CN1234609C - Process of producing high purify superfine aluminium oxide by industrial aluminium hydroxide - Google Patents
Process of producing high purify superfine aluminium oxide by industrial aluminium hydroxide Download PDFInfo
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- CN1234609C CN1234609C CN 200410021968 CN200410021968A CN1234609C CN 1234609 C CN1234609 C CN 1234609C CN 200410021968 CN200410021968 CN 200410021968 CN 200410021968 A CN200410021968 A CN 200410021968A CN 1234609 C CN1234609 C CN 1234609C
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- aluminium hydroxide
- slurry
- slip
- inorganic ceramic
- sodium
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to a method for producing ultrafine aluminum oxide with high purity by industrial aluminum hydroxide. The present invention has six processes of alkali fusion, trash extraction, carbon division, washing and sodium removal, solid-liquid separation and calcining dispersion. The present invention is characterized in that inorganic ceramic with film channel diameter phi 1 of 3 to 5mm and the film hole diameter phi 2 of 0.05 to 1.0 micrometer sold at markets is adopted; the inorganic ceramic film carries out washing and sodium removal on refining aluminum hydroxide powder. The particle size (D50) of the alumina product produced by the method of the present invention is less than 1 micrometer, the purity is above 99.9%, and Na2O content is controlled below 0.02%. Compared with the prior art, the method of the present invention has the advantages of wide raw material sources, cheap price, simple manufacturing technology, investment saving, little pollution, high product quality and easy realization of industrial production.
Description
One, technical field
The invention belongs to the compound of aluminium, be specifically related to the preparation of aluminum oxide.
Two, background technology
High-purity ultra-fine alumina is mainly used in the manufacturing fine ceramics, and for example it is an important source material of making the high-pressure mercury lamp translucent ceramic tube.Along with the progress of science and technology and the development of society, its purposes is more and more, and is increasing to its demand.In the prior art, Chinese invention patent that a name is called " high-purity ultra-fine alumina production technique and device " is arranged in Granted publication on May 21 (CN1034921C) in 1997; What it adopted is the tschermigite pyrolysis method, regularly advances the kiln body through preheating, dehydration, decomposition, phase inversion, cooling by the material puopulsion unit tschermigite (exsiccated ammonium alum), makes high-purity superfine alumina powder through superfine grinding again.But the ingredient requirement height that this operational path adopted, raw material sources are limited and price is high, simultaneously technological process energy consumption height, labour intensity is big, operating environment is poor, only is suitable for small-scale production.The Chinese invention patent that also has a name to be called " utilizing kaolinite (soil) to produce the technology of ultrapure aluminum oxide " applies on February 6th, 2002 open (CN1334240A); It is that kaolinite (soil) grog and acid-respons are generated aluminium salt, adds alkali again and forms aluminate, isolates impurity such as Fe, Ti earlier, adds the hydrate that acid forms aluminium then, again after drying, the washing, and the basic ion in the disposable rejecting product.But the product that this method is produced is not realized the super-refinement of powder, and Na in the product
2O content is still up to 0.02%, and purity is limited; Complex process, energy consumption height, material consumption and environmental pollution are big simultaneously.
Three, summary of the invention
The objective of the invention is to defective, adopt different processing methodes, reach 99.9%, Na with industrial production of aluminum hydroxide purity at the prior art existence
2The O foreign matter content is less than 0.02%, granularity (D
50) less than the high-purity superfine alumina powder of 1 μ m.
The technical solution used in the present invention is as follows.
The method of the industrial production of aluminum hydroxide ultra-fine alumina of a kind of usefulness,, removal of impurities molten by alkali, carbon branch, washing are taken off sodium, solid-liquid separation and calcining and are disperseed six step processes to form:
(1) alkali is molten
Industrial aluminium hydroxide and caustic soda are pressed Na
2O concentration 160-500g/L, alumina soda ratio α
k=1.35-5 is made into slip, send into the reactor internal heating to 120-170 ℃ of reaction 1.5-4 hour, obtain sodium metaaluminate dissolution fluid slip, slip is changed over to be cooled in the flash-pot below 111 ℃ again, by secondary steam and the recyclable utilization of water coolant that flash-pot produced.
(2) removal of impurities
The slip of will lowering the temperature is diluted to AL in dilution trap
2O
3Concentration is 80-140g/L, send in the removal of impurities reactor after will diluting the 0.1-2% adding hydrogen peroxide of slip again,, fed pressurized air 4 hours under the 0.4-0.8MPa condition at 90-120 ℃ by aluminium hydroxide weight, filter then, obtain to remove the refined liquid of impurity such as Si, Fe, Ca, Mg, Ti.
