CN102874854A - Preparation method of 5N high-purity nanometer alumina powder - Google Patents
Preparation method of 5N high-purity nanometer alumina powder Download PDFInfo
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- CN102874854A CN102874854A CN2012104364154A CN201210436415A CN102874854A CN 102874854 A CN102874854 A CN 102874854A CN 2012104364154 A CN2012104364154 A CN 2012104364154A CN 201210436415 A CN201210436415 A CN 201210436415A CN 102874854 A CN102874854 A CN 102874854A
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Abstract
The invention discloses a preparation method of 5N high-purity nanometer alumina powder. The preparation method is characterized by comprising the steps as follows: agitating a precursor of 5N aluminium isopropoxide, deionized water and dispersing agent based on mol ratio of 1: 10 to 30: 0.5 to 2 at 85 to 100 DEG C, and reflowing and hydrolyzing for 3 to 5 hours to obtain a hydrolyzing mixture; steaming the hydrolyzing mixture at 80 to 100 DEG C to obtain byproduct isopropanol which is generated in the hydrolyzing reaction and an azeotrope solution of the isopropanol and the water; then centrifugally filtering the product to obtain hydrated alumina; then transferring the hydrated alumina into a roasting furnace to be dried for 8 to 15 minutes at 80 to 110 DEG C; roasting the hydrated alumina for 25 to 45 minutes at 500 to 700 DEG C to obtain 5N high-purity gamma-Al2O3 powder with granularity of 5 to 50nm and D50 of 25nm; then continuously heating to reach 1050 to 1200 DEG C, and roasting for 30 to 50 minutes to obtain the 5N high-purity alpha-Al2O3 powder with granularity of 10 to 100nm and D50 of 50nm.
Description
Technical field
The present invention relates to a kind of method of 5N high purity nanometer alumina, particularly relate to aluminium alcoholates and disperse hydrolysis and microwave drying roasting process integration to prepare the method for 5N high purity nanometer alumina powder.
Background technology
The high purity nanometer alumina powder, not only purity is high, and granularity reach nano level (1～100nm), narrow particle size distribution, good dispersity.The small-size effect that nano-powder has, surface-interface effect, quantum size effect and macro quanta tunnel effect etc. make it have broad application prospects in fields such as catalysis, optical filtering, photoabsorption, medicine, magneticmedium and novel materials.High purity nanometer alumina has good optics, electric property and mechanical property is used widely in the modern high technology field of new, as being used as crystalline ceramics raw material, fluorescent material, sapphire crystal material, catalyzer, laserable material and semiconductor substrate etc.In recent years, development along with whole world LED industry, high purity aluminium oxide is processed to sapphire, be used for the LED substrate material and favored by the LED industry, present global 80%LED enterprise adopts sapphire as substrate material, along with the enforcement of eliminating the incandescent light plan both at home and abroad, its demand will constantly increase.
Produce high-purity α-Al both at home and abroad
2O
3The method of powder mainly contains the exsiccated ammonium alum pyrolysis method, aluminium carbonate ammonium pyrolysis method (being called again improvement exsiccated ammonium alum pyrolysis method), alkoxide hydrolysis, choline hydrolysis method, rafifinal activated water solution etc. also has some other method newly developed also to rest on laboratory stage.Wherein the aluminium alcoholates hydrolysis method is the important method that present production purity reaches high-purity alpha-alumina, also is industry research focus processing method, this method technological process environmental protection, and pollution-free, the shortcoming process costs is higher, technological process control is comparatively strict.The aluminum oxide powder product that this legal system is standby, its purity can reach 99.999%, and fine size needs special Countermeasures but granularity reaches nano level.
