CN109231245A - A kind of desilication method of silicon-aluminum containing material - Google Patents
A kind of desilication method of silicon-aluminum containing material Download PDFInfo
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- CN109231245A CN109231245A CN201811124679.XA CN201811124679A CN109231245A CN 109231245 A CN109231245 A CN 109231245A CN 201811124679 A CN201811124679 A CN 201811124679A CN 109231245 A CN109231245 A CN 109231245A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/06—Preparation 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/06—Preparation 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
- C01F7/0613—Pretreatment of the minerals, e.g. grinding
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/06—Preparation 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
- C01F7/062—Digestion
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/06—Preparation 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
- C01F7/0693—Preparation 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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Abstract
The present invention provides a kind of desilication method of silicon-aluminum containing material, includes the following steps: to be uniformly mixed after taking ferriferous oxide, silicon-aluminum containing material and carbon dust to carry out ore matching, grinding, obtain raw material；Wherein, iron oxide, aluminium oxide in silicon-aluminum containing material, carbon molar ratio be 2~2.4:4:1~1.2；Gained raw material are roasted into 30-60min at 1050~1200 DEG C, obtain clinker；Alkali leaching in sodium hydroxide solution will be added after gained clinker milled processed；Alkali is soaked gained ore pulp to be separated by solid-liquid separation, obtains siliceous lye and desiliconization slag.The present invention can be such that aluminium in silicon-aluminum containing material, silicon realization efficiently separates, and silica removal efficiency is high.Process flow is simple, it is low in cost, it can not only realize the desiliconization of the aluminium silicate minerals such as the cured stone of kaolin, illite, page, the intractable high silicon aluminum-containing mineral desiliconization such as silicon-aluminum containing material milltailings, gangue, flyash and high-speed rail silicon-aluminum containing material can also be made, had broad application prospects and good economic benefit.
Description
Technical field
The present invention relates to mineral engineering technology fields, and in particular to a kind of desilication method of silicon-aluminum containing material.
Background technique
China is the maximum alumina producing state in the whole world, and aluminium oxide annual output in 2017 is more than 60,000,000 tons.With excellent
Matter high aluminium silicon ratio ore it is depleted, developing and using has the low alumina -silica ratio of larger reserves containing bauxite resource is significant, gesture exists
It must go.Bayer process is a kind of industrial widely used chemical process from silicon-aluminum containing material production aluminium oxide.1887 by Austria
Land productivity engineer's karr Joseph's Bayer invention, the basic principle is that being converted aluminium hydroxide to strong caustic
Aluminium hydroxide is precipitated again by diluting and adding aluminium hydroxide crystal seed in sodium aluminate, and remaining sodium hydroxide solution is used again
In processing next group silicon-aluminum containing material, continuous production is realized.And during alumina producing Bayer process, the oxidation of dissolution
Silicon can further react with sodium aluminate solution and generate hydrated aluminum silicate (i.e. Sodium-silica slag) and enter in red mud, to cause
Na in solution2O and Al2O3Loss.Therefore it is current for how reducing the silicone content in high silicon aluminum-containing raw material to improve its alumina silica ratio
The main problem that alumina producing Bayer process faces.
Mainly there are physical method and chemical method for the desiliconization of silicon-aluminum containing material at present in the method for improving its alumina silica ratio.Physics
Method be using ore dressing method by silicon-aluminum containing material siliceous mineral and aluminium mineral separate, be suitble to Bayer process raw to obtain
The high aluminium silicon ratio mineral of production.The physical method of industrial application mainly has direct flotation and reverse flotation at present.Direct flotation is with flotation aluminium
For the purpose of mineral, alumina silica ratio can reach 11 or more in the obtained aluminium oxide concentrate of the method, the rate of recovery of aluminium oxide 85~
90%.But that there are concentrate treating capacities is big, floating agent dosage is high, processing mineral constituent complexity-disseminated grain size is thin for the method
Ore grinding energy consumption height and argillization serious problem when silicon-aluminum containing material.Reverse flotation is then the Ke Yiyou for the purpose of flotation siliceous mineral
Effect ground reduces ore grinding energy consumption using the difference of hardness between aluminosilicate and diaspore mineral, alumina silica ratio in obtained concentrate
9 or so can be reached, alumina recovery rate about 80%.Either all there is floating agent in concentrate and remain in direct flotation or reverse flotation
The problem of, and floating agent can cause damages to subsequent alumina producing Bayer process process.Chemical method can be divided into acid system again and subtract
Method.Acid system can realize the selectivity dissolution of aluminium in aluminium silicate mineral, will also result in the various metals for being soluble in acid at the same time
Oxide dissolution, causes foreign ion in infusion solution to increase, and subsequent removal of impurities is cumbersome.Heat chemistry alkaline leaching is de- as a kind of chemistry
Silicon method is considered as improving silicon-aluminum containing material alumina silica ratio most efficient method, and core is to make manosil AS by oxidizing roasting
Salt mineral decomposite the unformed silica for being soluble in alkali, and aluminium mineral is then decomposed into the α-Al for being insoluble in alkali2O3, to reach
The purpose of desiliconization.Although the method energy consumption is relatively high, its technical indicator is preferable, and alumina silica ratio can reach 11 in obtained concentrate
~15, the rate of recovery of aluminium oxide is 98% or more.But limiting the main reason for this method is widely applied is alkali leaching desiliconization
The dissolution rate of process silica is lower, and small-scale experiment desiliconization rate is 60~80%, but desiliconization rate when to pilot-plant test only has
30%~40%.In addition, above method is unsuitable for handling native mine milltailings, gangue, flyash and high-speed rail silicon-aluminum containing
The intractable high silicon aluminum-containing mineral such as material.
