CN1182037C - Prepn of high-purity alumina - Google Patents
Prepn of high-purity alumina Download PDFInfo
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- CN1182037C CN1182037C CNB021089914A CN02108991A CN1182037C CN 1182037 C CN1182037 C CN 1182037C CN B021089914 A CNB021089914 A CN B021089914A CN 02108991 A CN02108991 A CN 02108991A CN 1182037 C CN1182037 C CN 1182037C
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- CN
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- Prior art keywords
- choline
- aluminium
- high purity
- purity
- controlled
- Prior art date
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229960001231 choline Drugs 0.000 claims abstract description 34
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 33
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 33
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000004411 aluminium Substances 0.000 claims abstract description 30
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 28
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 7
- 230000004044 response Effects 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 5
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims description 4
- 235000019743 Choline chloride Nutrition 0.000 claims description 4
- 229960003178 choline chloride Drugs 0.000 claims description 4
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 238000007605 air drying Methods 0.000 claims description 3
- 230000005587 bubbling Effects 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000003456 ion exchange resin Substances 0.000 claims description 3
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 229920003023 plastic Polymers 0.000 claims description 3
- -1 polypropylene Polymers 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 3
- 239000004800 polyvinyl chloride Substances 0.000 claims description 3
- 238000003672 processing method Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 2
- 230000003014 reinforcing effect Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 18
- 239000000463 material Substances 0.000 abstract description 5
- 239000011734 sodium Substances 0.000 abstract description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 4
- 238000000227 grinding Methods 0.000 abstract description 4
- 229910052708 sodium Inorganic materials 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 3
- 150000002910 rare earth metals Chemical class 0.000 abstract description 3
- 239000000919 ceramic Substances 0.000 abstract description 2
- HMBHAQMOBKLWRX-UHFFFAOYSA-N 2,3-dihydro-1,4-benzodioxine-3-carboxylic acid Chemical compound C1=CC=C2OC(C(=O)O)COC2=C1 HMBHAQMOBKLWRX-UHFFFAOYSA-N 0.000 abstract 2
- 229940075419 choline hydroxide Drugs 0.000 abstract 2
- 238000005406 washing Methods 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 11
- 239000000047 product Substances 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 150000001412 amines Chemical class 0.000 description 5
- 239000005030 aluminium foil Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 239000002585 base Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 125000004433 nitrogen atom Chemical group N* 0.000 description 3
- 125000000962 organic group Chemical group 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004131 Bayer process Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003828 vacuum filtration Methods 0.000 description 2
- 229910000951 Aluminide Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- OIPILFWXSMYKGL-UHFFFAOYSA-N acetylcholine Chemical compound CC(=O)OCC[N+](C)(C)C OIPILFWXSMYKGL-UHFFFAOYSA-N 0.000 description 1
- 229960004373 acetylcholine Drugs 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 150000003818 basic metals Chemical class 0.000 description 1
- 229910001680 bayerite Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000002498 deadly effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229960002523 mercuric chloride Drugs 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- LWJROJCJINYWOX-UHFFFAOYSA-L mercury dichloride Chemical compound Cl[Hg]Cl LWJROJCJINYWOX-UHFFFAOYSA-L 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 150000003248 quinolines Chemical group 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000002110 toxicologic effect Effects 0.000 description 1
- 231100000027 toxicology Toxicity 0.000 description 1
- 229910001777 tschermigite Inorganic materials 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to a method for preparing high purity alumina, which is mainly characterized in that choline hydroxide reacts with high purity metallic aluminium to generate choline aluminum, the choline aluminum is hydrolyzed to generate aluminium hydroxide and choline hydroxide, and the aluminium hydroxide is filtered by washing, precipitated, calcined, ground, etc. to obtain high purity alpha-alumina. The method has the advantages of high product purity, good quality, low requirement for technological conditions, no pollution, low cost, etc. The high purity alumina prepared by the method is particularly suitable for being used in the fields of high voltage sodium lamp tubes, rare earth luminescent material, high grade grinding material, fine ceramics, etc.
Description
Technical field:
The present invention relates to the highly purified metallic aluminium of a kind of usefulness and prepare highly purified method of alumina as raw material through chemical reaction.