At present, effective measure of control that the aluminium alcoholates method is produced the employing of alumina in Nano level process mainly contain: (1) liquid reaction phase, the aluminium alcoholates hydrolytic process is introduced macromolecule dispersing agent, adsorb at the hydrolysate colloid surface, cause producing between particle infiltration repulsion potential energy and mix the repulsion energy, the difficulty of reuniting occurs thereby make, with do not add dispersion agent and compare, the product surface rule, granularity is thinner, good dispersity, but the introducing of macromolecule dispersing agent, can bring impurity into unavoidably, dispersion agent has bright excess residual in the roasting stage, thereby affects product purity.Therefore, selecting easily to purify, burn, excess is few, molecular weight is little, low-cost dispersion agent is the researchdevelopment direction; (2) drying stage is the process that very easily produces reunion.In order to reduce reunion, in the industry multiple drying means appears, at present such as supercritical drying, vacuum freeze-drying method, ultrasonic cavitation method, micro-wave drying method etc.With the traditional drying method relatively, these all play to reduce reunites, and reaches the purpose of powder nanometer, but exists technology controlling and process complicated, is difficult for the problems such as industrialization, serialization production, facility investment are large.Comparatively speaking, micro-wave drying method, although the disposable apparatus investment is large, but achievement in research shows that it exists that reaction is fast, productive rate is high, good product quality, convenient post-treatment, energy-conserving and environment-protective, safety, easily realize numerous advantages such as serialization production, it is the industry reform prior development direction, have broad prospect of application, existing microwave drying both at home and abroad prepares the research report of nano aluminium oxide; (3) the aluminium oxide calcining phase inversion stage also is very easily to produce reunion, causes the process of product chap.Conventional stove roasting normally reduces reunion by controlling temperature rise rate and maturing temperature and time, although can reach certain effect, totally there is complex technical process, energy consumption is high, the shortcomings such as easily polluted product, constant product quality be poor have limited its application in the high purity nanometer powders industry.At present, in the high-temperature roasting mode, microwave calcining is as a kind of baking modes of efficient homogenizing, have quick heating, homogeneous heating, energy-conserving and environment-protective, highly effective and safe, can effectively control powder size, be difficult for occuring the advantages such as reunion, at home and abroad ceramic industry, mineral metallurgy industry all are used widely, report in powder industry successful Application such as zirconium oxide in high purity, yttrium oxide, zinc oxide, tricobalt tetroxides is also arranged both at home and abroad, is the direction of the following primary study development of related application industry.
According to the retrieval, prepare in the document and patent of high purity nanometer alumina at alkoxide process, the report of using dispersion agent is a lot, (two one-step hydrolysis are produced research [J] the Chinese journal of scientific instrument .1995 of aluminium oxide nano micro mist such as Ning Guiling etc., 16(1): 314-318), Chinese patent " a kind of nanometer; the preparation method of submicron order aluminum oxide " (CN00125966.0) etc., the dispersion agent of wherein mentioning mainly contains polyoxyethylene glycol, polyvinyl alcohol, acetic acid, paraffin, methyl aceto acetate etc., these high molecular polymers are large except molecular weight, remaining residual object height burns, be difficult for purifying, outside the shortcomings such as easy introducing impurity effect product purity, price is more expensive, increases production cost.
According to the retrieval, the report that domestic and international microwave calcining technology is applied to high purity nanometer powders is more, such as (Preparation of nanosized ZnO by microwave-calcining [J] inorganic chemicals industry .2004,36(5) such as Cao Jun: 31-33), Chinese patent " a kind of method of utilizing microwave calcining to prepare tricobalt tetroxide " (CN201110198914.X) etc. all adopts Microwave Sintering Techniques to prepare powder body material.But its application of producing high purity nanometer alumina powder industry in the aluminium alcoholates hydrolysis method there is not yet report.
Summary of the invention
The objective of the invention is to provide for the deficiencies in the prior art a kind of preparation method of 5N high purity nanometer alumina powder, be characterized in the presence of dispersion agent, will make hydrolysed mix after the reaction of 5N aluminum isopropylate presoma back hydrolysis; Centrifuging obtains hydrated aluminum oxide, and dry in stoving oven, roasting obtains 5N high-purity gamma-Al
2O
3Then powder, continues the intensification roasting and obtains the high-purity α-Al of 5N
2O
3Powder has simple, as to save cost, energy-conserving and environment-protective advantage.
Purpose of the present invention is realized that by following technical measures wherein said raw material umber is molfraction except specified otherwise.
