CN106115755A - A kind of method utilizing aluminium scrap goods upgrading to prepare high purity aluminium oxide - Google Patents

A kind of method utilizing aluminium scrap goods upgrading to prepare high purity aluminium oxide Download PDF

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Publication number
CN106115755A
CN106115755A CN201610484240.2A CN201610484240A CN106115755A CN 106115755 A CN106115755 A CN 106115755A CN 201610484240 A CN201610484240 A CN 201610484240A CN 106115755 A CN106115755 A CN 106115755A
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CN
China
Prior art keywords
naalo
aluminium
aluminium scrap
goods
scrap goods
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CN201610484240.2A
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Chinese (zh)
Inventor
殷剑龙
陈长科
马冰
崔兰浩
潘庆云
张霖
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Shanghai Weng Ze Technology Co Ltd
Xinjiang Joinworld Co Ltd
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Shanghai Weng Ze Technology Co Ltd
Xinjiang Joinworld Co Ltd
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Priority to CN201610484240.2A priority Critical patent/CN106115755A/en
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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
    • C01F7/42—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation
    • C01F7/422—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation by oxidation with a gaseous oxidator at a high temperature
    • 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
    • C01F7/46—Purification of aluminium oxide, aluminium hydroxide or aluminates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The present invention discloses a kind of method utilizing aluminium scrap goods upgrading to prepare high purity aluminium oxide, comprises the steps: first the aluminium scrap goods cleaned up fusing to be obtained aluminum liquid, then will react generation Al (OH) after aluminum liquid mist with water3；The Al (OH) that will obtain3It is dissolved in NaOH solution, is centrifuged off insoluble matter, obtain the NaAlO of clarification2Solution；To NaAlO2Solution adds the Al (OH) as adsorption-edulcoration agent3Nano-particle, is centrifuged off precipitate；Again to NaAlO2Solution adds Al (OH)3Crystal seed, the Al (OH) of precipitation3Precipitate cleaned, dry, after roasting, obtain the high purity aluminium oxide of purity >=99.99%.The present invention not only solves the recycling problem of increasing aluminium scrap goods, and solves the problem reclaimed of often demoting in aluminium scrap goods removal process, and aluminium scrap goods are converted into the high-purity alumina powder of more than 4N level, and simple to operate, cost is relatively low.