Background technology:
High purity aluminium oxide is mainly used in rare-earth luminescent material, high-pressure sodium fluorescent tube and other is such as extraordinary aluminum oxide application scenarios such as abrasive material, catalyzer and structural ceramicss, metals content impurity seldom (less than 0.01%) in the high purity aluminium oxide, sulfide and muriate also are deleterious.
The method that prior art is produced high purity aluminium oxide has following several:
One is the rinsing of Bayer process aluminum oxide, contain excessive sodium and silicon in Bayer process aluminum oxide and the aluminium hydroxide, the concentration of these impurity can reduce by the conditioned disjunction rinsing incinerating aluminum oxide of separating out that changes aluminium hydroxide, but these technology both expensive are unreliable to controlling required impurity level.
Chinese patent literature 95103368.9 and 95105843.6 relates to a kind of processing method of producing aluminum oxide and alumina powder with salting-out process, and its main drawback is that purity is lower, and environmental pollution is serious.
Chinese patent literature 93110316.9 relates to a kind of high-purity ultra-fine alumina production technique and device, and the tschermigite decomposition makes γ-Al
2O
3, phase inversion is α-Al then
2O
3, calcining produces the corrodibility acid gas, has economy and environmental problem.
Select high pure metal aluminium to have very big advantage, because can on technical scale, a large amount of cheapnesss produce 99.99% aluminium now as the starting materials of producing aluminum oxide.
Preparing method of alumina from metallic aluminium has multiple, a kind of is the hydrothermal oxidization metallic aluminium, metallic aluminium is (350-400 degree) and the following aluminum oxide that generates of high pressure (68-308 normal atmosphere) at high temperature, and these conditions need high-pressure reaction vessel, make the metal complete reaction need long time.
CN1079718 puts into the activation of 0.5% mercuric chloride solution with fine aluminium sheet or bits and takes out after one minute, puts into the distilled water hydrolysis again, at last with high-temperature heat treatment come the size of controlled oxidation aluminium nano particle with mutually.Mercury is the deadly defect of this method to the infringement of environment and human body.
Metallic aluminium generates aluminium alcoholates with the alcohol reaction under non-water condition, aluminium alcoholates and water reaction generate oxyhydroxide, Chinese patent literature 91111373.8 and Chinese patent literature 97103240.8 disclose and have a kind ofly prepared the method for super-microfine high pure alumina by low-carbon (LC) aluminium alcoholates hydrolysis reaction, can obtain purity greater than 99.99%, even-grained ultra micro fineness pure alumina product.The stock of the alcohol that this arts demand is relatively large and Distallation systm, what catch fire during operation and explode is dangerous big, simultaneously the cost height of product.
CN87106229 discloses a kind of method of producing high-purity alpha-alumina, this method comprises the oxidation reaction product that is formed by aluminium mother metal and oxygen-containing gas oxidant, the direct oxidation fine aluminium has only when aluminium powder very thin (74 μ) just possible, metallic aluminium and oxygen or oxidant reaction are very fast, so the oxidized hot institute of aluminum oxide fusion, the oxidation that this means aluminium powder both had been difficult to control, and potential danger is arranged again.
Summary of the invention:
The purpose of this invention is to provide the preparation method that a kind of quality product height, processing condition require low, non-environmental-pollution, high purity aluminium oxide that cost is low.
The object of the present invention is achieved like this: a kind of preparation method of high purity aluminium oxide, and it is characterized in that adopting following processing method to obtain high-purity αYang Hualv: i) raw material: purity is 99.996% refined aluminium; The choline that adopts reinforcing yin essence ion exchange resin that choline chloride 60 is transformed and generate; The reaction vessel that ii) adopts polyvinyl chloride, tetrafluoroethylene or the polypropylene plastics of anti-highly basic to make, temperature is controlled by built-in pipeline by circulating water and hot water, is reflected to stir the realization down of pressurized air bubbling; Iii) temperature of reaction is controlled at 20-80 ℃, and choline concentration is controlled at 0.1-2.0M, and the aluminium hydroxide of acquisition is at 110 ℃ of air dryings; Iv) refined aluminium, water, choline react under above-mentioned processing condition, judge speed of response by monitoring hydrogen effusion speed, and be very low or when stopping when speed of response, removes slurry, carries out solid-liquid separation, periodically adds refined aluminium, removes slurry; Aluminium hydroxide obtains dry powder by filtration, spraying drying, choline loops back reaction vessel, dried aluminium hydroxide is placed in kiln in the high purity aluminium oxide crucible and calcines, and the aluminium hydroxide after the calcining is pulverized at ball mill with the high purity aluminium oxide ball and obtained αYang Hualv, and purity can reach 99.99%.
