CN102910657A - Method for preparing high-pure aluminum oxide - Google Patents
Method for preparing high-pure aluminum oxide Download PDFInfo
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- CN102910657A CN102910657A CN2012103524071A CN201210352407A CN102910657A CN 102910657 A CN102910657 A CN 102910657A CN 2012103524071 A CN2012103524071 A CN 2012103524071A CN 201210352407 A CN201210352407 A CN 201210352407A CN 102910657 A CN102910657 A CN 102910657A
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Abstract
The invention relates to a method for preparing high-pure aluminum oxide. The method comprises the following steps: organic acids such as ammonium sulfate and tartaric acid are added in purified industrial aluminum sulfate to remove iron, so as to obtain an aluminum ammonium sulfate solution; the aluminum ammonium sulfate is reacted with refined hydrochloric acid; the obtained crystal is washed, dried, fired and milled, and finally the high-pure aluminum oxide is obtained. The method is simple in production technology; and the obtained aluminum oxide has high purity which can reach 99.999% even 99.9999 spectrum purity.
Description
Technical field
The present invention relates to the alumina powder jointed preparation technical field of inorganics.Be specially a kind of method for preparing high purity aluminium oxide.
Background technology
Aluminum oxide is the base mateiral of many Industrial processes, occupies an important position in Chemical market.Common aluminum oxide mainly is to obtain from the bauxite smelting technology, and its purity is low, can not satisfy processing requirement in a lot of purposes.The aluminum oxide of purity more than 99.99% belongs to high purity aluminium oxide.High purity aluminium oxide has the advantages such as purity is high, particle diameter is tiny, distribution of particle sizes is even, demonstrate the light, electricity, magnetic, heat and the mechanical characteristics that are better than common aluminum oxide, can be used as a kind of new function material and be widely used in the light transmitant aluminium oxide sintered compact, the fluor carrier, special gas additive, monocrystal material, advanced ceramic, high-pressure mercury lamp, physics and chemistry instrument, semiconductor substrate, turbine nuclear power machine and equipment, bearing, catalyzer and carrier, cutting tool, high hardness material, refractory materials, laserable material, lagging material.Owing to having this output value advantage, so scientific worker both domestic and external gives great concern to the development and application of high purity aluminium oxide.For improving the aluminum oxide performance, several preparation methods below main the employing:
(1) improvement bayer's process.To prepare sodium aluminate solution take the aluminium hydroxide that sintering process is produced in the alumina technology as raw material such as Chinese patent 200410023998.3, through operations such as for several times desiliconization, deironing, calcium, magnesium, decomposition, washings, filter to isolate insoluble impurity, then hydrothermal synthesis reaction obtains boehmite, boehmite is made high-purity ultra-fine alumina through operations such as washing, high-temperature roastings.
(2) exsiccated ammonium alum method.This method is generally used first sulfuric acid dissolution AI (OH)
3, make alum liquor after, add ammonium sulfate and react with it, make exsiccated ammonium alum.Control temperature of reaction, reaction soln proportioning and pH, carry out building-up reactions, crystallization, filter washing lotion and can be recycled.After repeatedly refining, exsiccated ammonium alum dewaters in dehydration furnace of exsiccated ammonium alum makes aluminum oxide after the high-temperature roasting.Patent 200410100972.4 and 02111255.X have improved this method, and it adopts exsiccated ammonium alum and bicarbonate of ammonia is raw material, and the heatable reactor internal reaction that stirs at band generates the aluminium carbonate ammonium, after filtration, washing, oven dry, roasting obtain alumina particle.201010549193 adopt the industrial aluminum sulphate of purifying to add aluminum ammonium sulfate solution and the hydrochloric acid that the organic acid deironing such as ammonium sulfate and tartrate make reacts, and the gained crystallization finally makes high purity aluminium oxide through washing, dry, calcining, grinding.