Summary of the invention
Dissolution rate in order to solve the problems, such as silicon-aluminum containing material silica in Conventional thermal alkali leaching desiliconization process is lower,
And the problem of high silicon aluminum-containing mineral desiliconization hardly possible, the present invention propose a kind of desilication method of silicon-aluminum containing material, technical solution is such as
Under:
The present invention provides a kind of desilication methods of silicon-aluminum containing material, and described method includes following steps:
1) it is uniformly mixed after taking ferriferous oxide, silicon-aluminum containing material and carbon dust to carry out ore matching, grinding, obtains raw material；
Wherein, iron oxide in ferriferous oxide, aluminium oxide in silicon-aluminum containing material, carbon molar ratio be 2~2.4:4:1~1.2；
2) raw material obtained by step 1) are roasted at 1050~1200 DEG C 30~60min, obtains clinker；
3) alkali in lye will be added after clinker milled processed obtained by step 2) to soak；
4) step 3) alkali is soaked gained ore pulp to be separated by solid-liquid separation, obtains siliceous lye and desiliconization slag.
The method, step 1) the silicon-aluminum containing material include kaolin, high silicon silicon-aluminum containing material, silicon-aluminum containing material ore dressing
Tailing, gangue or flyash.
The method, the step 2) roasting is to carry out in reducing atmosphere.
The method, the step 3) milled processed are the particle that clinker partial size is processed into d (0.5)≤45 μm.
The method, the caustic sodium concentration of the step 3) lye are 100~150g/L.
The method, the step 3) sodium hydroxide solution and clinker quality ratio are 3~10.
The method, the step 3) sodium hydroxide solution and clinker quality are than preferably 3~5.
The method, step 3) the alkali leaching temperature is 95~125 DEG C.
The method, step 3) the alkali leaching time is 60~120min
Raw material are roasted in a reducing atmosphere with addition of iron oxide, second step in the first step of the present invention, obtain soluble oxygen
The hercynite of SiClx solid solution and cristobalite solid solution and indissoluble.
Third step carries out desiliconization processing by sodium hydroxide solution, during the reaction the silica in silica solid solution
Into sodium hydroxide solution, sodium silicate solution is formed.The solid phase that 4th step obtains after being separated by solid-liquid separation is the high aluminium silicon ratio after desiliconization
Material further can extract aluminium oxide therein using Bayer process.
By taking kaolinic desiliconization as an example, in ore matching, need to the ratio of aluminium oxide, carbon in iron oxide, kaolin into
Row control.When kaolin is with addition of iron oxide, it is desirable that iron oxide and Alumina from Kaolin molar ratio carry out ore matching in 2~2.4:4,
To guarantee that Alumina from Kaolin can be reacted into hercynite phase with ferrous oxide, and silica is then changed into quartz admittedly
Solution or cristobalite solid solution.When iron oxide and Alumina from Kaolin molar ratio are more than 2.4:4, ferrous oxide meeting and oxygen
SiClx reaction generates ferrous metasilicate, to reduce the dissolution rate of silicon solid solution.
By taking kaolinic desiliconization as an example, in reducing roasting process, then need to close maturing temperature and calcining time
Reason control.Guarantee the generation of hercynite in roasting clinker first.It is solid to be changed into silica for the silica in kaolin at this time
Solution or cristobalite solid solution.It is soluble in this characteristic of dilute alkaline soln using silicon solid solution, can be soaked by alkali and realize that roasting is ripe
The desiliconization of material.Secondly, need to effectively inhibit the generation of mullite.The raising of maturing temperature and the extension of calcining time can promote
The mullite phase for further reacting and generating indissoluble with aluminic acid ferrous iron into-cristobalite solid solution-will certainly reduce alkali leaching desiliconization effect
Rate.Therefore maturing temperature and the selection of time must control within the scope of reasonable, and it is brilliant both to guarantee to roast iron aluminium point in clinker
The generation of stone, but other side's quartz solid solution occurs the mullite that secondary response generates with aluminic acid ferrous iron and is mutually effectively inhibited.