Purpose of the present invention can also realize like this: temperature of reaction is controlled at 75 ℃, and choline concentration is controlled at 0.5M.
The present invention has following advantage: 1) product purity height, quality is good.The finished product aluminum oxide purity can reach 99.99%; 2) processing condition with gentleness are operated in the reactor that band stirs, and environmentally friendly, toxicological harmless is pollution-free; 3) cost is lower, and is attractive economically.
Embodiment:
The present invention is circulating reaction a---process of separating out that replaces the sodium hydroxide in the Bayer technology that everybody is familiar with choline.With the processing condition operation of gentleness, environmentally friendly, attractive economically in the reaction vessel that band stirs.
Indirectly produce aluminum oxide or make aluminium indirectly and water or the reaction of other water-soluble oxidizers generate aluminium hydroxide, calcining then, this method is than direct oxidation method controls reaction speed (and the amount of bringing into of controlling product impurity) preferably.
Basic metal and four closes ammonium hydroxide (molecular formula [(CH
3)
3N (CH
2CH
2OH)] OH, be abbreviated as ROH) reaction can easily metallic aluminium be converted into aluminium hydroxide and not produce any pollution, particularly four close ammonium hydroxide and have four organic groups to be connected with covalent linkage with nitrogen-atoms in the amine, ROH is a highly basic, on intensity with alkali metal hydroxide seemingly, this and organic amine (as an amine, diamines, triamine) are that weakly alkaline conclusion is completely contradicted, the intensity of ROH derives from being connected of four organic groups and nitrogen-atoms, the organic group of covalent linkage has been avoided contact (as the amine) of nitrogen-atoms with water, forces OH
-Ionization fully, choline is operated in a looping fashion among the present invention, and Recycle design makes the consumption of reagent reach minimum, and the amount of by-products that produces during calcining is minimum.
It is that the molecular structural formula of choline is because its low toxicity reaches suitability preferably that choline is used for the present invention:
High purity aluminium oxide preparation process chemical equation of the present invention is:
R wherein
+OH
-Be choline molecular formula [(CH
3)
3N (CH
2CH
2OH)] OH's writes a Chinese character in simplified form.
The present invention adopts 99.996% refined aluminium as raw material, and its foreign metal is analyzed as table 1.
Choline can utilize choline chloride 60 is prepared by strong basic ion exchange resin, choline concentration is controlled at 0.1-2.0M (doing the standard titration with hydrochloric acid), choline chloride 60 is incomplete to the conversion of choline, choline alkalescence is stronger than ammonia and amine, but a little less than sodium hydroxide, its toxicity is because its corrodibility and strong basicity.
Reaction vessel is made by plastics of anti-highly basic such as polyvinyl chloride, tetrafluoroethylene, polypropylene, stirs the pressurized air bubbling and realizes, temperature is controlled by built-in pipeline by circulating water and hot water, and the system architecture material is to keeping product purity very important.Speed of response is judged that by the speed that monitors the hydrogen effusion reactant is by vacuum filtration, sedimentation, press filtration, and a large amount of unreacted metal were restored in this step, and aluminium hydroxide is at 110 ℃ of air dryings.
During mass production, an amount of metallic aluminium, water, acetylcholine response are very low or stop to speed of response, remove slurry, carry out solid-liquid separation, periodically add metallic aluminium, remove slurry.Aluminium hydroxide obtains dry powder by filtration, spraying drying, and choline loops back reaction vessel, and dry back aluminium hydroxide is placed in kiln in the high purity aluminium oxide crucible to be calcined, and the aluminium hydroxide after the calcining is pulverized in ball mill with the high purity aluminium oxide ball.
