CN106276993B - A kind of nano aluminium oxide thickened pulp and preparation method thereof - Google Patents
A kind of nano aluminium oxide thickened pulp and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to field of nanometer material technology, specially a kind of nano aluminium oxide thickened pulp and preparation method thereof.The thickened pulp is made up of the average grain diameter of primary particle in below 50nm 15~20 parts of 0.3~0.6 part of 0.1~0.3 part of 5~10 parts of 100 parts of nano aluminium oxide, organic inhibitor, rust resisting pigment, auxiliary agent, organic solvent；Each component is weighed in proportion, and organic inhibitor, rust resisting pigment, auxiliary agent are well mixed with organic solvent；Nano alumina powder is gradually added into during high speed dispersor is not stalled and moved, after all required nano alumina powders are added, is further continued for disperseing 5~30 minutes, dispersing speed is 1500~2500rpm；The nanometer alumina slurry of gained is ground 1~10 hour in ball mill or sand mill, makes its average grain diameter below 100 nanometers, nano aluminium oxide thickened pulp is obtained.The thickened pulp good dispersion, storage stabilization, solids content height, viscosity are low, compatibility is strong, have anti-corrosion function concurrently.
Description
Technical field
The invention belongs to field of nanometer material technology, specially a kind of nano aluminium oxide thickened pulp and preparation method thereof.
Background technology
Nano aluminium oxide has important application in fields such as ceramics, coating, fiber, rubber.It has been found that nanometer Al2O3
Powder has very strong absorbability to below 250nm ultraviolet light, if adding in coating, it is likely that improve the anti-of organic coating
Aging ability；If their wearability can be improved by adding in rubber or plastics；If adding in sunblock lotion, cosmetics, it can
Improve its uvioresistant performance.With containing nanometer Al2O3The clothing that is made of fiber there is infrared absorption function.While nanometer Al2O3
Polishing fluid can also as high optics glass and jewel polishing.But because the specific surface area of nano aluminium oxide is big, surface hangs
Floating key is more, is particularly easy to form aggregate, under the generation of aggregate will make effect of the nano aluminium oxide in decentralized medium obvious
Drop.Therefore nano aluminium oxide can effectively stable dispersion be nano aluminium oxide apply key issue.
United States Patent (USP) USP5,877,106 methods for referring to preparation 50~100nm aluminum oxide, thus nano aluminium oxide preparation
Catalyst and catalyst carrier can be used for engine exhaust gas treatment.United States Patent (USP) USP 5,972,820 reports one kind and prepared surely
Method of the fixed average grain diameter in 1~50nm aluminum oxide.The method for how disperseing nano aluminium oxide is not all mentioned in these patents.
As a rule, the successful use of nano alumina particles is strongly dependent on nano-particle and is scattered in liquid phase
Ability.Some special application fields, such as：Cosmetics, coating, weaving, polishing and catalysis etc., are required for particle to disperse well
And stably exist, it is impossible to which the phenomenon such as occur reuniting, and the activity of nano-particle could be shown well.It is such in order to meet
Need, someone is specialized in now and reapplied after how nano powder being prepared into the thickened pulp of high degree of dispersion.
The content of the invention
It is an object of the invention to provide a kind of nano aluminium oxide thickened pulp and preparation method thereof, thickened pulp dispersiveness
Good, storage is stable, solids content is high, viscosity is low, compatibility is strong, and with anti-corrosion function.
The technical scheme is that：
A kind of nano aluminium oxide thickened pulp, is counted by weight, and the thickened pulp is by the average grain diameter of primary particle in 50nm
Following 100 parts of nano aluminium oxide, 5~10 parts of organic inhibitor, 0.1~0.3 part of rust resisting pigment, 0.3~0.6 part of auxiliary agent, have
15~20 parts of compositions of machine solvent；
Organic inhibitor is to nitro sodium laurate, to nitro potassium laurate, to nitro sodium palmitate, to nitro palmitic acid
Potassium, to nitro odium stearate or to nitro potassium stearate, molecular structure is as follows：
Wherein, M represents sodium ion or potassium ion, and R represents laurate, palmitic acid or stearic long-chain；
Or, organic inhibitor is a nitro sodium laurate, a nitro potassium laurate, a nitro sodium palmitate, a nitro
Palmitic acid potassium, a nitro odium stearate or a nitro potassium stearate, molecular structure are as follows：
Wherein, M represents sodium ion or potassium ion, and R represents laurate, palmitic acid or stearic long-chain；
Rust resisting pigment is the one or more of the phosphate containing strontium, the phosphate containing zinc, phosphate containing aluminium；It is organic
Solvent is the mixed solvent of benzene class organic solvent, based organic solvent and organic solvent of ketone.Phosphate containing strontium, such as：Germany
HEUCOPHOS SRPP or HEUCOPHOS SAPP of Heubach companies etc.；Phosphate containing zinc, such as：Zinc orthophosphate or
Polyphosphoric acids zinc etc.；Phosphate containing aluminium, such as：Aluminium triphosphate etc..
