica ratio.CN102092734A is open
A kind of utilize coal ash for manufacturing for the method for mullite, with flyash, In Powdered Aluminium source and Kaolin for raw material through toning
Join to fire and obtain mullite.CN101643359A disclose a kind of utilize coal ash for manufacturing for the method for porzite powder,
By flyash with bauxite carries out dispensing, mullite is prepared in calcining.CN102765944A discloses one and utilizes fine coal
Ash prepares the method for mullite, flyash and aluminium oxide is carried out dispensing, calcining, obtains not coming of higher aluminum silicon ratio
Stone product.Generally, existing research is both needed to additionally add the high aluminum mineral such as bauxite, commercial alumina, and cost is relatively
High and impurity content is difficult to be greatly lowered.Based on this, our unit's early stage proposes diluted acid activation, deep desilication
Technical thought, CN102583411A and CN102583409A discloses and a kind of utilizes flyash to produce mullite
Method, with aluminous fly-ash as raw material, through processes such as pretreatment, desiliconization, acid activation, secondary desiliconization, sintering
Obtain mullite.Compared with proposing thinking with early stage, this thinking achieves and prepares high-quality without high aluminum mineral
The technical thought of mullite, alumina content can reach 60%-70%, but the impurity such as ferrum calcium not yet realize the degree of depth and take off
Remove, it is difficult to reach high-end aluminum silica refractory and use requirement.
Summary of the invention
For the studies above present situation, present invention further propose that two sections of acid treatment processes of desiliconization flyash so that place
After reason, in aluminous fly-ash, alumina content reaches 65%, and iron content is down to about 0.3%, and sodium content is down to less than 0.1%,
Calcium content is down to less than 0.5%, it is achieved effectively controlling and the significantly lifting of alumina content of impurity content.Enter one
Step uses the aluminous fly-ash after this process, through washing, the mullite product of the calcining and other processes high trade mark of synthesis.
The technical problem to be solved in the present invention is mainly realized by below scheme:
The present invention utilizes the method that two sections of acid treatments of aluminous fly-ash prepare mullite, comprises the following steps:
(1) aluminous fly-ash is mixed with sodium hydroxide dilute alkaline soln carry out pre-desiliconizing process, filter after process
Operation obtains filter cake and filtrate；
(2) the filter cake dilute hydrochloric acid that step (1) is produced is carried out desiliconization activation processing, through being filtrated to get filter cake；
(3) the filter cake concentrated hydrochloric acid that step (2) is produced is carried out acid treatment remove impurity process, through being filtrated to get two
Secondary acid treatment filter cake；
(4) quadratic acid produced by step (3) is processed filter cake wash, filter, roasting, obtain whiteness
Preferably, the product mullite product that alumina silica ratio is higher.
The method that two sections of acid treatments of aluminous fly-ash prepare mullite, wherein step (1) institute is utilized according to the present invention
The dilute alkaline soln stated is sodium hydroxide, potassium hydroxide etc., and concentration is at 4.5-5.5mol/L；After mixing, slip product contains admittedly
Amount is at 300g/L-400g/L, and the treatment temperature of described pre-desiliconizing is between 80-100 DEG C, and the process time is 1.5-4.0h.
Described dilute alkaline soln is the filter operation involved by 1-5mL/g step (1) with the liquid-solid ratio of aluminous fly-ash, uses
Filter method well known in the art.
The method that two sections of acid treatments of aluminous fly-ash prepare mullite, the acid in step (2) is utilized according to the present invention
Can be one or more in hydrochloric acid, sulphuric acid, nitric acid, oxalic acid etc., hydrogen ion concentration be at 0.5-1.5mol/L, liquid
Gu ratio is between 8.0-12.0, reaction temperature is at 45-65 DEG C, and the response time is 20-60min.
The method that two sections of acid treatments of aluminous fly-ash prepare mullite, the acid in step (3) is utilized according to the present invention
Can be hydrochloric acid, sulphuric acid, nitric acid, oxalic acid etc., hydrogen ion concentration at 5.0-7.0mol/L, liquid-solid ratio between 3-5,
Reaction temperature is between 60-80 DEG C, and the response time is 0.5-1.5h.
Utilizing, according to the present invention, the method that two sections of acid treatments of aluminous fly-ash prepare mullite, step (4) is water washed
Cheng Zhong, water and quadratic acid process filter cake quality ratio are between 2-4, between washing temperature is 80-95 DEG C, after washing
Quadratic acid processes before filter cake enters kiln roasting and fully washs to PH more than 3.0, and sintering temperature is at 800-1200 DEG C.
