CN104402007A - Technology for extracting silicon dioxide from Al2O3 extracted slag of fly ash - Google Patents

Technology for extracting silicon dioxide from Al2O3 extracted slag of fly ash Download PDF

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Publication number
CN104402007A
CN104402007A CN201410712130.8A CN201410712130A CN104402007A CN 104402007 A CN104402007 A CN 104402007A CN 201410712130 A CN201410712130 A CN 201410712130A CN 104402007 A CN104402007 A CN 104402007A
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China
Prior art keywords
sio
slag
solution
aluminum
silicon
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CN201410712130.8A
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Chinese (zh)
Inventor
张婷婷
雷绍民
张勋
张凤凯
徐腾
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XINYI TIANYUE QUARTZ Co Ltd
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XINYI TIANYUE QUARTZ Co Ltd
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Abstract

A technology for extracting silicon dioxide from Al2O3 extracted slag of fly ash comprises the step of cleaning the Al2O3 extracted slag of the fly ash obtained via an acid leaching reaction to be neutral, and further comprises the steps: (1) concentrated alkali leaching: mixing a slag cake and an NaOH solution for reaction for 80-120min at 110-120 DEG C, adding hot water to sufficiently dissolve generated Na2SiO3 into a sodium silicate solution, obtaining an Na2SiO3 solution and alkaline leaching reaction residue after filtration and separation, (2) carbonation and ferrum removal: carbonating the Na2SiO3 solution to form a precipitate SiO2, cleaning SiO2 with HCl at a concentration of 5-30% to remove ferrum from SiO2, then cleaning with distilled water to be neutral to form SiO2 with upper purity, (3) low-temperature drying: drying SiO2 after the ferrum removal for a certain time at 70 DEG C to form SiO2 powder with a particle size of about 10 micrometers, and (4) causticization: causticizing an Na2CO3 solution formed by carbonating the Na2SiO3 solution with CaO, and allowing generated CO2 gas to return to the carbonation technology and CaO to return to the causticization technology.