General organic inhibitor is mainly element containing unpaired electron, such as：O, N, S compound and it is various contain polarized
The chemical substance of group, particularly containing amino, aldehyde radical, carboxyl, hydroxyl, sulfydryl various compounds.And the present invention is to nitro
Or the organic inhibitor of a nitro is to contain-C6H5NO2The compound of structure, it is with commonly containing NO3 -（Nitrate anion）、NO2 -（Nitrous
Acid group）And other organic inhibitors containing N are dramatically different.The organic inhibitor of the present invention can act synergistically with rust resisting pigment, should
Phosphating coat can be formed with metal interface by using in coating, play corrosion-resisting function.
Described nano aluminium oxide thickened pulp, the weight of benzene class organic solvent, based organic solvent and organic solvent of ketone
Ratio is 1：（3~6）：（11~13）, certain froth breaking effect can be played, so as to omit defoamer.Also, benzene class is organic molten
Agent consumption is less, is conducive to environmental protection.
Described nano aluminium oxide thickened pulp, benzene class organic solvent is toluene or dimethylbenzene, and based organic solvent is acetic acid
Ethyl ester or butyl acetate, organic solvent of ketone are acetone or cyclohexanone.
Described nano aluminium oxide thickened pulp, auxiliary agent is the anti-settling agent, the wetting and dispersing that are commonly used in dope preparing process
Agent and levelling agent.
The preparation method of described nano aluminium oxide thickened pulp, is comprised the following steps that：
（1）Each component is weighed in proportion；
（2）Organic inhibitor, rust resisting pigment, auxiliary agent are well mixed with organic solvent；
（3）Nano alumina powder is gradually added into during high speed dispersor is not stalled and moved, all required nano aluminium oxides
After powder is added, it is further continued for disperseing 5~30 minutes, dispersing speed is 1500~2500rpm；
（4）The nanometer alumina slurry of gained is ground 1~10 hour in ball mill or sand mill, makes its average grain diameter
Below 100 nanometers（Generally 10~100 nanometers）, obtain nano aluminium oxide thickened pulp.
In the present invention, organic inhibitor to nitro or a nitro is connected in last alkyl with linear carboxylate
On the phenyl ring of ester.Briefly, it is on the phenyl ring in carboxylate compounds to nitro or a nitro.
In above-mentioned chemical equation, n=8,12,16 respectively correspond to laurate, palmitic acid and stearic acid, M represent Na or
K。
Grinding distribution equipment of the present invention is the common equipment in paint manufacturing process, including high speed dispersor, sand mill and
Ball mill etc..
Advantages of the present invention and have the beneficial effect that：
1st, the present invention have developed a kind of the nano oxidized of high solids content according to the present Research of nano-alumina dispersions
Aluminium thickened pulp, disperses to nano aluminium oxide energy stable and uniform to exist, forms high degree of dispersion, homogenization and stabilized dispersion
System, additive composition used is simple, does not have any pollution to human body and environment, and the preparation technology of the thickened pulp is very simple
It is single, the function modified effect of nano material has greatly been played, and the scattered physical efficiency realizes industrialized production.
2nd, the present invention is due to the technical scheme using nano material, rust resisting pigment and organic inhibitor compound use so that
The permeability resistance of nano aluminium oxide thickened pulp, corrosion resistance are significantly improved.Meanwhile, organic inhibitor used, rust resisting pigment are nontoxic,
Be conducive to environmental protection.
3rd, nano aluminium oxide thickened pulp of the present invention has excellent storage stability, the features such as being difficult to sink to the bottom.Six can at least be kept
Do not precipitate within individual month, it is not stratified, best can meet the requirement of bin stability more than a year and a half.
