CN103496724A - Preparation method of nano alumina sol and gel - Google Patents
Preparation method of nano alumina sol and gel Download PDFInfo
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Abstract
The invention provides a preparation method of nano alumina sol and gel, nano alumina particles are used as a raw material, lactic acid is used as a dispersing agent, and the high-solid-content nano alumina sol is obtained by combination of high speed stirring and dispersion by using a high-energy ball mill; under stirring, the prepared nano alumina sol is added with a certain amount of a hexamethylenetetramine water solution, and the nano alumina gel is obtained by heating for a certain time for gelatinization. The preparation method is simple and easy, the solid content of the nano alumina sol prepared by dispersing is equal to or more than 30%, and the nano alumina sol is small in particle size and uniform in distribution, and can stably exist for a long time in water.
Description
Technical field
The present invention relates to the preparation method of a kind of nano aluminium oxide colloidal sol and gel, belong to chemical technology field.
Background technology
Nano aluminium oxide colloidal sol has excellent physicochemical property, and purposes is extremely widely arranged in productive life, is used to make catalyzer and carrier, fine ceramics, fiber reinforcement alumina ceramic composite material, new coating.But, because the nano aluminium oxide particle diameter is little, specific surface area and surface can be all very large, be easy to reunite, solid content is difficult to improve.Considerably less about nano aluminium oxide colloidal sol, the gel research report of high solids content both at home and abroad, according to correlative study, major cause is that the solubleness of aluminum oxide in water is very limited.
At present, relate to the technology of preparing at nano aluminium oxide colloidal sol about the patent of nano aluminium oxide colloidal sol more both at home and abroad more.In the preparation method of alumina sol, usually take organic alkoxide or inorganic salt master is raw material.The organic salt raw material method that aluminum isopropylate is raw material as take, the nano aluminium oxide colloidal sol that this kind of method prepared is expensive, makes the application of sol-gel method be subject to certain limitation; Another kind method is with the inorganic salt raw material method, and metallic aluminium is dissolved in hydrochloric acid or aluminum chloride, obtains water white aluminium colloidal sol.Perhaps that aluminum nitrate and ammonium citrate is soluble in water according to a certain ratio, with concentrated nitric acid or strong aqua regulator solution pH value, can obtain aluminium colloidal sol.These two kinds of preparation method's preparation process are large to environmental hazard, and cost is high, and it is low finally to make nano aluminium oxide colloidal sol solid content, generally lower than 20wt%.Chinese patent CN201210120945.8 discloses a kind of nano oxidized aluminum slurry for preparing stable dispersion by sol-gel method, and the solid content of alumina sol is up to 13wt%.Chinese patent CN201010274945.4 discloses a kind ofly take boehmite as raw material, disperse and the regulator solution pH value makes nano aluminium oxide colloidal sol to 2-5, but the maximum concentration of nano aluminium oxide is no more than 25wt%.At present, in the method for document and patent report, the solid content of the nano aluminium oxide colloidal sol of preparation is unsatisfactory.
Summary of the invention
The object of the invention is to overcome the prior art deficiency, provide that a kind of environmental friendliness, nano aluminium oxide particle diameter are little, size distribution evenly, solid content >=30%[solid content=nano aluminium oxide quality/(total mass of nano aluminium oxide and deionized water)] colloidal sol and the preparation method of gel.
Technical solution of the present invention: a kind of preparation method of nano aluminium oxide colloidal sol, realize by following steps:
The first step, prepare nano aluminium oxide suspension,
A1.1, take nano alumina particles and deionized water by a certain percentage;
The mass ratio of nano alumina particles and deionized water is 3:7～1:1; The size distribution of aluminum oxide inorganic nanoparticles is mainly at 5～500nm, and median size is 20～100nm, and can select low-cost boehmite nano particle is raw material, also can select other kind aluminum oxide inorganic nanoparticles.
A1.2, nano alumina particles is joined in deionized water by stirring, obtain the nano aluminium oxide mixed solution;
A1.3, add a certain amount of lactic acid and appropriate amount of addition agent in the nano aluminium oxide mixed solution, obtain nano aluminium oxide suspension after stirring;
Lactic acid is dispersion agent, addition is 0.2～5% of nano alumina particles quality, preferably addition is 2～3%, addition increases since 0.2%, the viscosity of nano aluminium oxide suspension diminishes gradually, the nano aluminium oxide colloidal sol solid content that it prepares increases gradually from 30%, while to addition, being 2～3%, the viscosity of nano aluminium oxide suspension reaches trough, the nano aluminium oxide colloidal sol solid content of preparation can reach 50%, afterwards along with the increase of addition, the viscosity of nano aluminium oxide suspension increases gradually, the nano aluminium oxide colloidal sol solid content that it prepares reduces gradually from 50%, addition is for being less than 0.2% or while being greater than 5%, the viscosity of nano aluminium oxide suspension is large, and the nano aluminium oxide colloidal sol solid content of preparation can't reach 30%.