(3) organo-aluminium alcoholate salt solution solution.It is aluminum alkoxide hydrolysis and alkyl aluminum hydrolysis technique that the organoaluminum hydrolysis mainly contains aluminium alcoholates.Obtain colloidal sol behind the organoaluminum hydrolysis of alkoxide, treated gel again, through separating solidifying ultrafine powder presoma, so ultrafine powder.Patent 00105215.2 and 97103240.8 is to adopt the organic synthesis method that aluminium and Organic Alcohol are added catalyzer to react, and generates aluminium alcoholates, again through purify, the techniques such as refining hydrolysis, roasting, make aluminum oxide.Comprehensive these methods all exist technical process complexity, the complicated harshness of operational condition, it is large to relate to many, the main content difference of raw material types, impurity component varies, solution heating energy consumption is high, need to acquire the problem such as Special Equipment, make investment of production equipment large, product cost increases, and is difficult at home and abroad promote the use of in the existing industrial production.
Summary of the invention
The invention provides a kind of method for preparing high purity aluminium oxide, it is characterized in that: may further comprise the steps:
1) industrial 18 water Tai-Ace S 150 are joined in the deionized water, slowly heating makes it dissolving under constantly stirring, to 60-95 ℃, concentrated solution makes solution proportion at 1.32-1.38g/L, cooled and filtered, crystallization is analysed dried, and the filtrate sedimentation is removed impurity recycling and used after 20 hours.
2) industrial top grade ammonium sulfate is dissolved in deionized water, under constantly stirring, makes it dissolving, remove by filter the filtrate that mechanical impurity obtains clarifying.
3) will analyse dried crystalline sulfuric acid aluminium deionized water dissolving, under constantly stirring, slowly add ammoniumsulphate soln, to 60-95 ℃, add the organic acids such as tartrate or citric acid, and continue heating and keep solution temperature constant, filtered while hot during to be crystallized will separating out.Filtrate is concentrated, crystallisation by cooling, recrystallization twice again after crystallization dried, mother liquor reclaims and reuses.The organic acid add-ons such as its unresolvable tartaric acid or citric acid are the 1-10% of exsiccated ammonium alum weight.
4) technical hydrochloric acid is added in the round-bottomed flask, gradually slowly heating, the hydrogen chloride gas that evaporates filters through gac, silica wool first, removes Fe, heavy metal, SO
4 2-, the impurity such as free chlorine pass into conductivity water again it are absorbed, and become refining hydrochloric acid HCL weight content 30-38% for subsequent use.
5) get the exsiccated ammonium alum of recrystallization, add deionized water dissolving and filter, add the refining hydrochloric acid of HCL weight content 25-36%, constantly stir, until till aluminum chloride separates out fully.The crystallization of aluminum chloride is analysed dried, with purified salt acid elution crystal surface, remove SO
4 2-
6) with above-mentioned highly purified AlCl
3Crystallization place retort furnace 600-800 ℃ calcination 3-6 hour, pulverize, grind, sieving obtains high purity alumina powder.
The high purity alumina powder index that a process for preparing is: aluminum oxide purity 〉=99.999%; Even 〉=99.9999% spectroscopically pure, muriate [Cl]≤5 * 10
-3, vitriol [SO
4]≤4 * 10
-3, nitrate [NO
3]≤8 * 10
-4
Embodiment
Embodiment 1
Technical hydrochloric acid is added in the round-bottomed flask, gradually slowly heating, the hydrogen chloride gas that evaporates filters through gac, silica wool first, removes Fe, heavy metal, SO
4 2-, the impurity such as free chlorine pass into conductivity water again it are absorbed, and become high purity hydrochloric acid for subsequent use.The hydrochloric acid that uses among embodiment 2, embodiment 3, the embodiment 4 is the hydrochloric acid of this method preparation.