Description

A kind of technique extracting silicon-dioxide from aluminum-extracted pulverized fuel ash slag
Technical field
The present invention relates to a kind of silicon-dioxide extracting method, particularly relate to a kind of method extracting silicon-dioxide from aluminum-extracted pulverized fuel ash slag.
Background technology
Flyash is the solid waste of power station discharge, is one of maximum source of pollution of society.In flyash, aluminium, silicone content are very high, if by simple technique, aluminium in extract powder coal ash, both can solve a large amount of flyash and pile up the pollution problem brought, and flyash can have been made again to turn waste into wealth, become a kind of secondary resource of cheapness.Aluminum oxide in extract powder coal ash and silicon-dioxide not only have good environmental benefit and social benefit, and are feasible technically.But at present can whole extraction and isolation to the aluminum oxide in flyash and silicon-dioxide, the aluminum oxide of generation high added value and the technique of silica product also few.
After particularly flyash extracts aluminum oxide, residue waste residue is close to 60% of powdered coal ash, wherein dioxide-containing silica is up to 85%, in prior art, proposes flyash acid system and puies forward the technique that aluminium slag directly prepares cement, although industrial feasible, but this technique not only deficiency in economic performance, added value of product is low, and due to output large, locality cannot all utilize, and thus can not realize the comprehensive utilization of flyash high added value.
Summary of the invention
For overcoming the deficiencies in the prior art, the object of the present invention is to provide a kind of wet-leaching technique, because in slag after aluminum-extracted pulverized fuel ash, dioxide-containing silica is higher, two-step approach can be taked, first prepare water glass, and then silicon powder product is prepared in reprocessing, be intended to the silicon powder product producing variation, added value is high, economic worth good, the market competitiveness is large, a new road is opened up in the comprehensive utilization that becomes more meticulous for flyash.
For achieving the above object, the present invention is achieved through the following technical solutions: a blob of slag (aluminum-extracted pulverized fuel ash slag) cleaning remaining after acid-leaching reaction being extracted from flyash aluminum oxide is extremely neutral, for the preparation of SiO 2product, also comprises following technical process:
(1) concentrated base leaches: after the NaOH solution being 40% ~ 60% by a described blob of slag and concentration mixes, wherein, the solid-to-liquid ratio of a described blob of slag and NaOH solution is 100 ~ 200 weight parts: 1000ml, 110 dEG Creact 80 ~ 120min at ~ 120 DEG C, then add the Na that hot water makes generation 2siO 3abundant dissolving forms sodium silicate solution, can obtain Na after filtering separation 2siO 3solution and alkali leaching reaction recrement;
(2) carbon divide, deironing: carbon divides described Na 2siO 3solution, is precipitated SiO 2, this precipitates SiO 2middle iron level is higher, cleans SiO with the HCl that concentration is 5% ~ 30% 2removing iron wherein, then cleans SiO with distilled water 2to neutral, the SiO that purity is higher can be obtained 2;
(3) cryodrying: by the SiO after deironing 2in lower than 70 dEG Clower dry certain hour, can obtain the SiO that particle diameter is about about 10 μm 2powder;
(4) causticization: the Na obtained after sodium silicate solution carbon is divided 2cO 3solution CaO causticization, generates NaOH solution and CaCO 3precipitation, returns concentrated base extract technology after the NaOH solution evaporation concentration of generation, the CaCO of generation 3precipitate after Roasting Decomposition, the CO of generation 2gas returns carbonation decompsition process, and CaO returns causticization process.
Preferably, the described technique extracting silicon-dioxide from aluminum-extracted pulverized fuel ash slag, wherein, described alkali leaching reaction recrement returns Leaching by strong acid curing technique.
Preferably, the described technique extracting silicon-dioxide from aluminum-extracted pulverized fuel ash slag, wherein, described carbon divides takes secondary carbon method, makes the precipitated silica purity that obtains higher.
Preferably, the described technique extracting silicon-dioxide from aluminum-extracted pulverized fuel ash slag, wherein, described SiO 2siO in powder 2content>=99.75%.
Preferably, the described technique extracting silicon-dioxide from aluminum-extracted pulverized fuel ash slag, wherein, described causticization temperature is 75 ~ 80 dEG C, the time is 5 ~ 15min, CaO 2add-on is CaO 2: Na 2siO 3=1 ~ 1.2: 1.
Preferably, the described technique extracting silicon-dioxide from aluminum-extracted pulverized fuel ash slag, wherein, described blob of slag cleaning is to neutrality, with the HCl solution stirring reaction certain hour that concentration is 5% ~ 30%, except iron a large amount of in removing slag, then cleaning is to neutral, drying can obtain silicon powder, SiO in described silicon powder 2content>=99.55%.
Beneficial effect of the present invention: the discharge of (1) flyash causes very large pollution and harm to environment, with aluminum-extracted pulverized fuel ash slag for raw material prepares silicon powder and silicon-dioxide, reach and economize on resources, the object of turning bane into boon, in production process, achieve the discharge of contamination-free; (2) silicon powder prepared is mainly used in the industry of silicon rubber and does reinforcing filler, in addition, also can be used as the additive of paint, coating; The high-purity silicon dioxide prepared, as a kind of industrial raw material of basis, can be widely used in microelectronics, photoelectron, advanced ceramic, coating, medicine and other fields.(3) technique Raw realizes recycle, and acid consumption, alkaline consumption are low, and waste sludge discharge amount is low, all takes effective circulation treatment measure, meet the requirement of national development recycling economy to water, gas, various pollutent.