4th, using the nano aluminium oxide thickened pulp good dispersion prepared of technology of the present invention, particle mean size 100nm with
Under, the problem of nano powder is very easily reunited is solved, the nano-meter characteristic that nano aluminium oxide can be made excellent fully demonstrates out.
5th, the nano aluminium oxide thickened pulp solid content that the present invention is prepared reaches as high as more than 80%, and the thickened pulp is viscous
Degree is low（Less than 500 mPas）, it is easy to use, be a kind of high concentration high dispersive system, improve the use effect of nano aluminium oxide
Rate.The nano aluminium oxide thickened pulp is applied to coating, ceramics, rubber, daily-use chemical industry, magnetic material, electronic material, ink, spinning
Knit, the multiple fields such as cosmetics and adhesive.
Embodiment
Below, the present invention is further elaborated on by embodiment.
Embodiment 1
Count by weight, nano aluminium oxide thickened pulp is by the average grain diameter of primary particle in the nano oxidized of below 50nm
100 parts of aluminium, 8 parts of organic inhibitor, 0.2 part of rust resisting pigment, 0.5 part of auxiliary agent, 18 parts of compositions of organic solvent.Wherein, organic inhibition
Agent is that, to nitro sodium laurate, rust resisting pigment is the phosphate SRPP containing strontium, and auxiliary agent is：BYK-P104S wetting dispersing agents（Moral
State Bi Ke chemistry BYK companies）0.2 part, BYK-310 levelling agents（German Bi Ke chemistry BYK companies）0.2 part, BENTONE 34 has
Machine bentonite anti-settling agent（RHEOX companies of the U.S.）0.1 part, organic solvent is：1 part of toluene, 5 parts of ethyl acetate, 12 parts of acetone.
The preparation method of nano aluminium oxide thickened pulp, is comprised the following steps that：
（1）Each component is weighed in proportion；
（2）Organic inhibitor, rust resisting pigment, auxiliary agent are well mixed with organic solvent；
（3）Nano alumina powder is gradually added into during high speed dispersor is not stalled and moved, all required nano aluminium oxides
After powder is added, it is further continued for disperseing 15 minutes, dispersing speed is 2000rpm；
（4）The nanometer alumina slurry of gained is ground 5 hours in ball mill or sand mill, makes its average grain diameter 80
Nanometer is following, obtains nano aluminium oxide thickened pulp.
Embodiment 2
Count by weight, nano aluminium oxide thickened pulp is by the average grain diameter of primary particle in the nano oxidized of below 50nm
100 parts of aluminium, 5 parts of organic inhibitor, 0.3 part of rust resisting pigment, 0.3 part of auxiliary agent, 15 parts of compositions of organic solvent.Wherein, organic inhibition
Agent is that, to nitro sodium palmitate, rust resisting pigment is the phosphate SAPP containing strontium, and auxiliary agent is：DISPERBYK-106 wetting dispersing agents
（German Bi Ke chemistry BYK companies）0.1 part, BYK- VP-354 levelling agents（German Bi Ke chemistry BYK companies）0.1 part,
The organobentonite anti-settling agents of BENTONE 27（RHEOX companies of the U.S.）0.1 part, organic solvent is：1 part of dimethylbenzene, butyl acetate 3
Part, 11 parts of cyclohexanone.
The preparation method of nano aluminium oxide thickened pulp, is comprised the following steps that：
（1）Each component is weighed in proportion；
（2）Organic inhibitor, rust resisting pigment, auxiliary agent are well mixed with organic solvent；
（3）Nano alumina powder is gradually added into during high speed dispersor is not stalled and moved, all required nano aluminium oxides
After powder is added, it is further continued for disperseing 10 minutes, dispersing speed is 2500rpm；
（4）The nanometer alumina slurry of gained is ground 6 hours in ball mill or sand mill, makes its average grain diameter 60
Nanometer is following, obtains nano aluminium oxide thickened pulp.
Embodiment 3
Count by weight, nano aluminium oxide thickened pulp is by the average grain diameter of primary particle in the nano oxidized of below 50nm
100 parts of aluminium, 10 parts of organic inhibitor, 0.1 part of rust resisting pigment, 0.6 part of auxiliary agent, 20 parts of compositions of organic solvent.Wherein, organic inhibition
Agent is that rust resisting pigment is zinc orthophosphate, and auxiliary agent is to nitro odium stearate：DISPERBYK-110 wetting dispersing agents（German Bi Ke
Chemical BYK companies）0.2 part, BYK-310 levelling agents（German Bi Ke chemistry BYK companies）0.2 part, BENTONE SD-2 organic bentonites
The native anti-settling agent of profit（RHEOX companies of the U.S.）0.2 part, organic solvent is：1 part of toluene, 6 parts of butyl acetate, 13 parts of cyclohexanone.