Auxiliary agent comprises flow agent, defoamer and wetting agent, be adopted as fluorine-carbon modified polyacrylic ester one or more, its consumption is selected according to practical situation, common engineering experience addition is 0～10% of nano alumina particles quality.
Add lactic acid and auxiliary agent and regulate ph value of mixture to 2～5, high-speed stirring obtains nano aluminium oxide suspension in 2～5 hours.
Second step, the nano aluminium oxide suspension that utilizes ball mill to obtain the first step carries out grinding dispersion, obtains nano aluminium oxide colloidal sol.
Adopt high energy ball mill, by the further grinding dispersion of nano aluminium oxide suspension, reduce the nano aluminium oxide colloidal sol that the nano aluminium oxide particle diameter obtains a kind of dispersed high solids content.Wherein the ratio of grinding media to material of ball mill is generally selected 1:1～3:1, also can select suitable ratio of grinding media to material according to practical situation; Under identical preparation condition, the particle diameter of abrading-ball is less, and after its ball milling, the particle diameter of nano aluminium oxide is less, and in engineering reality, the particle diameter of abrading-ball is chosen as 0.5～5mm, also can select as required the abrading-ball of appropriate particle size; During ball milling, the general 100～450rmp that selects of rotating speed, also can slow down or speedup according to practical situation; The ball mill pulverizing time is longer, and after ball milling, the particle diameter of nano aluminium oxide is less, and higher its corresponding ball mill pulverizing time of solid content is also longer, and in engineering reality, the general selection of ball mill pulverizing time is 5～80 hours, according to practical situation, extends or shortens.
A kind of preparation method of nano oxidized alumina gel, realize by following steps:
The first step, prepare nano aluminium oxide suspension,
A1.1, take nano alumina particles and deionized water by a certain percentage;
A1.2, nano alumina particles is joined in deionized water by stirring, obtain the nano aluminium oxide mixed solution;
A1.3, add a certain amount of lactic acid and appropriate amount of addition agent in the nano aluminium oxide mixed solution, obtain nano aluminium oxide suspension after stirring;
Second step, the nano aluminium oxide suspension that utilizes ball mill to obtain the first step carries out grinding dispersion, obtains nano aluminium oxide colloidal sol;
The 3rd step, gel,
The nano aluminium oxide colloidal sol that second step is obtained, under agitation add a certain amount of vulkacit H aqueous solution, and the gel certain hour, obtain nano oxidized alumina gel at a certain temperature.
(1) under high-speed stirring (500～1000rpm), adding the vulkacit H aqueous solution that concentration is 20～50wt%, the vulkacit H consumption is the vulkacit H that every 100ml nano aluminium oxide colloidal sol adds 0.4～1.4g.
Vulkacit H is mixed with the aqueous solution of 20～50wt%, is to consider for manufacturability, and its change in concentration does not have much affect to gel, and concentration can not be too high, otherwise can cause moment to solidify, and affects gel quality affects; Gelation rate is relevant to the vulkacit H quality with intensity, and every 100m1 nano aluminium oxide colloidal sol adds the vulkacit H of 0.4～1.4g, and the vulkacit H consumption is more, and its gelation rate and intensity are better.The vulkacit H addition is relevant to the solid content of nano aluminium oxide colloidal sol, if will obtain identical gel-strength (under gel time and temperature the same terms), the solid content of nano aluminium oxide colloidal sol is less, and corresponding vulkacit H addition is more; Every 100ml nano aluminium oxide colloidal sol adds the scope that exceeds 0.4～1.4g, if the vulkacit H addition very little, lower than 0.4g, gelation rate is slow, if the vulkacit H addition is too many, higher than 1.4g, nano aluminium oxide colloidal sol moment solidifies, and gel-strength is not high.
(2) nano aluminium oxide colloidal sol is sealed and put into baking oven, heat under 80～90 ℃ and carry out gelation in 48～96 hours, obtain nano oxidized alumina gel.