Embodiment
The present invention is described in further detail below, can implement according to this with reference to specification sheets word to make those skilled in the art.
Embodiment 1:
A blob of slag (aluminum-extracted pulverized fuel ash slag) cleaning remaining after acid-leaching reaction being extracted from flyash aluminum oxide is extremely neutral, for the preparation of SiO 2product, also comprises following technical process:
(1) concentrated base leaches: carry after NaOH solution 1000ml that an aluminium blob of slag 100 weight part and concentration are 40% mixes described in getting, react 90min, then add the Na that hot water makes generation at 110 DEG C 2siO 3abundant dissolving forms sodium silicate solution, can obtain Na after filtering separation 2siO 3solution and alkali leaching reaction recrement;
(2) carbon divide, deironing: take secondary carbon method, carbon divides described Na 2siO 3solution, make the precipitated silica purity that obtains higher, this precipitates SiO 2middle iron level is higher, cleans SiO with the HCl that concentration is 5% 2removing iron wherein, then cleans SiO with distilled water 2to neutral, the SiO that purity is higher can be obtained 2;
(3) cryodrying: by the SiO after deironing 2dry certain hour at lower than 70 DEG C, can obtain the SiO that particle diameter is about about 10 μm 2powder, the SiO obtained 2siO in powder 2content is 99.78%.
(4) causticization: the Na obtained after sodium silicate solution carbon is divided 2cO 3solution CaO causticization, causticization temperature is 75 DEG C, and the time is 15min, CaO 2add-on is CaO 2: Na 2siO 3=1: 1, generate NaOH solution and CaCO 3precipitation, returns concentrated base extract technology after the NaOH solution evaporation concentration of generation, the CaCO of generation 3precipitate after Roasting Decomposition, the CO of generation 2gas returns carbonation decompsition process, and CaO returns causticization process.
Embodiment 2:
A blob of slag (aluminum-extracted pulverized fuel ash slag) cleaning remaining after acid-leaching reaction being extracted from flyash aluminum oxide is extremely neutral, for the preparation of SiO 2product, can also comprise following technical process:
(1) concentrated base leaches: carry after NaOH solution 1000ml that an aluminium blob of slag 150 weight part and concentration are 50% mixes described in getting, react 80min, then add the Na that hot water makes generation at 120 DEG C 2siO 3abundant dissolving forms sodium silicate solution, can obtain Na after filtering separation 2siO 3solution and alkali leaching reaction recrement;
(2) carbon divide, deironing: take secondary carbon method, carbon divides described Na 2siO 3solution, make the precipitated silica purity that obtains higher, this precipitates SiO 2middle iron level is higher, cleans SiO with the HCl that concentration is 15% 2removing iron wherein, then cleans SiO with distilled water 2to neutral, the SiO that purity is higher can be obtained 2;
(3) cryodrying: by the SiO after deironing 2lower than less than 60 DEG C dry certain hours, the SiO that particle diameter is about about 12 μm can be obtained 2powder, the SiO obtained 2siO in powder 2content is 99.85%.
(4) causticization: the Na obtained after sodium silicate solution carbon is divided 2cO 3solution CaO causticization, causticization temperature is 80 dEG C, the time is 10min, CaO 2add-on is CaO 2: Na 2siO 3=1.1: 1, generate NaOH solution and CaCO 3precipitation, returns concentrated base extract technology after the NaOH solution evaporation concentration of generation, the CaCO of generation 3precipitate after Roasting Decomposition, the CO of generation 2gas returns carbonation decompsition process, and CaO returns causticization process.
Embodiment 3:
A blob of slag (aluminum-extracted pulverized fuel ash slag) cleaning remaining after acid-leaching reaction being extracted from flyash aluminum oxide is extremely neutral, for the preparation of SiO 2product, can also comprise following technical process:
(1) concentrated base leaches: carry after NaOH solution 1000ml that an aluminium blob of slag 200 weight part and concentration are 60% mixes described in getting, react 120min, then add the Na that hot water makes generation at 115 DEG C 2siO 3abundant dissolving forms sodium silicate solution, can obtain Na after filtering separation 2siO 3solution and alkali leaching reaction recrement;
(2) carbon divide, deironing: take secondary carbon method, carbon divides described Na 2siO 3solution, make the precipitated silica purity that obtains higher, this precipitates SiO 2middle iron level is higher, cleans SiO with the HCl that concentration is 30% 2removing iron wherein, then cleans SiO with distilled water 2to neutral, the SiO that purity is higher can be obtained 2;
(3) cryodrying: by the SiO after deironing 2lower than 70 dEG Cfollowing dry certain hour, can obtain the SiO that particle diameter is about about 15 μm 2powder, the SiO obtained 2siO in powder 2content is 99.85%.
(4) causticization: the Na obtained after sodium silicate solution carbon is divided 2cO 3solution CaO causticization, causticization temperature is 80 dEG C, the time is 15min, CaO 2add-on is CaO 2: Na 2siO 3=1.2: 1, generate NaOH solution and CaCO 3precipitation, returns concentrated base extract technology after the NaOH solution evaporation concentration of generation, the CaCO of generation 3precipitate after Roasting Decomposition, the CO of generation 2gas returns carbonation decompsition process, and CaO returns causticization process.
Embodiment 4:
The present invention can also comprise following distortion, and to prepare silicon powder, described blob of slag cleaning is to neutrality, with the HCl solution stirring reaction certain hour that concentration is 25%, except iron a large amount of in removing slag, then cleaning is to neutral, drying can obtain silicon powder, SiO in described silicon powder 2content>=99.55%.
Although embodiment of the present invention are open as above, but it is not restricted to listed in specification sheets and embodiment utilization, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and shown here embodiment.