The preparation method of nano aluminium oxide thickened pulp, is comprised the following steps that：
（1）Each component is weighed in proportion；
（2）Organic inhibitor, rust resisting pigment, auxiliary agent are well mixed with organic solvent；
（3）Nano alumina powder is gradually added into during high speed dispersor is not stalled and moved, all required nano aluminium oxides
After powder is added, it is further continued for disperseing 30 minutes, dispersing speed is 1500rpm；
（4）The nanometer alumina slurry of gained is ground 4 hours in ball mill or sand mill, makes its average grain diameter 40
Nanometer is following, obtains nano aluminium oxide thickened pulp.
Embodiment 4
Count by weight, nano aluminium oxide thickened pulp is by the average grain diameter of primary particle in the nano oxidized of below 50nm
100 parts of aluminium, 7 parts of organic inhibitor, 0.2 part of rust resisting pigment, 0.4 part of auxiliary agent, 17 parts of compositions of organic solvent.Wherein, organic inhibition
Agent be between nitro potassium laurate, rust resisting pigment is polyphosphoric acids zinc, and auxiliary agent is：BYK-P104S wetting dispersing agents（German Bi Ke
Chemical BYK companies）0.2 part, BYK-310 levelling agents（German Bi Ke chemistry BYK companies）0.1 part, the organic swellings of BENTONE 34
Native anti-settling agent（RHEOX companies of the U.S.）0.1 part, organic solvent is：1 part of dimethylbenzene, 5 parts of ethyl acetate, 11 parts of acetone.
The preparation method of nano aluminium oxide thickened pulp, is comprised the following steps that：
（1）Each component is weighed in proportion；
（2）Organic inhibitor, rust resisting pigment, auxiliary agent are well mixed with organic solvent；
（3）Nano alumina powder is gradually added into during high speed dispersor is not stalled and moved, all required nano aluminium oxides
After powder is added, it is further continued for disperseing 20 minutes, dispersing speed is 2000rpm；
（4）The nanometer alumina slurry of gained is ground 8 hours in ball mill or sand mill, makes its average grain diameter 80
Nanometer is following, obtains nano aluminium oxide thickened pulp.
Embodiment 5
Count by weight, nano aluminium oxide thickened pulp is by the average grain diameter of primary particle in the nano oxidized of below 50nm
100 parts of aluminium, 6 parts of organic inhibitor, 0.3 part of rust resisting pigment, 0.4 part of auxiliary agent, 19 parts of compositions of organic solvent.Wherein, organic inhibition
Agent be between nitro palmitic acid potassium, rust resisting pigment is aluminium triphosphate, and auxiliary agent is：DISPERBYK-106 wetting dispersing agents（Germany
Bi Ke chemistry BYK companies）0.1 part, BYK- VP-354 levelling agents（German Bi Ke chemistry BYK companies）0.2 part, BENTONE 27
Organobentonite anti-settling agent（RHEOX companies of the U.S.）0.1 part, organic solvent is：1 part of toluene, 6 parts of ethyl acetate, 12 parts of acetone.
The preparation method of nano aluminium oxide thickened pulp, is comprised the following steps that：
（1）Each component is weighed in proportion；
（2）Organic inhibitor, rust resisting pigment, auxiliary agent are well mixed with organic solvent；
（3）Nano alumina powder is gradually added into during high speed dispersor is not stalled and moved, all required nano aluminium oxides
After powder is added, it is further continued for disperseing 5 minutes, dispersing speed is 2500rpm；
（4）The nanometer alumina slurry of gained is ground 3 hours in ball mill or sand mill, makes its average grain diameter 60
Nanometer is following, obtains nano aluminium oxide thickened pulp.