The preparation method of 5N high purity nanometer alumina powder may further comprise the steps:
(1) with 5N aluminum isopropylate presoma: deionized water: dispersion agent is 1: 10～30: 0.5～2 mol ratio, in the reactor of adding with agitator, thermometer and reflux exchanger, in 85～100 ℃ of temperature, stirring, back hydrolysis reaction 3～5h obtain hydrolysed mix;
(2) it is 80～100 ℃ in temperature first with the said hydrolyzed mixture, time 0.5～3h distill out by product Virahol that hydrolysis reaction generates and with the azeotrope solution of water, solution separates through dehydration and obtains Virahol and can be directly used in the synthetic raw material of high puring aluminium isopropoxide; Product obtains hydrated aluminum oxide by centrifuging again, and filtrate is aqueous dispersant, returns step (1) and recycles, and the centrifuging time is 15～30min;
(3) hydrated aluminum oxide that step (2) is obtained changes in the stoving oven, and in 80～110 ℃ of temperature, dry 8～15min at 500～700 ℃ of roasting 25～45min of temperature, obtains 5N high-purity gamma-Al
2O
3Powder, granularity are at 5～50nm, and D50 is 25nm, then, continue to be warming up to 1050～1200 ℃ of roasting 30～50min, obtain the high-purity α-Al of 5N
2O
3Powder, granularity are at 10～100nm, and D50 is 50nm.
Described dispersion agent is at least a in glucose, sucrose, the maltose.
Described stoving oven is microwave baking furnace.
Performance test
1. crystal formation detects: X-ray diffraction instrument D/Max-3B;
2. granularity Detection: particle-size analyzer BI-XDC;
3. specific surface area detects: the full-automatic specific surface of BET (amassing) tester F-Sorb 2400;
4. purity detecting: micro-wave digestion melts sample, and ICP-OES detects.
Test result is as shown in Table 1 below.
The present invention has following advantage:
(1) in disperseing hydrolytic process, introduces aluminium alcoholates at least a as dispersion agent in glucose, sucrose, the maltose, such dispersion agent purity is high, molecular weight is little, the excess amount of burning is few, low price, dispersing property is good, is conducive to reduce the products production cost, improves product purity, the product granularity that obtains is thin, narrowly distributing, good dispersity, regular shape.
(2) at high purity nanometer alumina phase inversion roasting process, adopt the microwave calcining technology, can effectively control product granularity, the difficult reunion, so that product granularity reaches nano level, and narrowly distributing, good dispersity also has the advantage of energy-conserving and environment-protective, highly effective and safe in addition.Two kinds of techniques unite use, can not only obtain 5N purity high-alumina powder, and product granularity reaches nano level, obtain 5N high-purity gamma-Al
2O
3Powder, granularity 5～50nm, D50(25nm), obtain the high-purity α-Al of 5N
2O
3Powder, granularity 10～100nm, D50(50nm).
Embodiment
By the following examples the present invention is carried out concrete description; be necessary to be pointed out that at this present embodiment only is used for the present invention is further specified; can not be interpreted as the restriction to the invention protection domain, some nonessential improvement and adjustment that the person skilled in the art in this field can make according to the content of the invention described above.
Embodiment 1
In the reactor that joins in the 4.5L deionized water with stirring, thermometer and return channel, then 2.25Kg glucose is dissolved in the deionized water, after stirring, be warming up to 85 ℃, add again 5N aluminum isopropylate 5.1Kg, stirring, back hydrolysis reaction 3h are aluminum isopropylate: deionized water: the reaction in 1: 10: 0.5 of the mol ratio of glucose.After reaction finishes, elder generation's Distillation recovery by product Virahol and with the azeotrope of water, distillation time is 1.5h, centrifugation obtains hydrolysate hydrated aluminum oxide and glucose solution again, the centrifuging time is 20min, and glucose solution returns hydrolyzation system and recycles; Product filters the hydrated aluminum oxide that obtains and changes (2.45GHz, 0.3～2.85Kw is adjustable) in the microwave baking furnace over to, is warming up to 90 ℃, behind the freeze-day with constant temperature 15min, is warming up at 600 ℃ of roasting 40min, obtains γ type Al
2O
3Then powder, continues to be warming up to 1050 ℃ of roasting 40min, obtains α type Al
2O
3Powder.