Claims (6)

1. from aluminum-extracted pulverized fuel ash slag, extract a technique for silicon-dioxide, it is characterized in that, a blob of slag (aluminum-extracted pulverized fuel ash slag) cleaning remaining after acid-leaching reaction being extracted from flyash aluminum oxide is extremely neutral, for the preparation of SiO 2product, also comprises following technical process:
(1) concentrated base leaches: after being mixed with 40% ~ 60% concentration NaOH solution by a described blob of slag, wherein, the solid-to-liquid ratio of a described blob of slag and NaOH solution is 100 ~ 200 weight parts: 1000ml, reacts 80 ~ 120min, then add the Na that hot water makes generation at 110 DEG C ~ 120 DEG C 2siO 3abundant dissolving forms sodium silicate solution, can obtain Na after filtering separation 2siO 3solution and alkali leaching reaction recrement;
(2) carbon divide, deironing: carbon divides described Na 2siO 3solution, is precipitated SiO 2, this precipitates SiO 2middle iron level is higher, cleans SiO with the HCl that concentration is 5% ~ 30% 2removing iron wherein, then cleans SiO with distilled water 2to neutral, the SiO that purity is higher can be obtained 2;
(3) cryodrying: by the SiO after deironing 2dry certain hour at lower than 70 DEG C, can obtain the SiO that particle diameter is about about 10 μm 2powder;
(4) causticization: the Na obtained after sodium silicate solution carbon is divided 2cO 3solution CaO causticization, generates NaOH solution and CaCO 3precipitation, returns concentrated base extract technology after the NaOH solution evaporation concentration of generation, the CaCO of generation 3precipitate after Roasting Decomposition, the CO of generation 2gas returns carbonation decompsition process, and CaO returns causticization process.
2. from aluminum-extracted pulverized fuel ash slag, extract the technique of silicon-dioxide as claimed in claim 1, it is characterized in that, described alkali leaching reaction recrement returns Leaching by strong acid curing technique.
3. from aluminum-extracted pulverized fuel ash slag, extract the technique of silicon-dioxide as claimed in claim 2, it is characterized in that, described carbon divides takes secondary carbon method.
4. from aluminum-extracted pulverized fuel ash slag, extract the technique of silicon-dioxide as claimed in claim 3, it is characterized in that, described SiO 2siO in powder 2content>=99.75%.
5. from aluminum-extracted pulverized fuel ash slag, extract the technique of silicon-dioxide as claimed in claim 4, it is characterized in that, described causticization temperature is 75 ~ 80 DEG C, and the time is 5 ~ 15min, CaO 2add-on is CaO 2: Na 2siO 3=1 ~ 1.2: 1.
6. from aluminum-extracted pulverized fuel ash slag, extract the technique of silicon-dioxide as claimed in claim 5, it is characterized in that, described blob of slag cleaning is to neutrality, with the HCl solution stirring reaction certain hour that concentration is 5% ~ 30%, except iron a large amount of in removing slag, then cleaning is to neutral, and drying can obtain silicon powder, SiO in described silicon powder 2content>=99.55%.
CN201410712130.8A 2014-11-28 2014-11-28 Technology for extracting silicon dioxide from Al2O3 extracted slag of fly ash Pending CN104402007A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100119426A1 (en) * 2007-04-03 2010-05-13 Qin Jinguo Process for recovery of silica followed by alumina from coal fly ash
CN101734698A (en) * 2009-09-08 2010-06-16 东北大学 Method for preparing aluminum oxide from aluminiferous material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100119426A1 (en) * 2007-04-03 2010-05-13 Qin Jinguo Process for recovery of silica followed by alumina from coal fly ash
CN101734698A (en) * 2009-09-08 2010-06-16 东北大学 Method for preparing aluminum oxide from aluminiferous material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
吴艳: "从粉煤灰中提取氧化铝和二氧化硅的研究", 《中国学位论文全文数据库》 *
吴艳: "从粉煤灰中提取氧化铝和二氧化硅的研究", 《中国学位论文全文数据库》, 30 June 2011 (2011-06-30), pages 64 - 113 *

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Application publication date: 20150311