Description

A kind of method utilizing aluminium scrap goods upgrading to prepare high purity aluminium oxide
Technical field
The present invention relates to the preparation method of a kind of high-purity alumina powder, utilize the upgrading preparation of aluminium scrap goods particularly to one The method of 5N level high purity aluminium oxide, belongs to aluminium scrap utilization, inorganic material synthesis field.
Background technology
Aluminum has been widely used in the every aspect of our life as the metal that nature reserves are the highest.Along with to gold Belonging to improving constantly of material performance requirement, in recent years, aluminum alloy materials quickly grows.But, it is contemplated that natural resources reserves with And the appearance of a large amount of aluminium scrap goods has become as the key issue of environmental pollution, the most rationally process, process aluminium scrap goods and become The difficult problem that current mankind faces.
The current major way processing aluminium scrap goods remains employing and melts down melting, and this mode is primarily present aluminum products product The deficiencies such as matter degradation, the response rate are low, alloying element residual, production cost increase, range of application reduces.
Aluminium oxide is one of material that ceramic material range of application is the widest.Important as alumina material of high purity aluminium oxide Branch, is widely used in sapphire single-crystal, laser crystal Material synthesis (such as YAG monocrystalline etc.), crystalline ceramics (as aluminium oxide is saturating Bright pottery, YAG crystalline ceramics etc.) etc. aspect.Utilize inorganic chemistry method that aluminium scrap goods are changed into high purity alumina powder to be The safeguarding grades of aluminium scrap goods, upgrade recycling provide new developing direction.Patent documentation CN103214013A provides one to use Aluminum strip and heat alkali liquid, remove impurity is passed through CO2High-purity alumina powder is prepared in rear pickling, roasting, and this technological reaction is fierce, cleaner remove impurity Introducing impurity element, the operation of secondary dedoping step is complicated, purity reaches more than 99.999%, but it is tighter to ingredient requirement simultaneously Lattice, must use purity to reach the metallic aluminium of 98% as aluminum source, it is difficult to effectively to utilize a large amount of aluminium scrap goods.
Summary of the invention
It is an object of the invention to provide a kind of method utilizing aluminium scrap goods upgrading to prepare high purity aluminium oxide, by by aluminium scrap Goods are converted into high purity aluminium oxide, to reach aluminium scrap upgrading processing and to open up the purpose of aluminium scrap new application.
In order to solve above-mentioned technical problem, the invention provides following technical scheme:
A kind of method utilizing aluminium scrap goods upgrading to prepare high purity aluminium oxide, comprises the steps:
(1) first the aluminium scrap goods cleaned up fusing is obtained aluminum liquid, then generation Al (OH) will be reacted after aluminum liquid mist with water3, The main chemical reaction of this step is: Al+H2O → Al(OH)3；
(2) Al (OH) that step (1) is obtained3It is dissolved in NaOH solution, is centrifuged off insoluble matter, obtain the NaAlO of clarification2Molten Liquid, the main chemical reaction of this step is Al (OH)3 + NaOH → NaAlO2 + 2H2O；
(3) NaAlO prepared to step (2)2Solution adds the Al (OH) as adsorption-edulcoration agent3Nano-particle, is centrifuged and removes Remove precipitate；
(4) to the NaAlO processed through step (3)2Solution adds Al (OH)3Crystal seed, induces crystallize, the Al (OH) of precipitation3Precipitation Cleaned, dry, after roasting, obtain the high purity aluminium oxide of purity >=99.99%.
Further, described aluminium scrap goods are production, daily aluminum products waste material or waste aluminium goods, aluminum content >=95wt%.
Preferably, in step (1), first capture with steam after aluminum liquid mist, be subsequently adding the water of excess, through hydro-thermal reaction Generate Al (OH)3, then the Al (OH) that will generate3Drying, hydro-thermal reaction carries out (temperature is generally about 100 DEG C) under boiling.
Preferably, in step (2), the concentration of described NaOH solution is 0.05-0.2 mol/L.
Preferably, in step (2), described NaAlO2The caustic ratio α of solutionKControl at 1.3-1.4.
Preferably, in step (3), described Al (OH)3The particle diameter of nano-particle is 5-10nm, described Al (OH)3Nano-particle Addition be NaAlO2The 5-10 % of mole, the adsorption-edulcoration time controls at 1.5-3h.
Preferably, in step (4), described Al (OH)3The addition of crystal seed is NaAlO2The 15-25 % of mole, more preferably The described Al (OH) in ground3The addition of crystal seed is NaAlO2The 20% of mole, the Al (OH) that induction separates out3Precipitation capacity reaches NaAlO2 Mole about 90% time, stop induction crystallize and also carry out solid-liquid separation operation, the crystallize time is typically at 10-18h.
