CN103496724B - The preparation method of a kind of nano alumina sol and gel - Google Patents
The preparation method of a kind of nano alumina sol and gel Download PDFInfo
- Publication number
- CN103496724B CN103496724B CN201310386089.5A CN201310386089A CN103496724B CN 103496724 B CN103496724 B CN 103496724B CN 201310386089 A CN201310386089 A CN 201310386089A CN 103496724 B CN103496724 B CN 103496724B
- Authority
- CN
- China
- Prior art keywords
- nano
- aluminium oxide
- nano alumina
- gel
- alumina sol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Colloid Chemistry (AREA)
Abstract
The present invention proposes the preparation method of a kind of nano alumina sol and gel, and by taking nano alumina particles as raw material, lactic acid is dispersion agent, is combined with high energy ball mill disperse phase by high-speed stirring, prepares high solids content nano alumina sol; By obtained nano alumina sol, under agitation add a certain amount of vulkacit H aqueous solution, heating certain hour carries out gelation, obtains nano oxidized alumina gel.The present invention is simple, nano alumina sol solid content >=30% that dispersion is obtained, and particle diameter is little, is evenly distributed, and can in water long-term stable existence.
Description
Technical field
The present invention relates to the preparation method of a kind of nano alumina sol and gel, belong to chemical technology field.
Background technology
Nano alumina sol has excellent physicochemical property, has purposes extremely widely in productive life, is used to make catalyzer and carrier, fine ceramics, fiber reinforcement alumina ceramic composite material, new coating.But because nano aluminium oxide particle diameter is little, specific surface area and surface energy are all very large, are easy to reunite, and solid content is difficult to improve.The domestic and international nano alumina sol about high solids content, gel research report are considerably less, and according to correlative study, major cause is the solubleness of aluminum oxide in water is very limited.
At present, relate to the technology of preparing in nano alumina sol about the patent of nano alumina sol more both at home and abroad more.In the preparation method of alumina sol, usually with organic alkoxide or inorganic salt master for raw material.As taken aluminum isopropylate as the organic salt raw material method of raw material, the nano alumina sol that this kind of method is prepared is expensive, makes the application of sol-gel method receive a definite limitation; Another kind method is with inorganic salt raw material method, is dissolved in by metallic aluminium in hydrochloric acid or aluminum chloride, obtains water white Alumina gel.Or by aluminum nitrate and ammonium citrate soluble in water according to a certain ratio, with concentrated nitric acid or strong aqua regulator solution pH value, can Alumina gel be obtained.These two kinds of preparation method's preparation process are large to environmental hazard, and cost is high, and final obtained nano alumina sol solid content is low, generally lower than 20wt%.Chinese patent CN201210120945.8 discloses a kind of nanometer alumina slurry being prepared stable dispersion by sol-gel method, and the solid content of alumina sol is up to 13wt%.It is raw material with boehmite that Chinese patent CN201010274945.4 discloses a kind of, and dispersion also regulator solution pH value obtains nano alumina 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 alumina sol of preparation is unsatisfactory.
Summary of the invention
The object of the invention is to overcome prior art deficiency, provide that a kind of environmental friendliness, nano aluminium oxide particle diameter are little, even particle size distribution, 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 alumina sol, is realized by following steps:
The first step, prepares 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 Alumina Inorganic nano particle is mainly at 5 ~ 500nm, and median size is 20 ~ 100nm, and low-cost boehmite nano particle can be selected to be raw material, also can select other kind Alumina Inorganic nano particles.
A1.2, nano alumina particles is joined in deionized water by stirring, obtain nano aluminium oxide mixed solution;
A1.3, in nano aluminium oxide mixed solution, add a certain amount of lactic acid and appropriate amount of addition agent, after stirring, obtain nano aluminium oxide suspension;
Lactic acid is dispersion agent, addition is 0.2 ~ 5% of nano alumina particles quality, preferred addition is 2 ~ 3%, addition increases from 0.2%, the viscosity of nano aluminium oxide suspension diminishes gradually, its nano alumina sol solid content prepared increases gradually from 30%, when being 2 ~ 3% to addition, the viscosity of nano aluminium oxide suspension reaches trough, the nano alumina sol solid content of preparation can reach 50%, afterwards along with the increase of addition, the viscosity of nano aluminium oxide suspension increases gradually, its nano alumina sol solid content prepared reduces gradually from 50%, addition for be less than 0.2% or be greater than 5% time, the viscosity of nano aluminium oxide suspension is large, and the nano alumina sol solid content of preparation cannot 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, and common engineering experience addition is 0 ~ 10% of nano alumina particles quality.