The hydrochloric acid foreign matter content analytical results that the activated carbon filtration hydrogen chloride gas makes
| The technical hydrochloric acid foreign matter content | Hydrochloric acid foreign matter content after refining | |
| Iron (in Fe) massfraction | 0.008 | 0.001 |
| Free chlorine (in Cl) massfraction | 0.008 | 0.0006 |
| Heavy metal (in As) massfraction | 0.0001 | 0.00001 |
| Vitriol is (with SO 4 2-Meter) massfraction | 0.03 | 0.005 |
1000g18 water and wastewater industry Tai-Ace S 150 is joined in the deionized water, and slowly heating makes it dissolving under constantly stirring, and to 85 ℃, concentrated solution to proportion is 1.35g/L, cooled and filtered, and crystallization is analysed dried, removes impurity recycling after the filtrate sedimentation is spent the night and uses.
100g industry top grade ammonium sulfate is dissolved in deionized water, under constantly stirring, makes it dissolving, remove by filter the filtrate that mechanical impurity obtains clarifying.
To analyse dried crystalline sulfuric acid aluminium deionized water dissolving, under constantly stirring, slowly add ammoniumsulphate soln, to 95 ℃, add 5g tartrate, continue heating and keep solution temperature constant, filtered while hot during to be crystallized will separating out.Filtrate is concentrated, crystallisation by cooling, recrystallization twice again after crystallization dried, mother liquor reclaims and reuses.
Get the exsiccated ammonium alum 150g of recrystallization, add the 150ml deionized water dissolving and filter, add 20-36% hydrochloric acid, constantly stir, until till aluminum chloride separates out fully.The crystallization of aluminum chloride is analysed dried, with hydrochloric acid wash crystallization surface, remove micro-SO
4 2-
With above-mentioned highly purified AlCl
3Crystallization places 600 ℃ of calcinations of retort furnace 3 hours, pulverizes, grinds, sieving obtains high purity alumina powder.
The aluminum oxide figureofmerit of preparing is: aluminum oxide 〉=99.9999%, muriate (Cl)≤4.5 * 10
-3, vitriol (SO
4)≤3 * 10
-3, nitrate (NO
3)≤8 * 10
-4
Embodiment 2
1000g18 water and wastewater industry Tai-Ace S 150 is joined in the deionized water, and slowly heating makes it dissolving under constantly stirring, to 95 ℃, and the concentrated solution cooled and filtered, crystallization is analysed dried, and the filtrate sedimentation removes by filter the impurity upper strata stillness of night with Büchner funnel after 20 hours and recycles.
100g industry top grade ammonium sulfate is dissolved in deionized water, under constantly stirring, makes it dissolving, remove by filter the filtrate that mechanical impurity obtains clarifying.
To analyse dried crystalline sulfuric acid aluminium deionized water dissolving, under constantly stirring, slowly add ammoniumsulphate soln, to 85 ℃, add 8g tartrate, continue heating and keep solution temperature constant, filtered while hot during to be crystallized will separating out.Filtrate is concentrated, crystallisation by cooling, recrystallization twice again after crystallization dried, mother liquor reclaims and reuses.
Get the exsiccated ammonium alum of 150g recrystallization, add the 150ml deionized water dissolving and filter, add 20-36% hydrochloric acid, constantly stir, until till aluminum chloride separates out fully.The crystallization of aluminum chloride is analysed dried, with hydrochloric acid wash crystallization surface, remove micro-SO
4 2-
Above-mentioned highly purified AlCl3 crystallization is placed 600 ℃ of calcinations of retort furnace 4 hours, pulverize, grind, sieving obtains high purity alumina powder.
The aluminum oxide figureofmerit of preparing is: aluminum oxide 〉=99.9999%, muriate (Cl)≤3 * 10
-3, vitriol (SO
4)≤2 * 10-
3, nitrate (NO
3)≤6 * 10
-4
Embodiment 3
1500g18 water and wastewater industry Tai-Ace S 150 is joined in the deionized water, and slowly heating makes it dissolving under constantly stirring, to 95 ℃, and the concentrated solution cooled and filtered, crystallization is analysed dried, and the filtrate sedimentation is removed impurity recycling and is used after 20 hours.