Embodiment 6
Count by weight, nano aluminium oxide thickened pulp is by the average grain diameter of primary particle in the nano oxidized of below 50nm
100 parts of aluminium, 9 parts of organic inhibitor, 0.1 part of rust resisting pigment, 0.5 part of auxiliary agent, 16 parts of compositions of organic solvent.Wherein, organic inhibition
Agent be between nitro potassium stearate, rust resisting pigment is aluminium triphosphate, and auxiliary agent is：DISPERBYK-110 wetting dispersing agents（Germany finishes
Gram chemistry BYK companies）0.2 part, BYK-310 levelling agents（German Bi Ke chemistry BYK companies）0.1 part, BENTONE SD-2 it is organic
Bentonite anti-settling agent（RHEOX companies of the U.S.）0.2 part, organic solvent is：1 part of dimethylbenzene, 4 parts of butyl acetate, 11 parts of cyclohexanone.
The preparation method of nano aluminium oxide thickened pulp, is comprised the following steps that：
（1）Each component is weighed in proportion；
（2）Organic inhibitor, rust resisting pigment, auxiliary agent are well mixed with organic solvent；
（3）Nano alumina powder is gradually added into during high speed dispersor is not stalled and moved, all required nano aluminium oxides
After powder is added, it is further continued for disperseing 25 minutes, dispersing speed is 1500rpm；
（4）The nanometer alumina slurry of gained is ground 9 hours in ball mill or sand mill, makes its average grain diameter 40
Nanometer is following, obtains nano aluminium oxide thickened pulp.
Table 1
| The average grain diameter of nano aluminium oxide（nm） | The weight ratio of nano aluminium oxide（%） | Bin stability, level | Salt fog resistance, level | Dispersiveness | |
| Embodiment 1 | 50 | 78.9 | 10 | 1 | Be uniformly dispersed, soilless sticking phenomenon |
| Embodiment 2 | 30 | 82.9 | 8 | 0 | Be uniformly dispersed, soilless sticking phenomenon |
| Embodiment 3 | 10 | 76.5 | 6 | 0 | Be uniformly dispersed, soilless sticking phenomenon |
| Embodiment 4 | 50 | 80.3 | 9 | 1 | Be uniformly dispersed, soilless sticking phenomenon |
| Embodiment 5 | 30 | 79.6 | 8 | 0 | Be uniformly dispersed, soilless sticking phenomenon |
| Embodiment 6 | 10 | 79.6 | 8 | 0 | Be uniformly dispersed, soilless sticking phenomenon |
As it can be seen from table 1 nano aluminium oxide thickened pulp of the present invention has preferable bin stability, less average grain
Degree and higher salt fog resistance.
Application examples
The present invention is used to prepare the Chrome-free nano composite epoxy coating with high corrosion-resistant, is made up of, prepares two components
Process is as follows：
（1）The preparation method of component one：50kg bisphenol A type epoxy resin E-51 are added in dispersion cylinder, acetone is added
26kg, then adds the nano aluminium oxide thickened pulp 3kg of above-described embodiment 1~6, scattered 10 points in 400rpm using high speed dispersor
Clock, adds titanium dioxide 6kg, talcum powder 15kg, scattered 20 minutes with high speed dispersor 500rpm；Then ground with horizontal sand mill
Mill 2 hours, to fineness for after 25 microns, filtering, packaging are prepared into the component one of Chrome-free nano composite epoxy coating.Due to adopting
With the nano aluminium oxide thickened pulp of embodiment 1~6, the preparation process of component one is greatly simplified, production efficiency is improved, it is possible to
Reduce cost.
（2）The preparation method of component two：80kg curing agent TY203 is added in dispersion cylinder, 20kg cyclohexanone is added, used
Filtering, packaging after high speed dispersor 500rpm is scattered 15 minutes.
Two components press component one：Component two=4：1（Weight ratio）Chrome-free nano composite epoxy coating is made after proportioning stirring.
Spray and dried 7 days under the Chrome-free nano composite epoxy coating, normal temperature on 75mm × 150mm × 2mm LY12 aluminium alloys, dry film
Thickness is 20 ± 5 μm.
Result of implementation shows, in traditional coating, including fluorocarbon coating, polyurethane coating, epoxy coating, acrylic acid are applied
After material etc., the nano material thickened pulp for adding 0.5~3wt%, performance will improve 30%~50%, be primarily adapted for use in：Industrial heavy antisepsis
Coating, Heavy-duty Coatings In Ocean Chemical Industry and aircraft coating, high iron-dope, wind-powered electricity generation coating, healthy household coating etc., effect is particularly significant.