Preferably, in step (4), described sintering temperature, more than 1100 DEG C, more preferably 1200 DEG C, is gone out by high temperature Fall a small amount of Na+Deng impurity, thus the high purity aluminium oxide of purity >=99.999% can be obtained further.
Preferably, in step (4), after crystallize, to NaAlO2Residual liquid is passed through CO2Gas, CO2Flow velocity be 2.5-4L/ Min, the Al obtained (OH)3Nano-particle can be used as the adsorption-edulcoration agent of step (3), this 2NaAlO2 + CO2 + 3H2O → 2Al(OH)3 + Na2CO3。
Compared with prior art, the beneficial effects of the present invention is:
(1) aluminium scrap goods are changed into senior fine chemistry industry material by the method that the present invention synthesizes with inorganic chemistry.Not only solve The recycling problem of increasing aluminium scrap goods, and solve asking of recovery of often demoting in aluminium scrap goods removal process Aluminium scrap goods are converted into the high-purity alumina powder of more than 4N level by topic, can be as special cermacis, sapphire crystal, lithium battery The raw materials such as barrier film, connect metal and field of inorganic nonmetal；
(2) technique that direct hydrolysis and the molten kind of alkali divide abductive approach to combine is utilized, whole process device and simple to operate, cost Relatively low；
(3) in preparation process, final waste liquid NaAlO2It is passed through CO2High-purity nm Al (OH) can be obtained after carrying out carbonation decompsition process3With In remove impurity and induction kind point, neutralizing the OH-in solution simultaneously, reduce the pollution to environment, aluminium recovery prepared by aluminium scrap reaches 85% Above, effectively economize on resources.
Caustic ratio αKRefer to the contained caustic alkali (oxidation existed with the form such as sodium metaaluminate and sodium hydroxide in solution Sodium) with the ratio of the amount of the material of aluminium oxide.
Detailed description of the invention
Hereinafter the preferred embodiments of the present invention are illustrated, it will be appreciated that preferred embodiment described herein is only used In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1
(1) weigh 560g aluminium scrap goods (aluminum content is 96%), clean surface oil stain with organic solvent, and repeatedly rush with high purity water Wash post-drying, be weighed as 545g；
(2) obtaining aluminum liquid by melted, by aluminum liquid mist chemical conversion aluminum micro-nano granules and contact with steam, direct part activation is raw Become Al (OH)3, it is supplemented with 108g high purity water (resistivity >=14M Ω), boils and carry out hydro-thermal reaction, make aluminum be fully converted into Al (OH)3After, dry, obtain Al (OH)3Powder；
(3) Al (OH) that will obtain3Powder joins in the NaOH solution that concentration is 1mol/L, dissolves, and controls solution after dissolving Caustic ratio αK=1.3, utilize centrifugation that solid insoluble is got rid of (insoluble matter about 5.1g), obtain the NaAlO of clarification2Molten Liquid；
(4) to the NaAlO of clarification2Solution once adds the Al (OH) that 78g particle diameter is 5nm3Nano-particle carries out adsorption-edulcoration, The remove impurity time controls at 2.5h, and centrifugal solid-liquid is separated off precipitating (about 182g), obtains high-purity N aAlO2Solution；
(5) to high-purity N aAlO2Solution adds high-purity Al (OH) of 312g3Crystal seed (purity is 99.999%) carries out induction analysis Crystalline substance, after control induction time is 14h, solid-liquid separation, dry precipitation and be weighed as the high-purity Al of 1702g (OH)3, waste aluminum recovery rate is 89.5%, purity is 99.998%；
(6) NaAlO after step (5) solid-liquid separation2Waste liquid is passed through CO2Gas, controlling ventilation is 3L/min, can obtain The Al (OH) of particle diameter ＜ 10nm3Nano-particle, can serve as step (4) adsorption-edulcoration agent after drying；
(7) high-purity Al (OH) that step (5) is dried31200 DEG C of roastings, go out to fall a small amount of Na by high temperature+Deng impurity, obtain pure Degree is the high purity alumina powder of 99.999%, additionally by oxyhydrogen flame or high-frequency cold crucible technique (producing temperature ＞ 2000 DEG C) Purity can be obtained and reach high purity aluminium oxide broken grain or the polycrystal material of more than 99.9993%.
Finally it is noted that the foregoing is only the preferred embodiments of the present invention, it is not limited to the present invention, Although being described in detail the present invention with reference to previous embodiment, for a person skilled in the art, it still may be used So that the technical scheme described in foregoing embodiments to be modified, or wherein portion of techniques feature is carried out equivalent. All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included in the present invention's Within protection domain.