120g industry top grade ammonium sulfate is dissolved in deionized water, under constantly stirring, makes it dissolving, remove by filter the filtrate that mechanical impurity obtains clarifying.
To analyse dried crystalline sulfuric acid aluminium deionized water dissolving, under constantly stirring, slowly add ammoniumsulphate soln, to 95 ℃, add the organic acids such as 6g citric acid, continue heating and keep solution temperature constant, filtered while hot during to be crystallized will separating out.Filtrate is concentrated, crystallisation by cooling, recrystallization twice again after crystallization dried, mother liquor reclaims and reuses.
Get the exsiccated ammonium alum of 100g recrystallization, add the 120ml deionized water dissolving and filter, add 20-36% hydrochloric acid, constantly stir, until till aluminum chloride separates out fully.The crystallization of aluminum chloride is analysed dried, with hydrochloric acid wash crystallization surface, remove micro-SO
4 2-
With above-mentioned highly purified AlCl
3Crystallization places 600 ℃ of calcinations of retort furnace 4 hours, pulverizes, grinds, sieving obtains high purity alumina powder.
The aluminum oxide figureofmerit of preparing is: aluminum oxide 〉=99.999%, muriate (Cl)≤3 * 10
-3, vitriol (SO
4)≤2.5 * 10
-3, nitrate (NO
3)≤4.5 * 10
-3
Embodiment 4
The 1500g industrial aluminum sulphate is joined in the deionized water, and slowly heating makes it dissolving under constantly stirring, to 90 ℃, and the concentrated solution cooled and filtered, crystallization is analysed dried, and the filtrate sedimentation is removed impurity recycling and is used after 20 hours.
120g industry top grade ammonium sulfate is dissolved in deionized water, under constantly stirring, makes it dissolving, remove by filter the filtrate that mechanical impurity obtains clarifying.
To analyse dried crystalline sulfuric acid aluminium deionized water dissolving, under constantly stirring, slowly add ammoniumsulphate soln, to 75 ℃, add the organic acids such as 8g citric acid, continue heating and keep solution temperature constant, filtered while hot during to be crystallized will separating out.Filtrate is concentrated, crystallisation by cooling, recrystallization twice again after crystallization dried, mother liquor reclaims and reuses.
Get the exsiccated ammonium alum of 100g recrystallization, add the 150ml deionized water dissolving and filter, add 20-36% hydrochloric acid, constantly stir, until till aluminum chloride separates out fully.The crystallization of aluminum chloride is analysed dried, with hydrochloric acid wash crystallization surface, remove micro-SO
4 2-
With above-mentioned highly purified AlCl
3Crystallization places 800 ℃ of calcinations of retort furnace 6 hours, pulverizes, grinds, excessively obtains high purity alumina powder.
The aluminum oxide figureofmerit of preparing is: aluminum oxide 〉=99.999%, muriate (Cl)≤3.5 * 10
-3, vitriol (SO
4)≤2 * 10
-3, nitrate (NO
3)≤8 * 10
-4
Claims (1)
1. method for preparing high purity aluminium oxide is characterized in that: may further comprise the steps:
1) industrial 18 water Tai-Ace S 150 are joined in the deionized water, slowly heating makes it dissolving under constantly stirring, to 60-95 ℃, concentrated solution makes solution proportion at 1.32-1.38g/L, cooled and filtered, crystallization is analysed dried, and the filtrate sedimentation is removed impurity recycling and used after 20 hours;
2) industrial top grade ammonium sulfate is dissolved in deionized water, under constantly stirring, makes it dissolving, remove by filter the filtrate that mechanical impurity obtains clarifying;