(3) carbon branch
Refined liquid is sent into carbon divide in the groove, feed CO at 50-85 ℃
2Gas 1.5-15 hour, form aluminium hydroxide one yellow soda ash slip, after solid-liquid separation, obtain refining aluminium hydroxide powder then, return the molten recycle of alkali after the sodium carbonate solution causticization.
(4) sodium is taken off in washing
Adopt the membrane channel diameter of phi
1=3-5mm, film hole diameter Φ
2The commercially available inorganic ceramic film of=0.05-1.0 μ m washs refining aluminium hydroxide powder and to take off sodium; Its process is will make with extra care aluminium hydroxide powder with 50-85 ℃ of pure water to be modulated into the slurry that solid content is 5-20% in the jar of sizing mixing that band stirs, inject the inorganic ceramic film device then at a high speed, it produces the pressure of 0.035-0.43MPa in the membrane channel of ceramic membrane, make the inside and outside both sides of membrane channel form the pressure reduction of 0.1-0.4MPa, portion water and water-soluble Na+ constantly ooze out to the membrane channel outside with high speed from the membrane channel inboard by fenestra under differential pressure action, and slurry is concentrated; Concentrated aluminium hydroxide slurry reinjects after the membrane channel outflow turns back to the jar of sizing mixing the inorganic ceramic film device, so circulation causes the slurry volume constantly to reduce, when slurry volume reducing during to the 2/3-1/2 of original volume, replenishing pure water to slurry in the jar of sizing mixing returns to original volume and reinjects in the inorganic ceramic film device, circulation cleaning repeatedly is until the Na of slurry
2O content meets the index that quality product requires.Whole washing is taken off the sodium process and is carried out automatization control.
(5) solid-liquid separation
To send in the reactor through the aluminium hydroxide slurry that inorganic ceramic film washing is taken off behind the sodium, at 145-200 ℃, the 0.4-1.0MPa condition presses down to boil after 4-8 hour carries out liquid-solid separation, obtains aluminium hydroxide powder, and liquid can return washing and take off the sodium utilization.
(6) calcining disperses
Aluminium hydroxide powder obtains high-purity superfine alumina powder after 1100-1350 ℃ of calcining, dispersion.
Technology of the present invention compared with prior art, raw material sources are extensive, the relatively low and low price of impurity; Use caustic soda to do the recycle and reuse of solvent energy, product per ton only need replenish a small amount of alkali lye of flow process loss; Impurity such as the Si in the raw material, Fe, Ca, Mg, Ti are removed with the removal of impurities process of insoluble throw out and deep desilication deferrization through alkali is molten; It has avoided required a large amount of pulverizing and the calcination process of employing kaolinite (soil) raw material, whole process product calcining for once dispersion process, and energy consumption is relatively low; Product granularity (D
50) less than 1 μ m, purity reaches more than 99.9%; Particularly adopt the inorganic ceramic film washing of original creation to take off the sodium technology, make aluminium hydroxide in washing process, remain the flow at high speed state, powder granule is by flow at high speed, not only not can as the such further reunion of mode of washing such as press filtration, centrifugal, vacuum filtration and make powder be difficult to washing to take off sodium, thereby can make powder obtain being dispersed with and being beneficial to washing and obtaining Na at last to a certain degree on the contrary
2O content is less than 0.02% high-purity superfine alumina powder.The present invention has that technology is simple, cost is low, reduced investment, pollution less, advantage such as quality product height and easy realization of industrialization.
Four, embodiment
Below enumerate main technique condition and the quality product of three embodiment.