This method has the beneficial effect that:
By controlling suitable maturing temperature and calcining time, aluminium oxide and silica in material can be made to be kept completely separate, oxygen
Change aluminium and silica to be respectively present in hercynite and silica solid solution in roasting clinker, it is de- to be conducive to subsequent alkaline leaching
The progress of silicon.The invention is equally applicable to the desiliconization of low alumina -silica ratio raw material, is remarkably improved intractable high silicon aluminum-containing mineral
Alumina silica ratio.
The dissolution rate of silica is optimal up to 95% or more in embodiment.Available silica concentration is dissolved out through multistage to reach
285g/L, the sodium silicate solution that modulus is 3.0.
In conclusion the present invention can be such that aluminium in silicon-aluminum containing material, silicon realization efficiently separates, silica removal efficiency is high.This hair
Bright process flow is simple, low in cost, can not only realize the desiliconization of the aluminium silicate minerals such as the cured stone of kaolin, illite, page, also
The intractable low alumina -silica ratios such as silicon-aluminum containing material milltailings, gangue, flyash and high-speed rail silicon-aluminum containing material can be made containing aluminium
Raw material desiliconization has broad application prospects and good economic benefit.
Detailed description of the invention
Fig. 1 is the process flow chart of the desilication method of silicon-aluminum containing material of the present invention.
Specific embodiment
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with attached drawing and tool
Body embodiment is described in detail.
Kaolinic main chemical compositions used are as shown in table 1 in the embodiment of the present invention, and iron oxide used is the pure examination of chemistry
Agent.
1 kaolin of table and high silicon silicon-aluminum containing material chemical component (wt.%)
Embodiment 1
Iron oxide in molar ratio: Alumina from Kaolin: carbon=2.4:4:1.2 carries out ingredient, pelletizing.It will be small after drying
Ball is placed in corundum crucible, is roasted in reducing atmosphere, and external application coke carries out atmosphere adjusting.1100 DEG C of maturing temperature,
Calcining time 60min；Gained roasting clinker is finely ground to d (0.5)=43.52 μm or so, using sodium hydroxide aqueous slkali to roasting
Overburnt material carries out alkali and soaks desiliconization, and extraction temperature is 125 DEG C, liquid-solid ratio 5, caustic sodium concentration 125g/L, extraction time
120min, with this condition, the dissolution rate of silica are 91.13%, and the alumina silica ratio of leached mud is 9.11.
Embodiment 2
Iron oxide in molar ratio: Alumina from Kaolin: carbon=2.4:4:1.2 carries out ingredient, pelletizing.It will be small after drying
Ball is placed in corundum crucible, is roasted in reducing atmosphere, and external application coke carries out atmosphere adjusting.1100 DEG C of maturing temperature,
Calcining time 60min；Gained roasting clinker is finely ground to d (0.5)=43.52 μm or so, using sodium hydroxide aqueous slkali to roasting
Overburnt material carries out alkali and soaks desiliconization, and extraction temperature is 110 DEG C, liquid-solid ratio 3, caustic sodium concentration 125g/L, extraction time
120min, with this condition, the dissolution rate of silica are 87.04%, and the alumina silica ratio of leached mud is 6.25.
Embodiment 3
Iron oxide in molar ratio: aluminium oxide in high silicon silicon-aluminum containing material: carbon=2.4:4:1.2 carries out ingredient, pelletizing.It will do
Bead after dry is placed in corundum crucible, is roasted in reducing atmosphere, and external application coke carries out atmosphere adjusting.Maturing temperature
1100 DEG C, calcining time 60min；Gained roasting clinker is finely ground to d (0.5)=28.52 μm or so, using sodium hydroxide alkali soluble
Liquid carries out alkali to roasting clinker and soaks desiliconization, and extraction temperature is 110 DEG C, liquid-solid ratio 10, caustic sodium concentration 125g/L, when leaching
Between 120min, with this condition, the dissolution rate of silica is 77%, and the alumina silica ratio of leached mud is 8.57.
Embodiment 4
Iron oxide in molar ratio: aluminium oxide in flyash: carbon=2.2:4:1.1 carries out ingredient, pelletizing.It will be small after drying
Ball is placed in corundum crucible, is roasted in reducing atmosphere, and external application coke carries out atmosphere adjusting.1100 DEG C of maturing temperature,
Calcining time 30min；Gained roasting clinker is finely ground to d (0.5)=30.15 μm or so, using sodium hydroxide aqueous slkali to roasting
Overburnt material carries out alkali and soaks desiliconization, and extraction temperature is 110 DEG C, liquid-solid ratio 10, caustic sodium concentration 125g/L, extraction time
180min, with this condition, the dissolution rate of silica are 96.09%, and the alumina silica ratio of leached mud is 24.18.