Embodiment 2
In the reactor that joins in the 13.5L deionized water with stirring, thermometer and return channel, then with the 8.55Kg sucrose dissolved in deionized water, after stirring, be warming up to 85 ℃, add again 5N aluminum isopropylate 5.1Kg, stirring, back hydrolysis reaction 4h are aluminum isopropylate: deionized water: the reaction in 1: 30: 1 of the mol ratio of sucrose.。After reaction finishes, first Distillation recovery by product Virahol and with the azeotrope of water, distillation time is 40min, centrifugation obtains hydrolysate hydrated aluminum oxide and sucrose solution again, the centrifuging time is 15min, sucrose solution returns hydrolyzation system and recycles; Product filters the hydrated aluminum oxide that obtains and changes (2.45GHz, 0.3～2.85Kw is adjustable) in the microwave baking furnace over to, is warming up to 85 ℃, behind the freeze-day with constant temperature 15min, is warming up at 700 ℃ of roasting 35min, obtains γ type Al
2O
3Then powder, continues to be warming up to 1100 ℃ of roasting 40min, obtains α type Al
2O
3Powder.
Embodiment 3
In the reactor that joins in the 6.75L deionized water with stirring, thermometer and return channel, then 4.5Kg maltose is dissolved in the deionized water, after stirring, be warming up to 85 ℃, add again 5N aluminum isopropylate 5.1Kg, stirring, back hydrolysis reaction 3.5h are aluminum isopropylate: deionized water: the reaction in 1: 15: 0.5 of the mol ratio of sucrose.。After reaction finishes, first Distillation recovery by product Virahol and with the azeotrope of water, distillation time is 1h, centrifugation obtains hydrolysate hydrated aluminum oxide and maltose solution again, the centrifuging time is that the 25min sucrose solution returns hydrolyzation system and recycles; Product filters the hydrated aluminum oxide that obtains and changes (2.45GHz, 0.3～2.85Kw is adjustable) in the microwave baking furnace over to, is warming up to 95 ℃, behind the freeze-day with constant temperature 15min, is warming up at 600 ℃ of roasting 30min, obtains γ type Al
2O
3Then powder, continues to be warming up to 1150 ℃ of roasting 30min, obtains α type Al
2O
3Powder.
Example 4
In the reactor that joins in the 11.25L deionized water with stirring, thermometer and return channel, then with 4.5Kg glucose sugar and 8.55Kg sucrose dissolved in deionized water, after stirring, be warming up to 85 ℃, add again 5N aluminum isopropylate 5.1Kg, stirring, back hydrolysis reaction 3.5h are aluminum isopropylate: deionized water: glucose: the mol ratio of sucrose 1: 25: 1: 1 reaction.。After reaction finishes, elder generation's Distillation recovery by product Virahol and with the azeotrope of water, distillation time is 1h, and centrifugation obtains hydrolysate hydrated aluminum oxide, dextrose plus saccharose solution again, and the centrifuging time is that the 25min sucrose solution returns hydrolyzation system and recycles; Product filters the hydrated aluminum oxide that obtains and changes (2.45GHz, 0.3～2.85Kw is adjustable) in the microwave baking furnace over to, is warming up to 95 ℃, behind the freeze-day with constant temperature 15min, is warming up at 600 ℃ of roasting 30min, obtains γ type Al
2O
3Then powder, continues to be warming up to 1150 ℃ of roasting 30min, obtains α type Al
2O
3Powder.