Add lactic acid and auxiliary agent adjustment ph value of mixture to 2 ~ 5, high-speed stirring obtains nano aluminium oxide suspension in 2 ~ 5 hours.
Second step, utilizes ball mill to carry out grinding dispersion to the nano aluminium oxide suspension that the first step obtains, obtains nano alumina sol.
Adopt high energy ball mill, by further for nano aluminium oxide suspension grinding dispersion, reduce the nano alumina sol that nano aluminium oxide particle diameter obtains a kind of dispersed high solids content.Wherein the ratio of grinding media to material of ball mill generally selects 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 the abrading-ball of appropriate particle size as required; During ball milling, rotating speed generally selects 100 ~ 450rmp, 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 solid content its corresponding ball mill pulverizing time higher is also longer, and in engineering reality, the ball mill pulverizing time generally selects 5 ~ 80 hours, extends or shorten according to practical situation.
A preparation method for nano oxidized alumina gel, is realized by following steps:
The first step, prepares 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 nano aluminium oxide mixed solution;
A1.3, in nano aluminium oxide mixed solution, add a certain amount of lactic acid and appropriate amount of addition agent, after stirring, obtain nano aluminium oxide suspension;
Second step, utilizes ball mill to carry out grinding dispersion to the nano aluminium oxide suspension that the first step obtains, obtains nano alumina sol;
3rd step, gel,
The nano alumina sol obtained by second step, under agitation adds a certain amount of vulkacit H aqueous solution, at a certain temperature gel certain hour, obtains nano oxidized alumina gel.
(1) under high-speed stirring (500 ~ 1000rpm), adding the vulkacit H aqueous solution that concentration is 20 ~ 50wt%, vulkacit H consumption is the vulkacit H that every 100ml nano alumina sol adds 0.4 ~ 1.4g.
Vulkacit H is mixed with the aqueous solution of 20 ~ 50wt%, is that its change in concentration does not have much affect to gel, and concentration can not be too high, otherwise can cause and solidify instantaneously, affects gel quality in order to manufacturability is considered; Gelation rate is relevant to vulkacit H quality with intensity, and every 100m1 nano alumina sol adds the vulkacit H of 0.4 ~ 1.4g, and vulkacit H consumption is more, its gelation rate and intensity better.Vulkacit H addition is relevant to the solid content of nano alumina sol, to obtain identical gel-strength (gel time and temperature the same terms under), the solid content of nano alumina sol is less, and corresponding vulkacit H addition is more; Every 100ml nano alumina sol adds the scope exceeding 0.4 ~ 1.4g, if vulkacit H addition very little, lower than 0.4g, gelation rate is slow, if vulkacit H addition is too many, higher than 1.4g, nano alumina sol is solidified instantaneously, and gel-strength is not high.
(2) nano alumina sol sealed and put into baking oven, at 80 ~ 90 DEG C, heating carries out gelation in 48 ~ 96 hours, obtains nano oxidized alumina gel.
Gelling temp is selected higher, and under the same conditions, its gellation is higher, and gel time is longer, and under the same conditions, its gellation is 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), effectively reduces the reunion of nano aluminium oxide, improve the solubleness of nano aluminium oxide in water;
(2) to prepare nano alumina sol solid content high in the present invention, can reach 30%, be up to 50%, and be uniformly dispersed, have good stability, can in water long-term stable existence;
(3) simple, the environmental protection of present invention process, environmental friendliness, the nano alumina sol particle diameter obtained is little, purity is high, even particle size distribution, is suitable for large-scale industrial production;
(4) the present invention is by adding the vulkacit H aqueous solution, makes the smooth gel of nano alumina sol with high solids content, prepares the nano oxidized alumina gel with high solids content.
Figure of description
Fig. 1 is present invention process schema;
Fig. 2 is the SEM photo of nano aluminium oxide suspension;
Fig. 3 is the SEM photo of nano alumina sol;
Fig. 4 is before and after ball-milling processing, the particle diameter comparison diagram of nano aluminium oxide;
Fig. 5 is after different Ball-milling Time, 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) nano aluminium oxide suspension is prepared
3.5kg aluminum oxide nanoparticle is incorporated in 6.5kg deionized water by high-speed stirring, obtain nano aluminium oxide mixed solution, in nano aluminium oxide mixed solution, add lactic acid dispersion agent and the appropriate amount of addition agent of aluminum oxide nanoparticle quality 0.2%, stir the nano aluminium oxide suspension that 5 hours obtained granule contents are 35%.
