CN104591196A - Strengthening method for high-alumina fly ash alkali-soluble pre-desiliconization - Google Patents

Strengthening method for high-alumina fly ash alkali-soluble pre-desiliconization Download PDF

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CN104591196A
CN104591196A CN201410801107.6A CN201410801107A CN104591196A CN 104591196 A CN104591196 A CN 104591196A CN 201410801107 A CN201410801107 A CN 201410801107A CN 104591196 A CN104591196 A CN 104591196A
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desiliconizing
aluminous fly
ash alkali
enhancement method
described step
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CN104591196B (en
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荆富
彭志宏
郭新院
齐天贵
商兆会
刘桂华
饶拴民
周秋生
李红英
李小斌
樊红亮
孙文迁
王磊
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CHINA COAL PINGSHUO GROUP CO LTD
Central South University
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CHINA COAL PINGSHUO GROUP CO LTD
Central South University
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Abstract

The invention discloses a strengthening method for high-alumina fly ash alkali-soluble pre-desiliconization. The method comprises the following steps: (1) preparing a NaOH water solution with certain concentration; (2) proportioning the NaOH water solution, fly ashes and an additive in a low-pressure reaction kettle according to a proper ratio reacting in a low-pressure reaction kettle; and (3) carrying out liquid-solid separation on the reacted slurry to obtain a sodium silicate solution and desiliconized slag. By virtue of the strengthening method disclosed by the invention, the problems of high alkali liquor amount and low silicon dioxide dissolution rate in an existing high-alumina fly ash alkali-soluble pre-desiliconization process can be overcome; and the silicon dioxide dissolution rate can be greatly improved, so that the economic benefits of comprehensive utilization of overall fly ashes are significantly improved.