Table 1: the Al that makes for example 4
2O
3The product analysis detected result
Claims (3)
1. the preparation method of a 5N high purity nanometer alumina powder is characterized in that may further comprise the steps:
(1) with 5N aluminum isopropylate presoma: deionized water: dispersion agent is 1: 10～30: 0.5～2 mol ratio, in the reactor of adding with agitator, thermometer and reflux exchanger, in 85～100 ℃ of temperature, stirring, back hydrolysis reaction 3～5h obtain hydrolysed mix;
(2) it is 80～100 ℃ in temperature first with the said hydrolyzed mixture, time 0.5～3h distill out by product Virahol that hydrolysis reaction generates and with the azeotrope solution of water, solution separates through dehydration and obtains Virahol and can be directly used in the synthetic raw material of high puring aluminium isopropoxide; Product obtains hydrated aluminum oxide by centrifuging again, and filtrate is aqueous dispersant, returns step (1) and recycles, and the centrifuging time is 15～30min;
(3) hydrated aluminum oxide that step (2) is obtained changes in the stoving oven, and in 80～110 ℃ of temperature, dry 8～15min at 500～700 ℃ of roasting 25～45min of temperature, obtains 5N high-purity gamma-Al
2O
3Powder, granularity are at 5～50nm, and D50 is 25nm, then, continue to be warming up to 1050～1200 ℃ of roasting 30～50min, obtain the high-purity α-Al of 5N
2O
3Powder, granularity are at 10～100nm, and D50 is 50nm.
2. the preparation method of 5N high purity nanometer alumina powder as claimed in claim 1 is characterized in that dispersion agent is at least a in glucose, sucrose, the maltose.
3. the preparation method of 5N high purity nanometer alumina powder as claimed in claim 1 is characterized in that stoving oven is microwave baking furnace.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104085908A (en) * | 2014-07-16 | 2014-10-08 | 李春松 | Method for preparing high-purity aluminium oxide |
| CN104130004A (en) * | 2014-07-07 | 2014-11-05 | 山东理工大学 | Preparation method of high-strength block-shaped porous alumina nano-ceramic |
| CN104261447A (en) * | 2014-09-23 | 2015-01-07 | 成都冠禹科技有限公司 | Production method of 5N high-purity alpha alumina powder |
| CN105643480A (en) * | 2016-01-14 | 2016-06-08 | 洛阳三睿宝纳米科技有限公司 | Nano fiber oilstone |
| CN106747358A (en) * | 2016-12-27 | 2017-05-31 | 扬州中天利新材料股份有限公司 | Purity is the preparation method of the series of oxidation aluminium superfines of 5N |
| CN112939045A (en) * | 2021-02-03 | 2021-06-11 | 浙江爱科新材料有限公司 | Preparation method of superfine high-purity gamma-alumina |
| CN113912092A (en) * | 2021-12-01 | 2022-01-11 | 扬州中天利新材料股份有限公司 | Preparation method of alumina ultrafine powder with purity of 5N |
| CN114524449A (en) * | 2022-03-15 | 2022-05-24 | 先导薄膜材料（广东）有限公司 | Preparation method of high-purity alumina powder |
| CN115784280A (en) * | 2022-12-21 | 2023-03-14 | 江苏金石研磨有限公司 | Preparation method of low-cost nano alumina powder |
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| CN104130004A (en) * | 2014-07-07 | 2014-11-05 | 山东理工大学 | Preparation method of high-strength block-shaped porous alumina nano-ceramic |
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| CN105643480A (en) * | 2016-01-14 | 2016-06-08 | 洛阳三睿宝纳米科技有限公司 | Nano fiber oilstone |
| CN106747358A (en) * | 2016-12-27 | 2017-05-31 | 扬州中天利新材料股份有限公司 | Purity is the preparation method of the series of oxidation aluminium superfines of 5N |
| CN112939045A (en) * | 2021-02-03 | 2021-06-11 | 浙江爱科新材料有限公司 | Preparation method of superfine high-purity gamma-alumina |
| CN113912092A (en) * | 2021-12-01 | 2022-01-11 | 扬州中天利新材料股份有限公司 | Preparation method of alumina ultrafine powder with purity of 5N |
| CN114524449A (en) * | 2022-03-15 | 2022-05-24 | 先导薄膜材料（广东）有限公司 | Preparation method of high-purity alumina powder |
| CN115784280A (en) * | 2022-12-21 | 2023-03-14 | 江苏金石研磨有限公司 | Preparation method of low-cost nano alumina powder |
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