(2) grinding dispersion, obtains nano alumina sol
Be the nano aluminium oxide suspension of 35% by solid content, be the agate ball that 1:1 adds 3.5kg by ratio of grinding media to material, the particle diameter of abrading-ball is 5mm, and by the further grinding dispersion of planetary ball mill, under rotating speed is 250 revs/min of conditions, ball milling 24 hours obtained solid contents are the nano alumina sol of 35%.
Adopt scanning electronic microscope S-4800 (HitachiCo., Japan) pattern of aluminum oxide nanoparticle is characterized, as shown in Figure 2,3, Malvern laser particle analyzer (ZetasizerNanoZS) is adopted to characterize the size-grade distribution of nano aluminium oxide suspension, as shown in table one and Fig. 4.
Embodiment 2 ~ 8
Add 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 nano aluminium oxide mixed solution respectively, all the other are with embodiment 1.
Recorded the particle size results of nano aluminium oxide dispersion liquid by Malvern laser particle analyzer ZetasizerNanoZS, 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 (mm) of abrading-ball | 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% time, particle diameter reaches trough, and particle diameter starts to increase subsequently.
Embodiment 9 ~ 13
4.0kg nano alumina particles is incorporated in 6.0kg deionized water by high-speed stirring, adds the lactic acid dispersion agent of 2.0%, stir the nano aluminium oxide suspension that 5 hours obtained granule contents are 40%; Be the nano aluminium oxide suspension of 40% by above-mentioned granule content, be the agate ball that 1:1 adds 4.0kg by ratio of grinding media to material, the particle diameter of abrading-ball is 5mm, by the further grinding dispersion of planetary ball mill, the nano alumina sol of difference ball milling 0,10,20,40,60 hours obtained content 40% under rotating speed is 250 revs/min of conditions.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 (mm) of abrading-ball | 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 |
As can be seen from table two and Fig. 4, under equal conditions, Ball-milling Time is longer, and in its colloidal sol, nano aluminium oxide particle diameter is less.
Embodiment 14
The particle diameter of abrading-ball is 2mm, and all the other record the particle size results 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 (mm) of abrading-ball | 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, abrading-ball particle diameter is less, and in its colloidal sol, nano aluminium oxide particle diameter is less.
Embodiment 15,16
Respectively 4.5kg, 5kg nano alumina particles is incorporated into 5.5kg by high-speed stirring, in 5kg deionized water, adds the lactic acid dispersion agent of 3.0%, stir the nano aluminium oxide suspension that 10 hours obtained granule contents are 45%, 50%; Be 45% by above-mentioned content, the nano aluminium oxide suspension of 50%, be that 1:1 adds 4.5kg by ratio of grinding media to material, the agate ball of 5.0kg, the particle diameter of abrading-ball is 2mm, by the further grinding dispersion of planetary ball mill, under rotating speed is 250 revs/min of conditions, ball milling 20 hours obtained solid contents are the nano alumina sol of 45%, 50%.Record the particle size results of dispersion liquid, in table four.
Embodiment 17
Respectively 3.0kg nano alumina particles is incorporated in 7.0kg deionized water by high-speed stirring, adds the lactic acid dispersion agent of 0.2%, stir the nano aluminium oxide suspension that 10 hours obtained granule contents are 30%; Be the nano aluminium oxide suspension of 30% by above-mentioned content, be the agate ball that 1:1 adds 3.0kg by ratio of grinding media to material, the particle diameter of abrading-ball is 2mm, and by the further grinding dispersion of planetary ball mill, under rotating speed is 250 revs/min of conditions, ball milling 20 hours obtained solid contents are the nano alumina sol of 30%.Record the particle size results of dispersion liquid, in table four.
Table four
| Specific embodiment | 15 | 16 | 17 |
| Nanometer Al 2O 3Solid content (%) | 45 | 50 | 30 |
| The particle diameter (mm) of abrading-ball | 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
By nano alumina sol obtained for embodiment 12 under 500 revs/min of high-speed stirring, add 0.89g vulkacit H (being made into the vulkacit H aqueous solution of 20 ~ 50wt%).Then nano alumina sol sealed and put into baking oven, at 80 DEG C, heating 24,48, within 96 hours, carry out gelation, 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 (DEG C) | 80 | 80 | 80 |
| Gel time (h) | 24 | 48 | 96 |
| Vulkacit H (g) | 0.89 | 0.89 | 0.89 |
| Gel-strength (finger pressure) | Non-gel | More weak | Medium |
Embodiment 21 ~ 23
By nano alumina sol obtained for embodiment 12 under 500 revs/min of high-speed stirring, add 0.89g vulkacit H (being made into the vulkacit H aqueous solution of 20 ~ 50wt%).Then nano alumina sol sealed and put into baking oven, at 90 DEG C, heating 24,48, within 96 hours, carry out gelation, 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 (DEG C) | 90 | 90 | 90 |
| Gel time (h) | 24 | 48 | 96 |
| Vulkacit H (g) | 0.89 | 0.89 | 0.89 |
| Gel-strength (finger pressure) | More weak | Medium | Stronger |
As can be seen from table five and table six, under equal conditions, gel time is longer, and its gellation is higher, and under equal conditions, gelling temp is higher, and its gellation is higher.