Gelling temp is selected higher, and under the same conditions, its gel degree is just higher, and gel time is longer, and under the same conditions, its gel degree is just higher; Gelling temp and time can be selected according to practical situation in engineering.
The present invention's beneficial effect compared with prior art:
(1) the present invention adopts lactic acid as dispersion agent, utilizes the peculiar structure of lactic acid (containing hydroxyl and carboxyl), has effectively reduced the reunion of nano aluminium oxide, has improved the solubleness of nano aluminium oxide in water;
(2) to prepare nano aluminium oxide colloidal sol solid content high in the present invention, can reach 30%, is up to 50%, and be uniformly dispersed, have good stability, can be in water long-term stable existence;
(3) simple, the environmental protection of technique of the present invention, environmental friendliness, the nano aluminium oxide colloidal sol particle diameter obtained is little, purity is high, size distribution is even, is suitable for large-scale industrial production;
(4) the present invention, by adding the vulkacit H aqueous solution, makes to have the smooth gel of nano aluminium oxide colloidal sol of high solids content, prepares the nano oxidized alumina gel with high solids content.
Figure of description
Fig. 1 is process flow sheet of the present invention;
The SEM photo that Fig. 2 is nano aluminium oxide suspension;
The SEM photo that Fig. 3 is nano aluminium oxide colloidal sol;
Fig. 4 is before and after ball-milling processing, the particle diameter comparison diagram of nano aluminium oxide;
After Fig. 5 is different Ball-milling Times, nano aluminium oxide change of size trend map in the colloidal sol of solid content 40wt%.
Embodiment
Below in conjunction with accompanying drawing 1 and specific examples, the present invention is described in detail.
Embodiment 1
Preparation technology as shown in Figure 1,
(1) prepare nano aluminium oxide suspension
The 3.5kg aluminum oxide nanoparticle is incorporated in the 6.5kg deionized water by high-speed stirring, obtain the nano aluminium oxide mixed solution, the lactic acid dispersion agent and the appropriate amount of addition agent that add aluminum oxide nanoparticle quality 0.2% in the nano aluminium oxide mixed solution, stir and within 5 hours, make the nano aluminium oxide suspension that granule content is 35%.
(2) grinding dispersion, obtain nano aluminium oxide colloidal sol
The nano aluminium oxide suspension that is 35% by solid content, by ratio of grinding media to material, it is the agate ball that 1:1 adds 3.5kg, the particle diameter of abrading-ball is 5mm, by the further grinding dispersion of planetary ball mill, at rotating speed, is that under 250 rev/mins of conditions, ball milling makes the nano aluminium oxide colloidal sol that solid content is 35% in 24 hours.
Adopt scanning electronic microscope S-4800 (Hitachi Co., Japan) characterize the pattern of aluminum oxide nanoparticle, as shown in Figure 2,3, adopt the size-grade distribution of Malvern laser particle analyzer (Zetasizer Nano ZS) sign nano aluminium oxide suspension, as shown in table one and Fig. 4.
Add respectively lactic acid dispersion agent and the appropriate amount of addition agent of aluminum oxide nanoparticle quality 0.5%, 0.7%, 1.0%, 2.0%, 3.0%, 4.0% and 5.0 in the nano aluminium oxide mixed solution, all the other are with embodiment 1.
Record the particle diameter result of nano aluminium oxide dispersion liquid by Malvern laser particle analyzer Zetasizer Nano ZS, its test result is in Table one and Fig. 4.
Table one
| Specific embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 |
| Nanometer Al 2O 3Solid content (wt%) | 35 | 35 | 35 | 35 | 35 | 35 | 35 | 35 |
| The particle diameter of abrading-ball (mm) | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 |
| Ball-milling Time (h) | 24 | 24 | 24 | 24 | 24 | 24 | 24 | 24 |
| Lactic acid dispersant (%) | 0.2 | 0.5 | 0.7 | 1.0 | 2.0 | 3.0 | 4.0 | 5.0 |
| Nanometer Al 2O 3Particle diameter (nm) | 886 | 869 | 796 | 515 | 321 | 309 | 380 | 411 |
As can be seen from Table I, under equal conditions, increase the addition of lactic acid dispersion agent, the particle diameter of nano aluminium oxide reduces gradually, and 2.0～3.0% the time, particle diameter reaches trough, and particle diameter starts to increase subsequently.
Embodiment 9～13
The 4.0kg nano alumina particles is incorporated in the 6.0kg deionized water by high-speed stirring, adds 2.0% lactic acid dispersion agent, stir and within 5 hours, make the nano aluminium oxide suspension that granule content is 40%; The nano aluminium oxide suspension that is 40% by above-mentioned granule content, by ratio of grinding media to material, it is the agate ball that 1:1 adds 4.0kg, the particle diameter of abrading-ball is 5mm, by the further grinding dispersion of planetary ball mill, rotating speed be under 250 rev/mins of conditions respectively ball milling within 0,10,20,40,60 hours, make the nano aluminium oxide colloidal sol of content 40%.The particle diameter of nano aluminium oxide dispersion liquid is in Table two and Fig. 5.
Table two
| Specific embodiment | 9 | 10 | 11 | 12 | 13 |
| Nanometer Al 2O 3Solid content (%) | 40 | 40 | 40 | 40 | 40 |
| The particle diameter of abrading-ball (mm) | 5 | 5 | 5 | 5 | 5 |
| Ball-milling Time (h) | 0 | 10 | 20 | 40 | 60 |
| Lactic acid dispersant (%) | 2 | 2 | 2 | 2 | 2 |
| Nanometer Al 2O 3Particle diameter (nm) | 1044 | 647 | 485 | 326 | 288 |
From table two and Fig. 4, can find out, under equal conditions, Ball-milling Time is longer, and in its colloidal sol, the nano aluminium oxide particle diameter is less.
Embodiment 14
The particle diameter of abrading-ball is 2mm, and all the other record the particle diameter result of dispersion liquid, in Table three with embodiment 11.
Table three
| Specific embodiment | 11 | 14 |
| Nanometer Al 2O 3Solid content (%) | 40 | 40 |
| The particle diameter of abrading-ball (mm) | 5 | 2 |
| Ball-milling Time (h) | 20 | 20 |
| Lactic acid dispersant (%) | 2 | 2 |
| Nanometer Al 2O 3Particle diameter (nm) | 485 | 319 |
As can be seen from Table III, under equal conditions, the abrading-ball particle diameter is less, and in its colloidal sol, the nano aluminium oxide particle diameter is less.
Embodiment 15,16
By 4.5kg, the 5kg nano alumina particles is incorporated into 5.5kg by high-speed stirring respectively, in the 5kg deionized water, adds 3.0% lactic acid dispersion agent, stirs and within 10 hours, makes the nano aluminium oxide suspension that granule content is 45%, 50%; By above-mentioned content, be 45%, 50% nano aluminium oxide suspension, by ratio of grinding media to material, be that 1:1 adds 4.5kg, 5.0kg agate ball, the particle diameter of abrading-ball is 2mm, by the further grinding dispersion of planetary ball mill, at rotating speed, be that under 250 rev/mins of conditions, ball milling makes the nano aluminium oxide colloidal sol that solid content is 45%, 50% in 20 hours.Record the particle diameter result of dispersion liquid, in Table four.
Embodiment 17
Respectively the 3.0kg nano alumina particles is incorporated in the 7.0kg deionized water by high-speed stirring, adds 0.2% lactic acid dispersion agent, stir and within 10 hours, make the nano aluminium oxide suspension that granule content is 30%; The nano aluminium oxide suspension that is 30% by above-mentioned content, by ratio of grinding media to material, it is the agate ball that 1:1 adds 3.0kg, the particle diameter of abrading-ball is 2mm, by the further grinding dispersion of planetary ball mill, at rotating speed, is that under 250 rev/mins of conditions, ball milling makes the nano aluminium oxide colloidal sol that solid content is 30% in 20 hours.Record the particle diameter result of dispersion liquid, in Table four.
Table four
| Specific embodiment | 15 | 16 | 17 |
| Nanometer Al 2O 3Solid content (%) | 45 | 50 | 30 |
| The particle diameter of abrading-ball (mm) | 2 | 2 | 2 |
| Ball-milling Time (h) | 20 | 20 | 20 |
| Lactic acid dispersant (%) | 3 | 3 | 0.2 |
| Nanometer Al 2O 3Particle diameter (nm) | 1329 | 3015 | 880 |
Embodiment 18～20
The nano aluminium oxide colloidal sol that embodiment 12 is made, under 500 rev/mins of high-speed stirring, adds 0.89g vulkacit H (being made into the vulkacit H aqueous solution of 20～50wt%).Then nano aluminium oxide colloidal sol is sealed and put into baking oven, heat under 80 ℃ and carry out gelation in 24,48,96 hours, obtain nano oxidized alumina gel, the results are shown in Table five.
Table five
| Specific embodiment | 18 | 19 | 20 |
| Nanometer Al 2O 3Solid content (%) | 40 | 40 | 40 |
| Nanometer Al 2O 3Sol volume (ml) | 100 | 100 | 100 |
| Gelling temp (℃) | 80 | 80 | 80 |
| Gel time (h) | 24 | 48 | 96 |
| Vulkacit H (g) | 0.89 | 0.89 | 0.89 |
| Gel-strength (finger pressure) | Gel not | ? | Medium |
Embodiment 21～23
The nano aluminium oxide colloidal sol that embodiment 12 is made, under 500 rev/mins of high-speed stirring, adds 0.89g vulkacit H (being made into the vulkacit H aqueous solution of 20～50wt%).Then nano aluminium oxide colloidal sol is sealed and put into baking oven, heat under 90 ℃ and carry out gelation in 24,48,96 hours, obtain nano oxidized alumina gel, the results are shown in Table six.
Table six
| Specific embodiment | 21 | 22 | 23 |
| Nanometer Al 2O 3Solid content (%) | 40 | 40 | 40 |
| Nanometer Al 2O 3Sol volume (ml) | 100 | 100 | 100 |
| Gelling temp (℃) | 90 | 90 | 90 |
| Gel time (h) | 24 | 48 | 96 |
| Vulkacit H (g) | 0.89 | 0.89 | 0.89 |
| Gel-strength (finger pressure) | ? | Medium | Stronger |
From table five and table six, can find out, under equal conditions, gel time is longer, and its gel degree is higher, and under equal conditions, gelling temp is higher, and its gel degree is higher.
Embodiment 24～29
The nano aluminium oxide colloidal sol that embodiment 16,17 is made, under 500 rev/mins of high-speed stirring, adds respectively vulkacit H 0.4～1.4g (being made into the vulkacit H aqueous solution of 20～50wt%).Then nano aluminium oxide colloidal sol is sealed and put into baking oven, under 90 ℃, heating is carried out gelation in 48 hours, obtains nano oxidized alumina gel, the results are shown in Table seven.
Table seven
| Specific embodiment | 24 | 25 | 26 | 27 | 28 | 29 |
| Nanometer Al 2O 3Solid content (%) | 30 | 30 | 30 | 50 | 50 | 50 |
| Nanometer Al 2O 3Sol volume (nl) | 100 | 100 | 100 | 100 | 100 | 100 |
| Gelling temp (℃) | 90 | 90 | 90 | 90 | 90 | 90 |
| Gel time (h) | 48 | 48 | 48 | 48 | 48 | 48 |
| Vulkacit H (g) | 0.4 | 0.89 | 1.4 | 0.4 | 0.88 | 1.4 |
| Gel-strength (finger pressure) | ? | ? | Medium | Medium | Stronger | Stronger |
From table seven, to find out, under the low-solid content condition, the gel degree is lower; With the increase of vulkacit H amount, gel-strength increases.
The unspecified part of the present invention is known to the skilled person technology.
Claims (10)
1. the preparation method of a nano aluminium oxide colloidal sol is characterized in that realizing by following steps:
The first step, prepare nano aluminium oxide suspension,
A1.1, take nano alumina particles and deionized water by a certain percentage;
A1.2, nano alumina particles is joined in deionized water by stirring, obtain the nano aluminium oxide mixed solution;
A1.3, add a certain amount of lactic acid and appropriate amount of addition agent in the nano aluminium oxide mixed solution, obtain nano aluminium oxide suspension after stirring;
Second step, the nano aluminium oxide suspension that utilizes ball mill to obtain the first step carries out grinding dispersion, obtains nano aluminium oxide colloidal sol.
2. the preparation method of a kind of nano aluminium oxide colloidal sol according to claim 1, it is characterized in that: in described steps A 1.1, the mass ratio of nano alumina particles and deionized water is 3:7～1:1.
3. the preparation method of a kind of nano aluminium oxide colloidal sol according to claim 1, it is characterized in that: in described steps A 1.2, the lactic acid addition is 0.2～5% of nano alumina particles quality.
4. according to the preparation method of the described a kind of nano aluminium oxide colloidal sol of claim 1 or 3, it is characterized in that: in described steps A 1.2, the lactic acid addition is 2～3% of nano alumina particles quality.