Compared with prior art, the present invention is on the basis of the early stage one dense acid treatment process of step, for impurity such as ferrum calcium
The needs of deep removal, use diluted acid-concentrated acid two step process to process flyash after desiliconization, can ensure alumina content
Being greatly lowered of impurity is realized on the basis of raising.In mullite product after sintering, iron content is less than 0.4%, calcium
Content is less than 0.5%, can produce for high-grade refractory material as raw material.
Accompanying drawing explanation
Fig. 1 is that the flow chart of mullite is prepared in the two sections of acid treatments of aluminous fly-ash that utilize of the present invention.
Detailed description of the invention
Further describing the present invention below in conjunction with the fact that concrete case, these examples are only model's property, the most right
The scope of the present invention constitutes any restriction.Those skilled in the art it should be understood that without departing from the present invention spirit and
Technical scheme details and form can be modified or replace under scope, but these amendments and invention are all
Within belonging to scope of the invention.
Case study on implementation 1
Pre-desiliconizing: use alumina content be not less than 42% flyash and concentration be 4.5mol/L sodium hydroxide solution
By liquid-solid ratio 3:1 mix homogeneously post-heating to 80 DEG C, after with the speed responsing 3.5h of 300r/min, washing, filtering
Obtain desiliconization flyash.
Acid treatment: by desiliconization flyash and concentration be 0.5mol/L, 65 DEG C of hydrochloric acid be that 12:1 mixes according to liquid-solid ratio
Close, with 300r/min speed responsing 60min, wash, filter after the filter cake that obtains and concentration be 5.0mol/L, 80 DEG C
Concentrated hydrochloric acid by liquid-solid for 5:1 mix, with the speed responsing 1.5h of 300r/min, wash, filter after obtain secondary
Acid treatment filter cake.
Roasting: quadratic acid is processed filter cake at 80 DEG C, be washed to pH3.0 by liquid-solid mass ratio 2:1, filter laggard
Klining system, firing temperature is 800 DEG C, obtains alumina silica ratio and is about 2.5, and iron content is about 0.47%, and sodium content is 0.08%,
Calcium content is the mullite product of 0.5%.
Case study on implementation 2
Pre-desiliconizing: use alumina content be not less than 42% flyash and concentration be 5mol//L potassium hydroxide solution by
Liquid-solid ratio be 3:1 mix homogeneously post-heating to 100 DEG C, stir reaction 2.5h, washing, mistake with the speed of 300r/min
Desiliconization flyash is obtained after filter.
Acid treatment: by desiliconization flyash and concentration be 1.0mol//L, 55 DEG C of nitric acid be that 10:1 mixes according to liquid-solid ratio
Close, stir reaction 40min with the mixing speed of 300r/min, wash, filter after the filter cake that obtains with concentration be
6.0mol/L, the concentrated nitric acid of 70 DEG C are mixed for 4:1 as liquid-solid, with the speed responsing 1.0h of 300r/min, washing, mistake
Obtain quadratic acid after filter and process filter cake.
Roasting: quadratic acid is processed filter cake at 90 DEG C, be washed to pH4.0 by liquid-solid mass ratio 3:1, filter laggard
Klining system, firing temperature is 800 DEG C, obtains alumina silica ratio and is about 2.7, and iron content is about 0.39%, and sodium content is 0.02%,
Calcium content is the mullite product of 0.41%.
Case study on implementation 3
Pre-desiliconizing: use alumina content be not less than 42% flyash and NaOH concentration be 5.5mol/L hydroxide
Sodium solution by liquid-solid ratio be 3:1 mix homogeneously post-heating to 90 DEG C, stir reaction 1.5h with the speed of 300r/min,
Desiliconization flyash is obtained after washing, filtration.
Acid treatment: by desiliconization flyash and concentration be 1.5mol/L, 45 DEG C of hydrochloric acid be that 8:1 mixes according to liquid-solid ratio,
Stir reaction 20min with the mixing speed of 300r/min, wash, filter after the filter cake that obtains and concentration be 7.0mol/L,
The sulphuric acid of 60 DEG C by liquid-solid ratio be 3:1 mixing, with the speed responsing 0.5h of 300r/min, wash, filter after obtain
Quadratic acid processes filter cake.
Roasting: quadratic acid is processed filter cake at 95 DEG C, be washed to pH4.5 by liquid-solid mass ratio 4:1, filter laggard
Klining system, firing temperature is 1200 DEG C, obtains alumina silica ratio and is about 3.0, and iron content is about 0.35%, and sodium content is 0,
Calcium content is the mullite product of 0.25%.
Case study on implementation 4
Pre-desiliconizing: use alumina content be not less than 42% flyash and NaOH concentration be 4.5mol/L hydroxide
Sodium solution by liquid-solid ratio be 3:1 mix homogeneously post-heating to 100 DEG C, stir reaction 2.5h with the speed of 300r/min,
Desiliconization flyash is obtained after washing, filtration.
Acid treatment: by desiliconization flyash and concentration be 1.5mol/L, 55 DEG C of hydrochloric acid be that 8:1 mixes according to liquid-solid ratio,
Stir reaction 60min with the mixing speed of 300r/min, wash, filter after the filter cake that obtains and concentration be 6.0mol/L,
The concentrated hydrochloric acid of 60 DEG C by liquid-solid ratio be 5:1 mixing, with the speed responsing 1.5h of 300r/min, wash, filter after two
Secondary obtain acid treatment filter cake.
Roasting: quadratic acid is processed filter cake at 85 DEG C, be washed to pH3.5 by liquid-solid mass ratio 2:1, filter laggard
Klining system, firing temperature is 1000 DEG C, obtains alumina silica ratio and is about 2.5, and iron content is about 0.37%, and sodium content is 0,
Calcium content is the mullite product of 0.34%.
Case study on implementation 5
Pre-desiliconizing: use alumina content be not less than 42% flyash and NaOH concentration be 5.5mol/L hydroxide
Sodium solution by liquid-solid ratio be 3:1 mix homogeneously post-heating to 80 DEG C, stir reaction 3.5h with the speed of 300r/min,
Desiliconization flyash is obtained after washing, filtration.
Acid treatment: by desiliconization flyash and concentration be 1.0mol/L, 65 DEG C of hydrochloric acid be that 10:1 mixes according to liquid-solid ratio
Close, stir reaction 40min with the mixing speed of 300r/min, wash, filter after the filter cake that obtains with concentration be
7.0mol/L, the concentrated hydrochloric acid of 70 DEG C are 3:1 mixing by liquid-solid ratio, with the speed responsing 0.5h of 300r/min, wash,
Obtain quadratic acid after filtration and process filter cake.
Roasting: quadratic acid is processed filter cake at 80 DEG C, be washed to pH4.0 by liquid-solid mass ratio 4:1, filter laggard
Klining system, firing temperature is 900 DEG C, obtains alumina silica ratio and is about 2.8, and iron content is about 0.35%, and sodium content is 0,
Calcium content is the mullite product of 0.32%.
Case study on implementation 6
Pre-desiliconizing: use alumina content be not less than 42% flyash and NaOH concentration be 5.0mol/L hydroxide
Sodium solution by liquid-solid ratio be 3:1 mix homogeneously post-heating to 90 DEG C, stir reaction 1.5h with the speed of 300r/min,
Desiliconization flyash is obtained after washing, filtration.
Acid treatment: by desiliconization flyash and concentration be 0.5mol/L, 45 DEG C of hydrochloric acid be that 12:1 mixes according to liquid-solid ratio
Close, stir reaction 20min with the mixing speed of 300r/min, wash, filter after the filter cake that obtains with concentration be
5.0mol/L, the concentrated hydrochloric acid of 80 DEG C are 4:1 mixing by liquid-solid ratio, with the speed responsing 1.0h of 300r/min, wash,
Obtain quadratic acid after filtration and process filter cake.
Roasting: quadratic acid is processed filter cake at 90 DEG C, be washed to pH4.0, after filtration by liquid-solid mass ratio 2.5:1
Entering klining system, firing temperature is 800 DEG C, obtains alumina silica ratio and is about 2.9, and iron content is about 0.35%, and sodium content is 0,
Calcium content is the mullite product of 0.39%.
Above example is merely to illustrate the preferred embodiment of the present invention, but the present invention is not limited to above-mentioned embodiment party
Formula, in the ken that described field those of ordinary skill is possessed, is done within the spirit and principles in the present invention
Any amendment, equivalent substitute and improvement etc., its all should contain the technical scheme scope that is claimed in the present invention it
In.
Claims (9)
1. the method utilizing two sections of acid treatments of aluminous fly-ash to prepare mullite, comprises the following steps:
(1) aluminous fly-ash is mixed with dilute alkaline soln carry out pre-desiliconizing process, carry out filter operation after process and obtain filter cake and filtrate；Wherein, the hydroxyl concentration of described dilute alkaline soln is at 4.5-5.5mol/L；
(2) the filter cake diluted acid that step (1) is produced is processed, through being filtrated to get filter cake；Wherein, the hydrogen ion concentration of described diluted acid is 0.5-1.5mol/L；
(3) the filter cake concentrated acid that step (2) is produced is processed, process filter cake through being filtrated to get quadratic acid；Wherein, the hydrogen ion concentration of described concentrated acid is at 5.0-7.0mol/L；
(4) quadratic acid produced by step (3) is processed filter cake wash, filter, roasting, obtain mullite product.
The method preparing mullite the most according to claim 1, it is characterised in that the dilute alkaline soln described in step (1) is sodium hydroxide or potassium hydroxide solution.
The method preparing mullite the most according to claim 1 and 2, it is characterised in that the condition of described pre-desiliconizing reaction is that dilute alkaline soln is 1-5mL/g with the liquid-solid ratio of aluminous fly-ash, and treatment temperature is between 80-100 DEG C, and the process time is 1.5-3.5h.
The method preparing mullite the most according to claim 1, it is characterised in that the diluted acid described in step (2) is one or more in hydrochloric acid, sulphuric acid, nitric acid or oxalic acid.
5., according to the method preparing mullite described in claim 1 or 4, it is characterised in that the condition of step (2) described dilute acid pretreatment is, the liquid-solid ratio of diluted acid and filter cake is at 8.0-12.0mL/g, and reaction temperature is at 45-65 DEG C, and the response time is 20-60min.
The method preparing mullite the most according to claim 1, it is characterised in that step (3) described concentrated acid is one or more in hydrochloric acid, sulphuric acid, nitric acid or oxalic acid.
7. according to the method preparing mullite described in claim 1 or 6, it is characterised in that the condition that step (3) described concentrated acid processes is, concentrated acid is 3-5mL/g with the liquid-solid ratio of filter cake, and reaction temperature is between 60 DEG C-80 DEG C, and the response time is 0.5-1.5h.
The method preparing mullite the most according to claim 1, it is characterised in that in step (4), water and quadratic acid process filter cake quality ratio are between 2-4, between washing temperature is 80-95 DEG C.
9., according to the method preparing mullite described in claim 1 or 8, it is characterised in that in step (4), quadratic acid fully washs to pH more than 3.0 before processing filter cake roasting, and sintering temperature is at 800-1200 DEG C.
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Families Citing this family (11)
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| CN106220190A (en) * | 2015-11-12 | 2016-12-14 | 中国科学院过程工程研究所 | A kind of method utilizing aluminous fly-ash to prepare mullite |
| CN106518035B (en) * | 2016-11-18 | 2019-07-23 | 南昌航空大学 | A kind of method that modified coal ash high yield prepares high-purity mullite powder |
| CN107021765B (en) * | 2017-05-25 | 2020-03-10 | 中国科学院过程工程研究所 | Method for preparing mullite and co-producing polyaluminium chloride by using high-alumina fly ash |
| CN107199310B (en) * | 2017-05-25 | 2019-04-23 | 中国科学院过程工程研究所 | A method of precision casting sand is produced using aluminous fly-ash |
| CN111606339B (en) * | 2020-05-22 | 2023-01-10 | 内蒙古蒙泰集团有限公司 | Method for preparing aluminum-silicon oxide by using fly ash |
| CN115340391B (en) * | 2021-05-14 | 2023-10-20 | 中国科学院过程工程研究所 | Desilication fly ash and preparation method and application thereof |
| CN114506870A (en) * | 2022-03-15 | 2022-05-17 | 昆明理工大学 | Production of NaAlO by using high-alumina fly ash2/γ-Al2O3Method for preparing nano mesoporous material |
| CN115403364B (en) * | 2022-09-09 | 2023-07-14 | 天津大学 | Method for preparing columnar mullite by rapid sintering process after pretreatment of high-alumina fly ash |
| CN116282053A (en) * | 2022-09-09 | 2023-06-23 | 天津大学 | Method for preparing high-alumina-silica-ratio low-impurity primary crystal mullite by using high-alumina fly ash |
| CN115448708B (en) * | 2022-10-10 | 2023-05-26 | 天津大学 | Method for in-situ synthesis of high-strength low-heat-conductivity porous mullite ceramic by high-alumina fly ash pretreatment |
| CN118579815A (en) * | 2024-08-07 | 2024-09-03 | 内蒙古蒙泰集团有限公司 | Method for preparing aluminum silicon oxide by using high-alumina fly ash |
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| DE19952337B4 (en) * | 1999-09-16 | 2007-03-08 | Council Of Scientific & Industrial Research | Process for the preparation of silicon-containing precursors, the precursor itself and processes for the production of ceramic materials |
| CN102583409B (en) * | 2012-01-10 | 2014-07-02 | 中国科学院过程工程研究所 | Method for producing mullite and calcium silicate by using high-alumina fly ash |
| CN102583411B (en) * | 2012-01-10 | 2014-04-02 | 中国科学院过程工程研究所 | Method for producing mullite by using fly ash |
| CN103708480A (en) * | 2013-11-28 | 2014-04-09 | 内蒙古工业大学 | Method for preparing microcrystalline mullite from fly ash |
| CN103964866A (en) * | 2014-04-23 | 2014-08-06 | 中国地质大学（北京） | Method for preparing lightweight mullite refractory by high-alumina fly ash |
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