Embodiment 24 ~ 29
By nano alumina sol obtained for embodiment 16,17 under 500 revs/min of high-speed stirring, add vulkacit H 0.4 ~ 1.4g (being made into the vulkacit H aqueous solution of 20 ~ 50wt%) respectively.Then nano alumina sol sealed and put into baking oven, at 90 DEG C, heating carries 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 (DEG C) | 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) | More weak | More weak | Medium | Medium | Stronger | Stronger |
From table seven to find out, under low-solid content condition, gellation 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 (5)
1. a preparation method for nano alumina sol, is characterized in that being realized by following steps:
The first step, prepares 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;
A1.2, nano alumina particles is joined in deionized water by stirring, obtain nano aluminium oxide mixed solution;
A1.3, in nano aluminium oxide mixed solution, add a certain amount of lactic acid and appropriate amount of addition agent, nano aluminium oxide suspension is obtained after stirring, auxiliary agent is flow agent, defoamer and wetting agent, lactic acid addition is 0.2 ~ 5% of nano alumina particles quality, additive dosage is (0 of nano alumina particles quality, 10%], described auxiliary agent comprise fluorine-carbon modified polyacrylic ester one or more;
Second step, utilizes ball mill to carry out grinding dispersion to the nano aluminium oxide suspension that the first step obtains, obtains nano alumina sol.
2. the preparation method of a kind of nano alumina sol according to claim 1, is characterized in that: in described steps A 1.3, lactic acid addition is 2 ~ 3% of nano alumina particles quality.
3. a preparation method for nano oxidized alumina gel, is characterized in that being realized by following steps:
The first step, prepares 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;
A1.2, nano alumina particles is joined in deionized water by stirring, obtain nano aluminium oxide mixed solution;
A1.3, in nano aluminium oxide mixed solution, add a certain amount of lactic acid and appropriate amount of addition agent, nano aluminium oxide suspension is obtained after stirring, auxiliary agent is flow agent, defoamer and wetting agent, lactic acid addition is 0.2 ~ 5% of nano alumina particles quality, additive dosage is (0 of nano alumina particles quality, 10%], described auxiliary agent comprise fluorine-carbon modified polyacrylic ester one or more;
Second step, utilizes ball mill to carry out grinding dispersion to the nano aluminium oxide suspension that the first step obtains, obtains nano alumina sol;
3rd step, gel,
The nano alumina sol obtained by second step, under agitation adds a certain amount of vulkacit H aqueous solution, at a certain temperature gel certain hour, obtains nano oxidized alumina gel.
4. the preparation method of a kind of nano oxidized alumina gel according to claim 3, is characterized in that: in the described 3rd step vulkacit H aqueous solution, vulkacit H consumption is the vulkacit H that every 100mL nano alumina sol adds 0.4 ~ 1.4g.