The alkalescence of choline determines in the specific conductivity under the differing temps that by aqueous choline base solution under the measurement differing temps specific conductivity is to measure the easier method of cholinium ionization.The specific conductivity of same concentration differing temps is linear, increases with the rising of temperature, and this point is the same with other ionogen.The specific conductivity detected result shows that choline is a highly basic less than 0.5M the time.
Aqueous choline base solution is decomposed near 100 ℃ the time, and principal reaction is:
0.5M choline solution in 75 ℃ of waters bath with thermostatic control, place 28h and do not have change in concentration, obviously do not decompose, because any decomposition can cause the noticeable change led than electricity.Described thermolysis can not become the problem that the present invention applies, the severe condition that the choline that this experiment has repeated decomposes.In actually operating, choline solution partly is converted into the choline aluminide, and this also can reduce the rate of decomposition of choline conversely.As previously mentioned, purity is the alumina product sixty-four dollar question.Though inevitably can bring impurity in the operating process, as long as the final product purity of carefully handled has still surpassed 99.99% target (seeing Table 1).
Table 1
| ％ | Original aluminum | Aluminium hydroxide | The comminution by gas stream aluminum oxide |
| Si | 0.0015 | 0.0012 | 0.0020 |
| Fe | 0.0010 | 0.0010 | 0.0015 |
| Ca | 0.0010 | 0.0012 | 0.0010 |
| Mg | 0.0004 | 0.0004 | 0.0005 |
| Na | 0.0010 | 0.0011 | 0.0010 |
| Cu | 0.0015 | 0.0007 | 0.0010 |
| Impurity amounts to | 0.0064 | 0.0056 | 0.0070 |
| Purity | 99.9936 | 99.9944 | 99.9930 |
Calcining exist with the fore portion choline with aluminium hydroxide in, but can residual carbon and nitrogen after the calcining.The granularity of the aluminium hydroxide of producing in the reactor is decided by the existence of temperature, degree of supersaturation, crystal seed.Yet in plant-scale operation, these parameters all keep relative stability, yet size-grade distribution can change by the retouching operation parameter.The size-grade distribution that separate out, calcine, grinding and the correct coupling of fractionated can be produced any needs.
The specific surface of aluminium hydroxide is 25-60m
2/ g, high like this specific surface come from separate out during the reunion of small-crystalline.Calcinations of aluminum hydroxide can produce 2-400m
2/ g specific surface area.
When not having crystal seed, the crystalline phase of the aluminium hydroxide that choline and metallic aluminium reaction generate is a bayerite.
After producing aluminium hydroxide, adopt traditional calcining and grinding explained hereafter αYang Hualv, by the character optimizing that adjusting is separated out, calcined, grinding, progressive operation can make final αYang Hualv product, to satisfy the concrete needs of using.
The aluminum oxide of present method preparation is specially adapted to high-pressure sodium fluorescent tube, rare earth luminescent material, senior abrasive substance, fine ceramics field.
Embodiment: the aluminium foil 100g that 0.1mm is thick puts into 1000 milliliters beaker, the aqueous choline base solution that adds 600 milliliters of 0.5M, be placed in 75 ℃ the water bath with thermostatic control, per 30 minutes with the rod stirring once, reacted 24 hours, at this moment most aluminium foils have changed into aluminium hydroxide powder, remaining minute quantity unreacted aluminium foil completely is deposited in the bottom of beaker, crosses 100 mesh sieves, and sieve is aluminium hydroxide down, it on the sieve unreacted aluminium foil completely, about 5g that weighs after the oven dry, with the aluminium hydroxide vacuum filtration, filtrate is returned beaker, filter cake 1200 ℃ of calcinings 4 hours, obtains α-Al with the high temperature retort furnace
2O
3Powder 183g.