Example 1 example 2 examples 3
(1) alkali is molten
1) slip proportioning Na
2O (g/L) 180 250 350
α
k 1.5 2 3
2) temperature of reaction (℃) 130 150 170
3) reaction times (hour) 432
(2) removal of impurities
1) slip Al
2O
3Concentration (g/L) 80 100 120
2) H
2O
2Add-on is (with hydroxide 1.5 1 0.5
The per-cent of aluminium weight meter)
3) temperature (℃) 90 100 110
4) pressure (MPa) 0.5 0.6 0.8
(3) carbon branch
1) temperature (℃) 50 60 80
2) logical CO
2The gas time (hour) 358
(4) sodium is taken off in washing
1) inorganic ceramic film
Channel diameter (mm) 3.5 45
Film hole diameter (μ m) 0.2 0.5 1.0
2) slurry solid content (%) 5 10 20
3) membrane channel inside and outside differential pressure (MPa) 0.25 0.2 0.1
(5) solid-liquid separation
1) press boil temperature (℃) 158 170 145
2) pressure is boiled pressure (MPa) 0.6 0.75 0.45
3) press and to boil the time (hour) 864
(6) calcining temperature (℃) 1260 ± 10 1300 ± 10 1200 ± 10
Quality product
D
50Granularity (μ m) 0.4-0.8 0.4-0.8 0.4-0.8
Na
2O content (%) 0.0039 0.01 0.015
Al
2O
3Content (%) 99.95 99.92 99.9
Claims (1)
1, the method for the industrial production of aluminum hydroxide ultra-fine alumina of a kind of usefulness,, removal of impurities molten by alkali, carbon branch, washing are taken off sodium, solid-liquid separation and calcining and are disperseed six step processes to form, and it is characterized in that:
1), said alkali is molten is by Na with industrial aluminium hydroxide and caustic soda
2O concentration 160-500g/L, alumina soda ratio α
k=1.35-5 is made into slip, sends into the reactor internal heating to 120-170 ℃ of reaction 1.5-4 hour, obtains sodium metaaluminate dissolution fluid slip, slip is changed over to be cooled in the flash-pot below 111 ℃ again;
2), said removal of impurities is that the cooling slip is diluted to AL in dilution trap
2O
3Concentration is 80-140g/L, will dilute and send in the removal of impurities reactor after slip adds hydrogen peroxide by the 0.1-2% of aluminium hydroxide weight, at 90-120 ℃, feeds pressurized air 4 hours under the 0.4-0.8MPa condition, filters then, obtains refined liquid;
3), said carbon branch is refined liquid to be sent into carbon divide in the groove, feeds CO at 50-85 ℃
2Gas 1.5-15 hour, form aluminium hydroxide one yellow soda ash slip, after solid-liquid separation, obtain refining aluminium hydroxide powder then;
4), to take off sodium be to adopt the membrane channel diameter of phi in said washing
1=3-5mm, film hole diameter Φ
2The inorganic ceramic film of=0.05-1.0 μ m washs refining aluminium hydroxide powder and to take off sodium; Its process is will make with extra care aluminium hydroxide powder with 50-85 ℃ of pure water to be modulated into the slurry that solid content is 5-20% in the jar of sizing mixing that band stirs, then to inject the inorganic ceramic film device at a high speed, the high speed slurry produces the pressure of 0.035-0.43MPa in the membrane channel of ceramic membrane, make the inside and outside both sides of membrane channel form the pressure reduction of 0.1-0.4MPa, portion water and water-soluble Na+ constantly ooze out to the membrane channel outside with high speed from the membrane channel inboard by fenestra, and slurry is concentrated; Concentrated slurry reinjects after the membrane channel outflow turns back to the jar of sizing mixing the inorganic ceramic film device, so circulation causes the slurry volume constantly to reduce, when slurry volume reducing during to the 2/3-1/2 of original volume, replenishing 50-85 ℃ of pure water to slurry in the jar of sizing mixing returns to original volume and reinjects in the inorganic ceramic film device, circulation cleaning repeatedly is until the Na of slurry
2O content meets the index that quality product requires;
5) said solid-liquid separation is that the aluminium hydroxide slurry that takes off through inorganic ceramic film washing behind the sodium is sent in the reactor, and at 145-200 ℃, the 0.4-1.0MPa condition presses down to boil after 4-8 hour carries out liquid-solid separation, obtains aluminium hydroxide powder;
6), said calcining dispersion is that aluminium hydroxide powder obtains superfine alumina powder after 1100-1350 ℃ of calcining, dispersion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410021968 CN1234609C (en) | 2004-03-04 | 2004-03-04 | Process of producing high purify superfine aluminium oxide by industrial aluminium hydroxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410021968 CN1234609C (en) | 2004-03-04 | 2004-03-04 | Process of producing high purify superfine aluminium oxide by industrial aluminium hydroxide |
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| CN1559905A CN1559905A (en) | 2005-01-05 |
| CN1234609C true CN1234609C (en) | 2006-01-04 |
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| CN 200410021968 Expired - Fee Related CN1234609C (en) | 2004-03-04 | 2004-03-04 | Process of producing high purify superfine aluminium oxide by industrial aluminium hydroxide |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100395185C (en) * | 2005-11-22 | 2008-06-18 | 华东理工大学 | Preparation of superfine aluminium hydroxide |
| CN102583473A (en) * | 2012-02-16 | 2012-07-18 | 山东晶鑫晶体科技有限公司 | Production method of high-purity aluminum oxide |
| CN104140118A (en) * | 2013-05-06 | 2014-11-12 | 重庆任丙科技有限公司 | A producing method of high-purity aluminium oxide |
| CN103204530B (en) * | 2013-05-14 | 2014-10-22 | 昆明冶金研究院 | Method for removing sodium in preparation of high-purity alumina |
| CN104860342A (en) * | 2015-05-07 | 2015-08-26 | 贵州省分析测试研究院 | Method for preparing high-purity ultrafine aluminium oxide |
| CN110734081A (en) * | 2019-11-22 | 2020-01-31 | 江苏九九铝业有限公司 | Oxidant used in production of kinds of alumina |
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