5. the preparation method of a kind of nano oxidized alumina gel according to claim 3, is characterized in that: in described steps A 1.3, lactic acid addition is 2 ~ 3% of nano alumina particles quality.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310386089.5A CN103496724B (en) | 2013-08-30 | 2013-08-30 | The preparation method of a kind of nano alumina sol and gel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310386089.5A CN103496724B (en) | 2013-08-30 | 2013-08-30 | The preparation method of a kind of nano alumina sol and gel |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103496724A CN103496724A (en) | 2014-01-08 |
| CN103496724B true CN103496724B (en) | 2016-03-30 |
Family
ID=49862017
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310386089.5A Active CN103496724B (en) | 2013-08-30 | 2013-08-30 | The preparation method of a kind of nano alumina sol and gel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103496724B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3024071B1 (en) * | 2014-09-12 | 2018-04-25 | LG Chem, Ltd. | Method for preparing cathode material for lithium secondary battery, cathode material for lithium secondary battery, and lithium secondary battery containing same |
| CN105177991A (en) * | 2015-09-05 | 2015-12-23 | 苏州宏久航空防热材料科技有限公司 | Preparation method of silicon carbide fibers based on alumina sol |
| CN107117635A (en) * | 2017-06-28 | 2017-09-01 | 苏州纳迪微电子有限公司 | A kind of preparation method of ball-aluminium oxide powder |
| CN109504277A (en) * | 2018-10-26 | 2019-03-22 | 广州嘉睿复合材料有限公司 | A kind of nano hybridization ceramic resin and preparation method thereof |
| CN111218731B (en) * | 2019-12-26 | 2023-02-03 | 山东鲁阳浩特高技术纤维有限公司 | Sol for preparing alumina fiber and preparation method thereof |
| CN112754957B (en) * | 2021-01-29 | 2022-06-14 | 浙江芬尼奇工贸有限公司 | Hand washing-free gel |
| CN114716175B (en) * | 2022-04-28 | 2023-03-14 | 佳化化学科技发展（上海）有限公司 | Accelerating agent and preparation method and application thereof |
| CN114853453B (en) * | 2022-05-27 | 2023-03-17 | 航天特种材料及工艺技术研究所 | Hydrophobic ceramic aerogel material with micro-nano structure and preparation method thereof |
| CN115490527A (en) * | 2022-10-24 | 2022-12-20 | 宜兴兴贝耐火材料制品有限公司 | High-temperature-resistant anti-cracking silicon carbide wear-resistant plastic material and preparation method thereof |
| CN115676864A (en) * | 2022-10-25 | 2023-02-03 | 航天特种材料及工艺技术研究所 | Rapid preparation method and application of aluminum sol |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5258168A (en) * | 1989-07-19 | 1993-11-02 | Aluminum Company Of America | Production of alunites |
| 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 |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01275421A (en) * | 1989-03-08 | 1989-11-06 | Mitsubishi Kasei Corp | Production of boehmite |
| JPH0664919A (en) * | 1992-08-21 | 1994-03-08 | Asahi Glass Co Ltd | Production of alumina sol |
| 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 (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5258168A (en) * | 1989-07-19 | 1993-11-02 | Aluminum Company Of America | Production of alunites |
| 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 |
| 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 |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103496724A (en) | 2014-01-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103496724B (en) | The preparation method of a kind of nano alumina sol and gel | |
| CN103223488B (en) | Preparation method for silver-coated silicon dioxide composite microsphere particles | |
| CN102407341B (en) | surface modified particle diameter mixed silver powder and preparation method thereof | |
| CN107971502B (en) | Preparation method of high-dispersity spherical silver powder | |
| CN102923770B (en) | Preparation method of yttrium-stabilized nanometer zirconium dioxide powder | |
| CN103861657B (en) | Preparation method of nano-silver loaded porous silicon dioxide | |
| CN104070177A (en) | Simple and novel preparation method for silver and gold nano-particles | |
| CN109371308B (en) | The method for preparing multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end | |
| CN102861618B (en) | Preparation method of alumina supporter | |
| CN106216710A (en) | A kind of preparation method of high-tap density high-crystallinity silver powder | |
| CN102600772B (en) | Preparation method of embedded nano-metallic aerogel | |
| CN108658130B (en) | Method for simultaneously preparing iron oxide and silicon dioxide aerogel from iron tailings | |
| CN102676164B (en) | Spherical calcium molybdate-base red phosphor and preparation method thereof | |
| CN107931629A (en) | A kind of preparation method of the positive galactic pole ball shape silver powder of photovoltaic | |
| CN106430266B (en) | Sol-gal process prepares the preparation method of nano aluminium oxide crystal seed | |
| CN103666118B (en) | The preparation method of ferric oxide aqueous color paste | |
| CN101386419B (en) | Composite nano cerium dioxide sol preparation method | |
| CN104328296A (en) | Preparation method of Al2O3/Mo composite material | |
| CN109534383A (en) | Synthesis method of cerium dioxide nanosheet | |
| CN107777718B (en) | A kind of Y2O3Nano-powder and preparation method thereof | |
| CN110066952A (en) | A kind of preparation method of zirconium oxide enhancing molybdenum alloy bar material | |
| CN109465464A (en) | A method of preparing alumina-based ceramic metal nano composite powder | |
| CN104495939A (en) | Hydrothermal synthesis method of nano-scale zirconium tungstate hollow spheres | |
| CN106365192A (en) | Preparation method of ultra-small scale rare-earth oxide nano-powder | |
| CN103043651B (en) | Alcohol-water carbon black and cerium oxide biphase nano composite slurry for preparing metal base micro-nano powder and preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |