CN105776270B - The preparation method of nano-aluminum hydroxide in a kind of pelite - Google Patents
The preparation method of nano-aluminum hydroxide in a kind of pelite Download PDFInfo
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- CN105776270B CN105776270B CN201610275569.8A CN201610275569A CN105776270B CN 105776270 B CN105776270 B CN 105776270B CN 201610275569 A CN201610275569 A CN 201610275569A CN 105776270 B CN105776270 B CN 105776270B
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- pelite
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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
- C01F7/20—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts
- C01F7/24—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts with nitric acid or nitrogen oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of preparation method of nano-aluminum hydroxide in pelite, pelite is levigate to below 74um, mixed by a certain percentage with certain density hydrochloric acid with nitric acid after drying again, mechanical agitation in water-bath is placed in leach, control extraction time, temperature, leachate cooled and filtered, gained filtrate is slowly added to sodium hydroxide solution regulation pH removal of impurities, pure aluminium salt is obtained after step-wise filtration, aluminum hydroxide precipitation is obtained after being passed through CO2 again, nano-aluminum hydroxide product is dried to obtain after filter washing.The preparation method preparation efficiency of the present invention is high, leach thorough, yield and utilization rate are high, and purity is high, and pelite is leached by the method hydrochloric acid and nitric acid mixed liquor of the present invention, by removal of impurities, the process such as purification, purification, can obtain the preferable nano-aluminum hydroxide powder of quality, preferable economic benefit can be obtained, while is again comprehensively utilized pelite resource.
Description
Technical field
The invention belongs to nano-aluminum hydroxide Preparation Technique of Powders field in pelite, is related to nanometer hydrogen in a kind of pelite
The preparation method of aluminum oxide.
Background technology
Pelite is the hydroxide containing aluminium, and China's pelite mainly contains diaspore and clay mineral symbiosis, in addition
Also containing siliceous and anatase etc..And as scarcity of resources aggravation and the reinforcement of people's environmental consciousness, pelite comprehensive utilization are got over
Widely paid close attention to get over.Essential mineral is diaspore and clay mineral in pelite, containing it is higher be Al2O3, utilize
Pelite cleans and can obtain nano-aluminum hydroxide powder again after being leached with nitration mixture, and gained nano-aluminum hydroxide powder can be widely used for
Various fire retardants and inorganic filler etc..
Nano-aluminum hydroxide is mainly prepared using solid phase method, vapor phase method and liquid phase method at present, but solid phase method needs very
High temperature, therefore equipment requirement is high, equipment purchase cost is expensive；Liquid phase method is the conventional side for preparing nano-aluminum hydroxide powder
Method, but liquid phase method is readily incorporated new impurity, causes the nano-aluminum hydroxide purity of preparation not high；And vapor phase method, when collecting
It is difficult to collect and low yield.
The content of the invention
The technical problem to be solved in the present invention is：A kind of preparation method of nano-aluminum hydroxide in pelite is provided, prepared
Efficiency high, leach thoroughly, yield and utilization rate are high, and purity is high, and preparation is simple, and preparation cost is low, to solve to deposit in the prior art
The problem of.
The technical scheme that the present invention takes is：
The preparation method of nano-aluminum hydroxide, this method comprise the following steps in a kind of pelite：
（1）Using pelite as raw material, after it is used into jaw crushing crusher machine, then the miberal powder particle mill that will be crushed with ball mill
Below granulation degree 74um；
（2）By step（1）In grind miberal powder sample drying after, by the mixed solution of hydrochloric acid and nitric acid with drying miberal powder
It is placed in water-bath and stirs in proportion, leaching involved chemical reaction has：
Al2O3+6HCl=2AlCl3+3H2O
Al2O3+6HNO3=2Al(NO3)3+3H2O
Fe2O3+6HCl=2FeCl3+3H2O
Fe2O3+6HNO3=2Fe(NO3)3+3H2O；
（3）By the filtering of gained leachate, washing, filtrate adds sodium hydroxide solution regulation pH removal of impurities, cleans involved
Chemical reaction has：
3OH-+Fe3+=Fe(OH)3↓ Mg2++3OH-=Mg（OH）2↓
Ca2++OH-=Ca(OH)2↓ Al(OH)3+ NaOH (excess)=NaAlO2+H2O；
（4）After removal of impurities CO is passed through in gained filtrate2Aluminum hydroxide precipitation is obtained, involved chemical reaction has：
NaAlO2 + CO2 + 2 H2O = Al(OH)3 ↓+ NaHCO3；
（5）Gained Al (OH)3Precipitation concentration is filtrated to get nano-aluminum hydroxide product.
Al in above-mentioned pelite2O3Content is 30%.
Above-mentioned steps（2）Mixed liquor used is the concentrated hydrochloric acid of volume fraction 20% and 20% concentrated nitric acid during middle leaching, and liquid-solid ratio is
Nitration mixture volume is 4 with powdered ore quality ratio：1.
Above-mentioned steps（2）In extraction time 2h, 80 DEG C of extraction temperature.
Above-mentioned steps（3）Middle sodium hydroxide solution pH is 13, is slowly added to filter when sodium hydroxide solution regulation pH is 4.5
Washing, then filtration washing when sodium hydroxide solution regulation pH is 13 is slowly added into filtrate.
Beneficial effects of the present invention：Compared with prior art, effect of the present invention is as follows：
（1）Increase specific surface area makes its reaction fully thorough after pelite is levigate, reacts faster, more efficient, and favorably
The Al in pelite2O3Leaching is more thorough, beneficial to the yield for improving nano-aluminum hydroxide, and impurity（Such as iron, calcium and magnesium）'s
Leach thoroughly, beneficial to follow-up contamination precipitation, make the purity of obtained nano-aluminum hydroxide higher；
（2）Hydrochloric acid and nitric acid mixed solution used is strong electrolyte, uses volume fraction as 20% concentrated hydrochloric acid and 20% dense nitre
Acid, liquid-solid ratio is mixed liquor volume and powdered ore quality ratio is 4：Under 1 proportioning, the Al in a diaspore can be preferably leached2O3
And impurity；
（3）Salpeter solution used is strong oxidizer, can be directly ferrous oxidising into ferric iron by part in pelite, is removed from
The process of subsequent oxidation, its is reduced later stage oxidation step, shorten preparation time, it is more efficient, also improve removal of impurities
Effect；
（4）Temperature at 80 DEG C, Ion transfer speed accelerate, make its chemical reaction rate fast, make its leach accelerate and it is thorough
Bottom, greatly improve leaching efficiency；
（5）It is thorough that time 2 h leaches it；
（6）Cleaned after leaching with the sodium hydroxide solution that pH is 13, filtration washing iron removaling when regulation pH is 4.5, then to filter
Filtration washing deliming when sodium hydroxide solution regulation pH is 13, magnesium are slowly added in liquid, removal of impurities is complete, allows obtained nanometer hydrogen-oxygen
It is purer to change aluminium；
In summary：Pelite is leached by the method hydrochloric acid and nitric acid mixed liquor of the present invention, by removal of impurities, purified,
The processes such as purification, can obtain the preferable nano-aluminum hydroxide powder of quality, can obtain preferable economic benefit, while make aluminum again
Rock resource is comprehensively utilized, and need not be bought high-end equipment in addition and be achieved that preparation, and equipment purchase cost is lower.
Brief description of the drawings
Fig. 1 is the preparation technology schematic flow sheet of the present invention.
Embodiment
Below in conjunction with the accompanying drawings and the present invention is described further specific embodiment.
Embodiment 1：The preparation method of nano-aluminum hydroxide, this method comprise the following steps in a kind of pelite：
（1）Using pelite as raw material, Al2O3Content is 30%, after it is used into jaw crushing crusher machine, then will be broken with ball mill
Broken miberal powder particle is ground below granularity 74um, and increase specific surface area makes its reaction fully thorough after pelite is levigate, reacts more
It hurry up, it is more efficient, and be advantageous to Al in pelite2O3Leach more thorough；
（2）By step（1）In grind miberal powder sample drying after, by the mixed solution of hydrochloric acid and nitric acid with drying miberal powder
It is placed in water-bath and stirs in proportion, mixed liquor used is the concentrated hydrochloric acid of volume fraction 20% and 20% concentrated nitric acid, and liquid-solid ratio is nitration mixture
Volume is 4 with powdered ore quality ratio：1, extraction time 2h, 80 DEG C of extraction temperature, volume fraction are used as 20% concentrated hydrochloric acid and 20% dense
Nitric acid, liquid-solid ratio is mixed liquor volume and powdered ore quality ratio is 4：Under 1 proportioning, can preferably it leach in a diaspore
Al2O3, temperature at 80 DEG C, Ion transfer speed accelerate, make its chemical reaction rate fast, make its leach accelerate and thoroughly, significantly
Improve leaching efficiency；
Step（2）Chemical reaction involved by middle leaching has：
Al2O3+6HCl=2AlCl3+3H2O
Al2O3+6HNO3=2Al(NO3)3+3H2O
Fe2O3+6HCl=2FeCl3+3H2O
Fe2O3+6HNO3=2Fe(NO3)3+3H2O；
（3）By the filtering of gained leachate, washing, filtrate adds sodium hydroxide solution regulation pH removal of impurities, sodium hydroxide solution
PH is 13, is slowly added to filtration washing iron removaling when sodium hydroxide solution regulation pH is 4.5, then hydroxide is slowly added into filtrate
Filtration washing deliming, magnesium when sodium solution regulation pH is 13；
Step（3）Chemical reaction involved by middle removal of impurities has：
3OH-+Fe3+=Fe(OH)3↓ Mg2++3OH-=Mg（OH）2↓
Ca2++OH-=Ca(OH)2↓ Al(OH)3+ NaOH (excess)=NaAlO2+H2O；
（4）After removal of impurities CO is passed through in gained filtrate2Obtain aluminum hydroxide precipitation；
Step（4）In involved chemical reaction have：
NaAlO2 + CO2 + 2 H2O = Al(OH)3 ↓+ NaHCO3；
（5）Gained Al (OH)3Precipitation concentration is filtrated to get nano-aluminum hydroxide product.