Claims (2)
1, a kind of preparation method of high purity aluminium oxide is characterized in that adopting following processing method to obtain high-purity αYang Hualv:
I) raw material: purity is 99.996% refined aluminium; The choline that adopts reinforcing yin essence ion exchange resin that choline chloride 60 is transformed and generate;
The reaction vessel that ii) adopts polyvinyl chloride, tetrafluoroethylene or the polypropylene plastics of anti-highly basic to make, temperature is controlled by built-in pipeline by circulating water and hot water, is reflected to stir the realization down of pressurized air bubbling;
Iii) temperature of reaction is controlled at 20-80 ℃, and choline concentration is controlled at 0.1-2.0M, and the aluminium hydroxide of acquisition is at 110 ℃ of air dryings;
Iv) refined aluminium, water, choline react under above-mentioned processing condition, judge speed of response by monitoring hydrogen effusion speed, and be very low or when stopping when speed of response, removes slurry, carries out solid-liquid separation, periodically adds refined aluminium, removes slurry; Aluminium hydroxide obtains dry powder by filtration, spraying drying, choline loops back reaction vessel, dried aluminium hydroxide is placed in kiln in the high purity aluminium oxide crucible and calcines, and the aluminium hydroxide after the calcining is pulverized at ball mill with the high purity aluminium oxide ball and obtained αYang Hualv, and purity can reach 99.99%.
2, the preparation method of high purity aluminium oxide according to claim 1 is characterized in that: temperature of reaction is controlled at 75 ℃, and choline concentration is controlled at 0.5M.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021089914A CN1182037C (en) | 2002-04-19 | 2002-04-19 | Prepn of high-purity alumina |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021089914A CN1182037C (en) | 2002-04-19 | 2002-04-19 | Prepn of high-purity alumina |
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| Publication Number | Publication Date |
|---|---|
| CN1374252A CN1374252A (en) | 2002-10-16 |
| CN1182037C true CN1182037C (en) | 2004-12-29 |
Family
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|---|---|---|---|
| CNB021089914A Expired - Lifetime CN1182037C (en) | 2002-04-19 | 2002-04-19 | Prepn of high-purity alumina |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974867B (en) * | 2006-11-28 | 2011-07-20 | 河南大学 | Aluminium anode consuming process in water solution for producing micron or nanometer aluminium particle |
| JP2010168271A (en) * | 2008-12-25 | 2010-08-05 | Sumitomo Chemical Co Ltd | Method for producing alumina |
| US8287826B2 (en) * | 2009-09-18 | 2012-10-16 | Eestor, Inc. | Selective-cation-removal purification of aluminum source |
| CN102173756B (en) * | 2011-01-30 | 2013-03-20 | 河北恒博精细陶瓷材料有限公司 | Preparation method of high-purity aluminum oxide sintered body for growing sapphire crystal |
| CN102674419B (en) * | 2011-11-22 | 2014-02-05 | 昆明马克西姆科技有限公司 | Preparation method of high-purity ultrafine Al2O3 powder |
| CN103241756A (en) * | 2012-02-03 | 2013-08-14 | 上海飞凯光电材料股份有限公司 | Preparation method for alumina solid |
| CN103663525B (en) * | 2012-09-24 | 2016-04-20 | 韩香娟 | Methylamine legal system is for high purity aluminium oxide |
| CN104903241A (en) * | 2012-12-17 | 2015-09-09 | 波拉尔蓝宝石有限公司 | Process for making high-purity aluminum oxide |
| CN103043692B (en) * | 2012-12-27 | 2016-03-30 | 西安迈克森新材料有限公司 | A kind of preparation method of high-purity aluminum oxide powder material |
| JP2022529200A (en) * | 2019-04-16 | 2022-06-20 | フィナジー リミテッド | Manufacture of high-purity alumina and co-products from used electrolytes in metal-air batteries |
| CN110683569A (en) * | 2019-11-13 | 2020-01-14 | 山东恒嘉高纯铝业科技股份有限公司 | Method for producing alumina superfine powder in large batch at low cost |
| CN115196658B (en) * | 2022-05-18 | 2023-11-21 | 陕西煤业化工技术研究院有限责任公司 | High-purity alumina powder prepared rapidly through self-catalysis and method |
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2002
- 2002-04-19 CN CNB021089914A patent/CN1182037C/en not_active Expired - Lifetime
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