Description

The enhancement method of the molten pre-desiliconizing of a kind of aluminous fly-ash alkali
Technical field
The present invention relates to resource and environment filed, particularly the enhancement method of the molten pre-desiliconizing of a kind of aluminous fly-ash alkali.
Background technology
The ground such as China Shanxi, Inner Mongol discharge and store up a large amount of aluminous fly-ash, not only waste valuable containing aluminium, containing silicon resource, and land occupation, contaminate environment, is detrimental to health.Therefore, comprehensive utilization of resources aluminous fly-ash has great importance.
It is the most promising technological line of current comprehensive utilization of resources aluminous fly-ash that pre-desiliconizing extracts white carbon black-sintering process extraction aluminum oxide, this technological line is first mixed at a certain temperature with alkaline solution by aluminous fly-ash, carry out pre-desiliconizing reaction, the part SiO in stripping aluminous fly-ash 2, after solid-liquid separation, obtain sodium silicate solution and desiliconization slag, sodium silicate solution is for the preparation of white carbon black or Calucium Silicate powder, and desiliconization slag then adopts sintering process to produce Al 2o 3.
Around the pre-desilicification process of aluminous fly-ash, related researcher has carried out a large amount of research work.Li Junqi etc. (alkaline process is to the pre-desiliconizing process [J] of flyash. light metal, 2010(11): 11-13) have studied aluminous fly-ash is reacted 2h under 90 DEG C of conditions, concentration of sodium hydroxide solution 30%, liquid-solid ratio is 30:1, pre-desiliconizing rate is 58%, but the alkali concn of this technology is too high, liquid-solid ratio is too large, without practicality.Wu Guodong etc. (in the molten flyash of low-temperature alkaline, the stripping law of Silicified breccias studies [J]. Research of Environmental Sciences, 2006,19 (1): 53-56.) first under 950 DEG C of conditions, pre-treatment has been carried out to aluminous fly-ash, then stripping 4-6h in the sodium hydroxide solution of 2-3 mol/L, temperature of reaction is 120-130 DEG C, and the solubility rate of silicon-dioxide is 29.23%.Du Zichuan etc. (aluminous fly-ash alkali solution-off silicon process reaction mechanism [J]. process engineering journal .2011,11 (3): 442-446.) aluminous fly-ash is reacted 2 h in 130 DEG C of alkaline solutions, SiO 2solubility rate 42.5%; If when temperature is higher than 130 DEG C, the formation of sodalite can aggravate, and causes silicon-dioxide solubility rate to reduce.Zhang Zhanjun etc. (extract amorphous Si O from aluminous fly-ash 2experimental study [J]. mineral journal, 2007,27 (2): 137-142.) have studied the silicon-dioxide extracted in sodium hydroxide solution in aluminous fly-ash, Optimizing Technical is: concentration of sodium hydroxide solution is 25%, at 95 DEG C of temperature, stripping reacts 4 hours, and the solubility rate of gained silicon-dioxide is 41.8%.
This technology at present in the molten temperature of reaction of the alkali in pre-desiliconizing stage below 130 DEG C, the subject matter of existence is that caustic is large; In flyash, silicon-dioxide solubility rate is lower, only has 40 ~ 44%, causes desiliconization slag alumina silica ratio low, A/S only about 1.6, thus badly influences the organization of production of subsequent oxidation aluminium abstraction process, worsens the technico-economical comparison of alumina producing.In the alumina extraction stage, in order to realize desilication, need by adding lime (CaO), by SiO 2be transformed into not containing Al 2o 3and Na 2calcium orthosilicate (the 2CaOSiO of O 2), in flyash, silicone content is higher, and alumina silica ratio is lower, and lime-crushed stone pile is larger, aluminum oxide production process mass flow and red mud quantum of output also larger.In order to optimize aluminum oxide production process technico-economical comparison, promote the sound development of whole total utilization of PCA project, in the urgent need to increasing substantially the silicon-dioxide solubility rate of the molten pre-desilicification process of coal ash alkali, improve the alumina silica ratio of flyash (i.e. desiliconization slag) after pre-desiliconizing as far as possible simultaneously.
Summary of the invention
The technical problem to be solved in the present invention overcomes the deficiencies in the prior art, provides the molten pre-desiliconizing enhancement method of coal ash alkali that a kind of processing step is simple, alkali lye consumption is little, silicon-dioxide solubility rate is high, desiliconization slag alumina silica ratio is high, easily combine with pre existing desiliconization production process.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is:
An enhancement method for the molten pre-desiliconizing of aluminous fly-ash alkali, comprises the following steps:
(1) the certain density NaOH aqueous solution is allocated;
(2) flyash added in the NaOH aqueous solution that step (1) allocates by certain liquid-solid ratio, then after adding certain additive mixing, be placed in low pressure reaction still together and react;
(3) solid-liquor separation is carried out to step (2) reacted slurries, obtain sodium silicate solution and desiliconization slag.
Further improvement as to technique scheme:
In described step (1), the concentration of the NaOH aqueous solution is with Na 2o meter controls at 150 ~ 200g/L.
In described step (2), the liquid-solid ratio of the NaOH aqueous solution and flyash is 5:1 ~ 10:1.
In described step (2), institute's doping is the one in glucose, EDTA and Sodium Fluoride, and the consumption of described additive counts 1 ~ 5g/L by stripping volume.
In described step (2), described reaction is stirred at temperature 130 DEG C ~ 150 DEG C; Reaction times is 5min ~ 60min.
In described step (3), carrying out solid-liquor separation to described slurries is adopt centrifugation or filtering under pressure, sharp separation.
In described step (3), the sodium silicate solution obtained after solid-liquor separation is for the production of white carbon black, and desiliconization slag is used for sintering process and extracts aluminum oxide.
According to research, in order to improve the silicon-dioxide solubility rate of the molten pre-desilicification process of alkali, and ensure that aluminum oxide is not dissolved as far as possible, the factors such as such as temperature of reaction, reaction times, liquid-solid ratio, additive types and addition all mutually can restrict, influence each other, need these processing parameters and the solid-liquor separation time that control the molten process of alkali well, the realization of aforementioned object can be ensured better.
Above-mentioned enhancement method of the present invention is mainly based on following technical thought: the reaction of aluminous fly-ash in sodium hydroxide solution comprises the molten reaction of alkali of amorphous vitreum and mullite, glass state material dissolves very fast, form water glass, after this along with the prolongation in reaction times, mullite also can dissolve gradually, aluminum oxide enters solution and generates sodium aluminate, and then with water glass in conjunction with precipitated sodium white residue, causes silicon-dioxide solubility rate to decline thus; Temperature raises, and the reaction molten with alkali of usual amorphous vitreum and mullite all can be strengthened, and mullite enters into the aluminum oxide of solution not only bad for white carbon black production after reacting, and silicon-dioxide solubility rate can be caused to decline on the contrary.Technical thought of the present invention is the molten process kinetics of alkali of regulation and control flyash, and by adding additive, while promotion amorphous glass body dissolves, suppresses the dissolving of mullite, enters alkaline solution, avoid the generation of Sodium-silica slag to reduce aluminum oxide as far as possible.
Compared to existing technology, the present invention has the following advantages:
1) enhancement method of the molten pre-desiliconizing of aluminous fly-ash alkali of the present invention, technique is simple, alkali lye consumption is little, by adding additive, and the kinetics of regulation and control reaction, while promotion amorphous glass body dissolves, the dissolving of mullite can be suppressed, enter alkaline solution to reduce aluminum oxide as far as possible, avoid the generation of Sodium-silica slag, the solubility rate of silicon-dioxide in the molten pre-desilicification process of alkali can be increased substantially, bring up to 55 ~ 60% from present 40 ~ 44%;
2) the desiliconization slag alumina silica ratio obtained by the enhancement method of the molten pre-desiliconizing of aluminous fly-ash alkali of the present invention can bring up to more than 2.0, thus mass flow and the red mud quantum of output that follow-up sintering method extracts alumina process can be reduced, significantly improve the economic benefit of whole utilization of fly ash.
Embodiment
For the ease of understanding the present invention, hereafter will do to describe more comprehensively, meticulously to the present invention in conjunction with preferred embodiment, but protection scope of the present invention is not limited to following specific embodiment.
Embodiment 1
Select and consist of SiO 248%, Al 2o 3the flyash of 42%, A/S 0.875, compound concentration is Na 2the alkali lye (the NaOH aqueous solution) of O 150g/L, be that flyash joins in alkali lye by 10:1 by liquid-solid ratio, add glucose 1g/L by volume, mixing, be placed in low pressure reaction still together and carry out stirring reaction at 130 DEG C of temperature, the time is 10min, again fast filtering separation is carried out to gained slurries, obtain sodium silicate solution and desiliconization slag, the A/S of desiliconization slag is 2.01, and silicon-dioxide solubility rate is 55.55%.The sodium silicate solution obtained after solid-liquor separation is for the production of white carbon black, and desiliconization slag is used for sintering process and extracts aluminum oxide.
Embodiment 2
Select and consist of SiO 248%, Al 2o 3the flyash of 42%, A/S 0.875, compound concentration is Na 2the alkali lye (the NaOH aqueous solution) of O 200g/L, be that flyash joins in alkali lye by 10:1 by liquid-solid ratio, add EDTA 2g/L by volume, mixing, be placed in low pressure reaction still together and carry out stirring reaction at 140 DEG C of temperature, the time is 20min, again quick centrifugation is carried out to gained slurries, obtain sodium silicate solution and desiliconization slag, the A/S of desiliconization slag is 2.09, and silicon-dioxide solubility rate is 57.42%.The sodium silicate solution obtained after solid-liquor separation is for the production of white carbon black, and desiliconization slag is used for sintering process and extracts aluminum oxide.
Embodiment 3
Select and consist of SiO 248%, Al 2o 3the flyash of 42%, A/S 0.875, compound concentration is Na 2the alkali lye (the NaOH aqueous solution) of O 170g/L, be that flyash joins in alkali lye by 5:1 by liquid-solid ratio, add Sodium Fluoride 5g/L by volume, mixing, be placed in low pressure reaction still together and carry out stirring reaction at 150 DEG C of temperature, the time is 5min, again the separation of sheet frame fast press-filtration is carried out to gained slurries, obtain sodium silicate solution and desiliconization slag, the A/S of desiliconization slag is 2.12, and silicon-dioxide solubility rate is 59.56%.The sodium silicate solution obtained after solid-liquor separation is for the production of white carbon black, and desiliconization slag is used for sintering process and extracts aluminum oxide.
Embodiment 4
Select and consist of SiO 249%, Al 2o 3the flyash of 40.5%, A/S 0.827, compound concentration is Na 2the alkali lye (the NaOH aqueous solution) of O 150g/L, be that flyash joins in alkali lye by 8:1 by liquid-solid ratio, add glucose 2g/L by volume, mixing, be placed in low pressure reaction still together and carry out stirring reaction at 130 DEG C of temperature, the time is 60min, again fast filtering separation is carried out to gained slurries, obtain sodium silicate solution and desiliconization slag, the A/S of desiliconization slag is 1.96, and silicon-dioxide solubility rate is 55.07%.The sodium silicate solution obtained after solid-liquor separation is for the production of white carbon black, and desiliconization slag is used for sintering process and extracts aluminum oxide.
Embodiment 5
Select and consist of SiO 249%, Al 2o 3the flyash of 40.5%, A/S 0.827, compound concentration is Na 2the alkali lye (the NaOH aqueous solution) of O 160g/L, be that flyash joins in alkali lye by 10:1 by liquid-solid ratio, add Sodium Fluoride 1g/L by volume, mixing, be placed in low pressure reaction still stirring reaction at 150 DEG C of temperature together, the time is 10min, again quick centrifugation is carried out to gained slurries, obtain sodium silicate solution and desiliconization slag, the A/S of desiliconization slag is 1.99, and silicon-dioxide solubility rate is 56.15%.
Embodiment 6
Select and consist of SiO 249%, Al 2o 3the flyash of 40.5%, A/S 0.827, compound concentration is Na 2the alkali lye (the NaOH aqueous solution) of O 180g/L, be that flyash joins in alkali lye by 7:1 by liquid-solid ratio, add EDTA 4g/L by volume, mixing, be placed in low pressure reaction still stirring reaction at 130 DEG C of temperature together, the time is 20min, again fast filtering separation is carried out to gained slurries, obtain sodium silicate solution and desiliconization slag, the A/S of desiliconization slag is 2.13, and silicon-dioxide solubility rate is 59.78%.

Claims (7)

1. an enhancement method for the molten pre-desiliconizing of aluminous fly-ash alkali, comprises the following steps:
(1) the certain density NaOH aqueous solution is allocated;
(2) flyash added in the NaOH aqueous solution that step (1) allocates by certain liquid-solid ratio, then after adding certain additive mixing, be placed in low pressure reaction still together and react;
(3) solid-liquor separation is carried out to step (2) reacted slurries, obtain sodium silicate solution and desiliconization slag.
2. the enhancement method of the molten pre-desiliconizing of aluminous fly-ash alkali according to claim 1, is characterized in that, in described step (1), the concentration of the NaOH aqueous solution is with Na 2o meter controls at 150 ~ 200g/L.
3. the enhancement method of the molten pre-desiliconizing of aluminous fly-ash alkali according to claim 1, is characterized in that, in described step (2), the liquid-solid ratio of the NaOH aqueous solution and flyash is 5:1 ~ 10:1.
4. the enhancement method of the molten pre-desiliconizing of aluminous fly-ash alkali according to claim 1, is characterized in that, in described step (2), institute's doping is the one in glucose, EDTA and Sodium Fluoride, and the consumption of described additive counts 1 ~ 5g/L by stripping volume.
5. the enhancement method of the molten pre-desiliconizing of aluminous fly-ash alkali according to claim 1, is characterized in that, in described step (2), described reaction is stirred at temperature 130 DEG C ~ 150 DEG C; Reaction times is 5min ~ 60min.
6. the enhancement method of the molten pre-desiliconizing of aluminous fly-ash alkali according to claim 1, is characterized in that, in described step (3), carrying out solid-liquor separation to described slurries is adopt centrifugation or filtering under pressure, sharp separation.
7. the enhancement method of the molten pre-desiliconizing of aluminous fly-ash alkali according to claim 1, is characterized in that, in described step (3), the sodium silicate solution obtained after solid-liquor separation is for the production of white carbon black, and desiliconization slag is used for sintering process and extracts aluminum oxide.
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Cited By (5)

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CN105621428A (en) * 2016-01-29 2016-06-01 卓达新材料科技集团有限公司 Method for preparing sodium silicate by using common pulverized fuel ash from pulverized coal furnace
CN108421526A (en) * 2018-03-16 2018-08-21 锡林郭勒职业学院 A kind of two step of hydro-thermal/acidleach prepares method and the application of flyash defluorinating agent
CN109319792A (en) * 2018-11-08 2019-02-12 渤海大学 A kind of method that high added value comprehensively utilizes silicon, aluminium, potassium in potash feldspar ore
CN110935717A (en) * 2019-12-16 2020-03-31 金海华 Modification method of high-alumina fly ash
DE112021000399T5 (en) 2020-08-26 2022-11-17 Huaneng Clean Energy Research Institute Process for deep desiliconization of fly ash and recovery of silicon resources

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CN103318930A (en) * 2013-06-27 2013-09-25 中国铝业股份有限公司 Comprehensive utilization method and device of high iron bauxite
CN103352125A (en) * 2013-07-01 2013-10-16 金川集团股份有限公司 Method for high-efficiently enriching gold and platinum metal from complex low-grade chlorine soaked slag

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CN101780374A (en) * 2010-04-01 2010-07-21 史汉祥 Synchronized dust removal and desulfuration for smoke of coal-fired boiler and comprehensive utilization of flyash of coal-fired boiler
CN102923745A (en) * 2012-12-07 2013-02-13 昆明冶金研究院 Method for removing silicon and iron from sodium aluminate solution
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105621428A (en) * 2016-01-29 2016-06-01 卓达新材料科技集团有限公司 Method for preparing sodium silicate by using common pulverized fuel ash from pulverized coal furnace
CN108421526A (en) * 2018-03-16 2018-08-21 锡林郭勒职业学院 A kind of two step of hydro-thermal/acidleach prepares method and the application of flyash defluorinating agent
CN108421526B (en) * 2018-03-16 2021-03-26 锡林郭勒职业学院 Method for preparing fly ash defluorinating agent by hydrothermal/acid leaching in two steps and application
CN109319792A (en) * 2018-11-08 2019-02-12 渤海大学 A kind of method that high added value comprehensively utilizes silicon, aluminium, potassium in potash feldspar ore
CN110935717A (en) * 2019-12-16 2020-03-31 金海华 Modification method of high-alumina fly ash
CN110935717B (en) * 2019-12-16 2022-09-27 安徽省繁昌县金狮粉磨有限责任公司 Modification method of high-alumina fly ash
DE112021000399T5 (en) 2020-08-26 2022-11-17 Huaneng Clean Energy Research Institute Process for deep desiliconization of fly ash and recovery of silicon resources

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