Claims (10)

1. the method utilizing aluminium scrap goods upgrading to prepare high purity aluminium oxide, comprises the steps:
(1) first the aluminium scrap goods cleaned up fusing is obtained aluminum liquid, then generation Al (OH) will be reacted after aluminum liquid mist with water3；
(2) Al (OH) that step (1) is obtained3It is dissolved in NaOH solution, is centrifuged off insoluble matter, obtain the NaAlO of clarification2Molten Liquid；
(3) NaAlO prepared to step (2)2Solution adds the Al (OH) as adsorption-edulcoration agent3Nano-particle, is centrifuged off Precipitate；
(4) to the NaAlO processed through step (3)2Solution adds Al (OH)3Crystal seed, induces crystallize, the Al (OH) of precipitation3Precipitation Cleaned, dry, after roasting, obtain the high purity aluminium oxide of purity >=99.99%.
Method the most according to claim 1, it is characterised in that described aluminium scrap goods for produce, daily aluminum products waste material or Waste aluminium goods, aluminum content >=95wt%.
Method the most according to claim 1, it is characterised in that in step (1), first captures with steam after aluminum liquid mist, It is subsequently adding the water of excess, generates Al (OH) through hydro-thermal reaction3, then the Al (OH) that will generate3Dry.
Method the most according to claim 1, it is characterised in that in step (2), the concentration of described NaOH solution is 0.05- 0.2 mol/L。
Method the most according to claim 1, it is characterised in that in step (2), described NaAlO2The caustic ratio α of solutionK Control at 1.3-1.4.
Method the most according to claim 1, it is characterised in that in step (3), described Al (OH)3The particle diameter of nano-particle is 5-10nm。
Method the most according to claim 1, it is characterised in that in step (3), described Al (OH)3The addition of nano-particle For NaAlO2The 5-10 % of mole.
Method the most according to claim 1, it is characterised in that in step (4), described Al (OH)3The addition of crystal seed is NaAlO2The 15-25 % of mole.
Method the most according to claim 1, it is characterised in that in step (4), described sintering temperature is more than 1100 DEG C.
Method the most according to claim 1, it is characterised in that in step (4), after crystallize, to NaAlO2Residual liquid is passed through CO2Gas, CO2Flow velocity be 2.5-4L/min, obtain Al (OH)3Nano-particle.
CN201610484240.2A 2016-06-28 2016-06-28 A kind of method utilizing aluminium scrap goods upgrading to prepare high purity aluminium oxide Pending CN106115755A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109052442A (en) * 2018-10-18 2018-12-21 中铝山东有限公司 A kind of production method of electron level high heat resistance aluminium hydroxide
CN109455748A (en) * 2018-12-17 2019-03-12 北京建工金源环保发展股份有限公司 A method of recycling aluminum nitrate from waste acid liquor
CN110156056A (en) * 2019-04-18 2019-08-23 新疆众和股份有限公司 A method of special-alumina is prepared containing phosphorus waste liquid using corrosive aluminum foil
CN111662173A (en) * 2020-06-03 2020-09-15 中铝山东有限公司 Aluminum hydroxy oxalate and preparation method thereof, and high-purity aluminum oxide
WO2022221903A1 (en) * 2021-04-19 2022-10-27 Dingo HPA Pty Ltd Process for forming high purity alumina

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CN105347378A (en) * 2015-10-13 2016-02-24 刘冠华 Preparation method for alumina powder, and alumina powder

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109052442A (en) * 2018-10-18 2018-12-21 中铝山东有限公司 A kind of production method of electron level high heat resistance aluminium hydroxide
CN109052442B (en) * 2018-10-18 2021-04-13 中铝山东有限公司 Production method of electronic grade high heat-resistant aluminum hydroxide
CN109455748A (en) * 2018-12-17 2019-03-12 北京建工金源环保发展股份有限公司 A method of recycling aluminum nitrate from waste acid liquor
CN110156056A (en) * 2019-04-18 2019-08-23 新疆众和股份有限公司 A method of special-alumina is prepared containing phosphorus waste liquid using corrosive aluminum foil
CN110156056B (en) * 2019-04-18 2021-12-28 新疆众和股份有限公司 Method for preparing special alumina by using phosphorus-containing waste liquid generated by corroding aluminum foil
CN111662173A (en) * 2020-06-03 2020-09-15 中铝山东有限公司 Aluminum hydroxy oxalate and preparation method thereof, and high-purity aluminum oxide
CN111662173B (en) * 2020-06-03 2023-03-24 中铝山东有限公司 Aluminum hydroxy oxalate and preparation method thereof, and high-purity aluminum oxide
WO2022221903A1 (en) * 2021-04-19 2022-10-27 Dingo HPA Pty Ltd Process for forming high purity alumina

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Application publication date: 20161116