3) will analyse dried crystalline sulfuric acid aluminium deionized water dissolving, under constantly stirring, slowly add ammoniumsulphate soln, to 60-95 ℃, add organic acid tartrate or citric acid, and continue heating and keep solution temperature constant, filtered while hot during to be crystallized will separating out; Filtrate is concentrated, crystallisation by cooling, recrystallization twice again after crystallization dried, mother liquor reclaims and reuses; Wherein the add-on of organic acid tartrate or citric acid is the 1-10% of exsiccated ammonium alum weight;
4) technical hydrochloric acid is added in the round-bottomed flask, gradually slowly heating, the hydrogen chloride gas that evaporates filters through gac, silica wool first, removes Fe, heavy metal, SO
4 2-, free chlorine impurity passes into conductivity water again it is absorbed, and becomes the refining hydrochloric acid of HCL weight content 30-38% in order to using;
5) get the exsiccated ammonium alum of recrystallization, add deionized water dissolving and filter, add the refining hydrochloric acid of HCL weight content 25-36%, constantly stir, until till aluminum chloride separates out fully; The crystallization of aluminum chloride is analysed dried, with the purified salt acid elution crystal surface of HCL weight content 25-36%, remove SO
4 2-
6) with above-mentioned highly purified AlCl
3Crystallization places in the retort furnace, at 600-800 ℃ of calcination 3-6 hour, pulverizes, grinds, sieving obtains high purity alumina powder;
The high purity alumina powder index that a process for preparing is: aluminum oxide purity 〉=99.999%; Muriate [Cl]≤5 * 10
-3, vitriol [SO
4]≤4 * 10
-3, nitrate [NO
3]≤8 * 10
-4
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| CN2012103524071A CN102910657A (en) | 2012-09-20 | 2012-09-20 | Method for preparing high-pure aluminum oxide |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103241754A (en) * | 2013-05-16 | 2013-08-14 | 贵阳一晶相光电科技有限公司 | Production method of high-purity aluminum oxide |
| CN104907090A (en) * | 2015-05-22 | 2015-09-16 | 宜兴汉光高新石化有限公司 | Catalytic reformate refining deolefination catalyst and preparation method thereof |
| CN105084400A (en) * | 2015-09-18 | 2015-11-25 | 东北大学 | Device and method for preparing activated aluminum oxide |
| CN110779830A (en) * | 2019-11-12 | 2020-02-11 | 攀枝花学院 | Method for analyzing free carbon in vanadium carbide |
| CN114273022A (en) * | 2021-12-23 | 2022-04-05 | 连云港原发新材料科技有限公司 | Filtering and impurity removing equipment for conveying high-purity alumina and implementation method thereof |
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| CN1201014A (en) * | 1997-06-04 | 1998-12-09 | 中国石油化工总公司 | Process for preparing high-purity aluminium oxide |
| CN1448340A (en) * | 2002-04-04 | 2003-10-15 | 苏州市宇光特种陶瓷材料厂 | Process for preparing high-purity ultra-fine alumina powder |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103241754A (en) * | 2013-05-16 | 2013-08-14 | 贵阳一晶相光电科技有限公司 | Production method of high-purity aluminum oxide |
| CN103241754B (en) * | 2013-05-16 | 2014-08-06 | 贵阳一晶相光电科技有限公司 | Production method of high-purity aluminum oxide |
| CN104907090A (en) * | 2015-05-22 | 2015-09-16 | 宜兴汉光高新石化有限公司 | Catalytic reformate refining deolefination catalyst and preparation method thereof |
| CN105084400A (en) * | 2015-09-18 | 2015-11-25 | 东北大学 | Device and method for preparing activated aluminum oxide |
| CN110779830A (en) * | 2019-11-12 | 2020-02-11 | 攀枝花学院 | Method for analyzing free carbon in vanadium carbide |
| CN114273022A (en) * | 2021-12-23 | 2022-04-05 | 连云港原发新材料科技有限公司 | Filtering and impurity removing equipment for conveying high-purity alumina and implementation method thereof |
| CN114273022B (en) * | 2021-12-23 | 2023-06-16 | 江苏汇联铝业有限公司 | Filtering impurity-removing equipment for conveying high-purity alumina and implementation method thereof |
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Application publication date: 20130206 |