Embodiment 5
Iron oxide in molar ratio: aluminium oxide=2.2:4 carries out ingredient, pelletizing in gangue.Bead after drying is placed in
It in corundum crucible, is roasted in reducing atmosphere, external application coke carries out atmosphere adjusting.1100 DEG C of maturing temperature, when roasting
Between 30min；Gained roasting clinker is finely ground to d (0.5)=35.51 μm or so, using sodium hydroxide aqueous slkali to roasting clinker
It carries out alkali and soaks desiliconization, extraction temperature is 110 DEG C, liquid-solid ratio 8, caustic sodium concentration 125g/L, extraction time 180min.Herein
Under the conditions of, the dissolution rate of silica is 96.34%, and the alumina silica ratio of leached mud is 23.67.It is dense that available silica is dissolved out through multistage
Spending is 285g/L, the sodium silicate solution that modulus is 3.0, and leaching experiment result is shown in Table 2.
Table 2 roasts clinker multistage alkali and soaks desiliconization result
Leaching condition: 110 DEG C, solid-to-liquid ratio 10g/50mL, t=180min
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, it can also make several improvements and retouch, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of desilication method of silicon-aluminum containing material, which comprises the steps of:
1) it is uniformly mixed after taking ferriferous oxide, silicon-aluminum containing material and carbon dust to carry out ore matching, grinding, obtains raw material；
Wherein, iron oxide in ferriferous oxide, aluminium oxide in silicon-aluminum containing material, carbon molar ratio be 2~2.4:4:1~1.2；
2) raw material obtained by step 1) are roasted at 1050~1200 DEG C 30~60min, obtains clinker；
3) alkali in lye will be added after clinker milled processed obtained by step 2) to soak；
4) step 3) alkali is soaked gained ore pulp to be separated by solid-liquid separation, obtains siliceous lye and desiliconization slag.
2. the desilication method of silicon-aluminum containing material according to claim 1, which is characterized in that step 1) the silicon-aluminum containing material packet
Include kaolin, high silicon silicon-aluminum containing material, silicon-aluminum containing material milltailings, gangue or flyash.
3. the desilication method of silicon-aluminum containing material according to claim 1, which is characterized in that the step 2) roasting is to restore
It is carried out in property atmosphere.
4. the desilication method of silicon-aluminum containing material according to claim 1, which is characterized in that the step 3) milled processed is will
Clinker partial size is processed into d (0.5)≤45 μm of particle.
5. the desilication method of silicon-aluminum containing material according to claim 1, which is characterized in that the caustic alkali of the step 3) lye
Concentration is 100~150g/L.
6. the desilication method of silicon-aluminum containing material according to claim 1, which is characterized in that liquid-solid ratio is 3~10 in step 3).
7. the desilication method of silicon-aluminum containing material according to claim 1, which is characterized in that liquid-solid ratio is preferably 3 in step 3)
~5.
8. the desilication method of silicon-aluminum containing material according to claim 1, which is characterized in that step 3) the alkali leaching temperature is 95
~125 DEG C.
9. the desilication method of silicon-aluminum containing material according to claim 1, which is characterized in that step 3) the alkali leaching time is 60
~120min.
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| CN112095017A (en) * | 2020-09-15 | 2020-12-18 | 中南大学 | Method for recycling fly ash based on reduction roasting-acid leaching |
| CN113621819A (en) * | 2021-07-21 | 2021-11-09 | 广东邦普循环科技有限公司 | Method for extracting valuable metals from low nickel matte converter slag |
| CN116332633A (en) * | 2023-03-16 | 2023-06-27 | 北京科技大学 | Method for synthesizing fused mullite and fused corundum-mullite by taking gangue as raw material |
| CN117550617A (en) * | 2023-12-29 | 2024-02-13 | 安徽金岩高岭土新材料股份有限公司 | Technology for preparing mullite by taking coal-series kaolinite as raw material |
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| CN113621819A (en) * | 2021-07-21 | 2021-11-09 | 广东邦普循环科技有限公司 | Method for extracting valuable metals from low nickel matte converter slag |
| CN113621819B (en) * | 2021-07-21 | 2022-11-15 | 广东邦普循环科技有限公司 | Method for extracting valuable metals from low-grade nickel matte converter slag |
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| CN117550617A (en) * | 2023-12-29 | 2024-02-13 | 安徽金岩高岭土新材料股份有限公司 | Technology for preparing mullite by taking coal-series kaolinite as raw material |
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