In summary：Pelite is leached by the method hydrochloric acid and nitric acid mixed liquor of the present invention, by removal of impurities, purified,
The processes such as purification, can obtain the preferable nano-aluminum hydroxide powder of quality, can obtain preferable economic benefit, while make aluminum again
Rock resource is comprehensively utilized, and need not be bought high-end equipment in addition and be achieved that preparation, and equipment purchase cost is lower.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
Those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, should all be contained
Cover within protection scope of the present invention, therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (2)
- A kind of 1. preparation method of nano-aluminum hydroxide in pelite, it is characterised in that：This method comprises the following steps：（1）Using pelite as raw material, after it is used into jaw crushing crusher machine, then with ball mill broken miberal powder particle is ground into grain Less than 74 μm of degree；（2）By step（1）In grind miberal powder sample drying after, by the mixed solution of hydrochloric acid and nitric acid with drying miberal powder press than Example, which is placed in water-bath, to be stirred, and leaching involved chemical reaction has：Al2O3+6HCl=2AlCl3+3H2OAl2O3+6HNO3=2Al(NO3)3+3H2OFe2O3+6HCl=2FeCl3+3H2OFe2O3+6HNO3=2Fe(NO3)3+3H2O；Step（2）Mixed liquor used is the concentrated hydrochloric acid of volume fraction 20% and 20% concentrated nitric acid during middle leaching, and liquid-solid ratio is nitration mixture volume It is 4 with powdered ore quality ratio：1；Step（2）In extraction time 2h, 80 DEG C of extraction temperature；（3）By the filtering of gained leachate, washing, filtrate adds sodium hydroxide solution regulation pH removal of impurities, and clean involved chemistry Reaction has：3OH-+Fe3+=Fe(OH)3↓ Mg2++3OH-=Mg（OH）2↓Ca2++OH-=Ca(OH)2↓ Al(OH)3+NaOH=NaAlO2+H2O,Wherein Al (OH)3When being reacted with NaOH, NaOH dosages are excessive；Step（3）Middle sodium hydroxide solution pH is 13, is slowly added to filtration washing when sodium hydroxide solution regulation pH is 4.5, then Filtration washing when sodium hydroxide solution regulation pH is 13 is slowly added into filtrate；（4）After removal of impurities CO is passed through in gained filtrate2Aluminum hydroxide precipitation is obtained, involved chemical reaction has：NaAlO2 + CO2 + 2 H2O = Al(OH)3 ↓+ NaHCO3；（5）Gained Al (OH)3Precipitation concentration is filtrated to get nano-aluminum hydroxide product.
- 2. the preparation method of nano-aluminum hydroxide in a kind of pelite according to claim 1, it is characterised in that：Pelite Middle Al2O3Content is 30%.
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| CN107265425B (en) * | 2017-07-28 | 2019-11-12 | 贵州大学 | The method for preparing lithium phosphate using pelite containing lithium |
| CN109399677B (en) * | 2018-12-10 | 2021-04-13 | 贵州博汇联润铝业有限公司 | Method for preparing aluminum hydroxide by using aluminum rock as raw material cell grinding and water milling seed crystal |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101734698A (en) * | 2009-09-08 | 2010-06-16 | 东北大学 | Method for preparing aluminum oxide from aluminiferous material |
| CN102515223A (en) * | 2011-12-09 | 2012-06-27 | 沈阳工业大学 | Method for efficient and comprehensive utilization of high-iron bauxite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101734698A (en) * | 2009-09-08 | 2010-06-16 | 东北大学 | Method for preparing aluminum oxide from aluminiferous material |
| CN102515223A (en) * | 2011-12-09 | 2012-06-27 | 沈阳工业大学 | Method for efficient and comprehensive utilization of high-iron bauxite |
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