Claims (5)
1. a kind of nano aluminium oxide thickened pulp, it is characterised in that：Count by weight, the thickened pulp by primary particle average grain
Footpath below 50nm 0.1~0.3 part of 5~10 parts of 100 parts of nano aluminium oxide, organic inhibitor, rust resisting pigment, auxiliary agent 0.3~
0.6 part, 15~20 parts of compositions of organic solvent；
Organic inhibitor be to nitro sodium laurate, to nitro potassium laurate, to nitro sodium palmitate, to nitro palmitic acid potassium,
To nitro odium stearate or to nitro potassium stearate, molecular structure is as follows：
Wherein, M represents sodium ion or potassium ion, and R represents laurate, palmitic acid or stearic long-chain；
Or, organic inhibitor is a nitro sodium laurate, a nitro potassium laurate, a nitro sodium palmitate, a nitro palmitin
Sour potassium, a nitro odium stearate or a nitro potassium stearate, molecular structure are as follows：
Wherein, M represents sodium ion or potassium ion, and R represents laurate, palmitic acid or stearic long-chain；
Rust resisting pigment is the one or more of the phosphate containing strontium, the phosphate containing zinc, phosphate containing aluminium；Organic solvent
It is the mixed solvent of benzene class organic solvent, based organic solvent and organic solvent of ketone.
2. according to the nano aluminium oxide thickened pulp described in claim 1, it is characterised in that：Benzene class organic solvent, esters are organic molten
The part by weight of agent and organic solvent of ketone is 1：（3~6）：（11~13）.
3. according to the nano aluminium oxide thickened pulp described in claim 1 or 2, it is characterised in that：Benzene class organic solvent be toluene or
Dimethylbenzene, based organic solvent is ethyl acetate or butyl acetate, and organic solvent of ketone is acetone or cyclohexanone.
4. according to the nano aluminium oxide thickened pulp described in claim 1, it is characterised in that：Auxiliary agent is anti-settling agent, wetting dispersing agent
And levelling agent.
5. the preparation method of the nano aluminium oxide thickened pulp described in a kind of claim 1, it is characterised in that comprise the following steps that：
（1）Each component is weighed in proportion；
（2）Organic inhibitor, rust resisting pigment, auxiliary agent are well mixed with organic solvent；
（3）Nano alumina powder is gradually added into during high speed dispersor is not stalled and moved, all required nano alumina powders add
After entering, it is further continued for disperseing 5~30 minutes, dispersing speed is 1500~2500rpm；
（4）The nanometer alumina slurry of gained is ground 1~10 hour in ball mill or sand mill, its average grain diameter is existed
Less than 100 nanometers, obtain nano aluminium oxide thickened pulp.
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| CN1304294C (en) * | 2004-08-03 | 2007-03-14 | 中国科学院过程工程研究所 | Big pore volume and high specific surface gamma-Al2O3 nanometer fibre powder preparation method |
| CN100346873C (en) * | 2005-09-09 | 2007-11-07 | 清华大学 | Method for preparing large pore capacity, high specific surface area alumina |
| CN100469699C (en) * | 2005-12-27 | 2009-03-18 | 上海材料研究所 | Method for the treatment of aluminum oxide powder |
| CN1868885B (en) * | 2006-05-12 | 2010-07-21 | 广西民族大学 | Self-dispersion type nanometer gamma A100H and its preparation method and use |
| CN100409927C (en) * | 2006-09-01 | 2008-08-13 | 哈尔滨工业大学 | Aluminium oxide granule/fragrant polyamide blending isolation film and preparation process thereof |
| CN101215430B (en) * | 2007-12-29 | 2010-07-21 | 株洲时代新材料科技股份有限公司 | Stabilization dispersion treatment method for nano aluminum oxide in organic solvent |
| US9023145B2 (en) * | 2008-02-12 | 2015-05-05 | Bunge Amorphic Solutions Llc | Aluminum phosphate or polyphosphate compositions |
| CN102030351B (en) * | 2009-09-24 | 2012-08-15 | 中国石油化工股份有限公司 | Macroporous aluminum oxide with bimodal pore distribution and preparation method thereof |
| CN101792164B (en) * | 2009-11-19 | 2012-02-15 | 国家纳米科学中心 | Method for preparing nano aluminum oxide through vacuum freeze drying technology |
| CN102229436B (en) * | 2011-06-03 | 2013-06-19 | 浙江工业大学 | Preparation method of gamma-aluminium oxide (Al2O3) nanofiber |
| CN103387250B (en) * | 2013-08-23 | 2015-11-18 | 厦门大学 | A kind of preparation method of gama-alumina |
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