5. the preparation method of a kind of nano aluminium oxide colloidal sol according to claim 1, it is characterized in that: in described steps A 1.2, auxiliary agent is flow agent, defoamer and wetting agent.
6. the preparation method of a nano oxidized alumina gel is characterized in that realizing by following steps:
The first step, prepare nano aluminium oxide suspension,
A1.1, take nano alumina particles and deionized water by a certain percentage;
A1.2, nano alumina particles is joined in deionized water by stirring, obtain the nano aluminium oxide mixed solution;
A1.3, add a certain amount of lactic acid and appropriate amount of addition agent in the nano aluminium oxide mixed solution, obtain nano aluminium oxide suspension after stirring;
Second step, the nano aluminium oxide suspension that utilizes ball mill to obtain the first step carries out grinding dispersion, obtains nano aluminium oxide colloidal sol;
The 3rd step, gel,
The nano aluminium oxide colloidal sol that second step is obtained, under agitation add a certain amount of vulkacit H aqueous solution, and the gel certain hour, obtain nano oxidized alumina gel at a certain temperature.
7. the preparation method of a kind of nano oxidized alumina gel according to claim 6, is characterized in that: the vulkacit H that in described the 3rd step vulkacit H aqueous solution, the vulkacit H consumption is every 100ml nano aluminium oxide colloidal sol interpolation 0.4～1.4g.
8. the preparation method of a kind of nano oxidized alumina gel according to claim 6, it is characterized in that: in described steps A 1.1, the mass ratio of nano alumina particles and deionized water is 3:7～1:1.
9. the preparation method of a kind of nano oxidized alumina gel according to claim 6, it is characterized in that: in described steps A 1.2, the lactic acid addition is 0.2～5% of nano alumina particles quality.
10. the preparation method of a kind of nano oxidized alumina gel according to claim 6, it is characterized in that: in described steps A 1.2, the lactic acid addition is 2～3% of nano alumina particles quality.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01275421A (en) * | 1989-03-08 | 1989-11-06 | Mitsubishi Kasei Corp | Production of boehmite |
| US5258168A (en) * | 1989-07-19 | 1993-11-02 | Aluminum Company Of America | Production of alunites |
| JPH0664919A (en) * | 1992-08-21 | 1994-03-08 | Asahi Glass Co Ltd | Production of alumina sol |
| CN1237146A (en) * | 1996-03-05 | 1999-12-01 | 佐藤护郎 | Alumina sol, process for preparing the same, process for preparing alumina molding using the same, and alumina-based catalyst prepared thereby |
| CN1771198A (en) * | 2003-04-02 | 2006-05-10 | 圣戈本陶瓷及塑料股份有限公司 | Nanoporous ultrafine alpha-alumina powders and sol-gel process of preparing the same |
| CN101928029A (en) * | 2010-09-08 | 2010-12-29 | 苏州创元投资发展(集团)有限公司 | Method for preparing aluminum oxide sol |
| CN102311134A (en) * | 2010-07-07 | 2012-01-11 | 中国石油化工股份有限公司 | Spherical integral macroporous alumina and preparation method thereof |
| CN102659152A (en) * | 2012-04-24 | 2012-09-12 | 上海应用技术学院 | Method for preparing nanometer alumina slurry with good water dispersibility |
| JP2012193052A (en) * | 2011-03-15 | 2012-10-11 | Nissan Chem Ind Ltd | Organic solvent dispersion alumina sol, and method for producing the same |
-
2013
- 2013-08-30 CN CN201310386089.5A patent/CN103496724B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01275421A (en) * | 1989-03-08 | 1989-11-06 | Mitsubishi Kasei Corp | Production of boehmite |
| US5258168A (en) * | 1989-07-19 | 1993-11-02 | Aluminum Company Of America | Production of alunites |
| JPH0664919A (en) * | 1992-08-21 | 1994-03-08 | Asahi Glass Co Ltd | Production of alumina sol |
| CN1237146A (en) * | 1996-03-05 | 1999-12-01 | 佐藤护郎 | Alumina sol, process for preparing the same, process for preparing alumina molding using the same, and alumina-based catalyst prepared thereby |
| CN1771198A (en) * | 2003-04-02 | 2006-05-10 | 圣戈本陶瓷及塑料股份有限公司 | Nanoporous ultrafine alpha-alumina powders and sol-gel process of preparing the same |
| CN102311134A (en) * | 2010-07-07 | 2012-01-11 | 中国石油化工股份有限公司 | Spherical integral macroporous alumina and preparation method thereof |
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