CN108585798A - A kind of nano-porous alumina aeroge ceramic bead and preparation method thereof - Google Patents
A kind of nano-porous alumina aeroge ceramic bead and preparation method thereof Download PDFInfo
- Publication number
- CN108585798A CN108585798A CN201810438091.5A CN201810438091A CN108585798A CN 108585798 A CN108585798 A CN 108585798A CN 201810438091 A CN201810438091 A CN 201810438091A CN 108585798 A CN108585798 A CN 108585798A
- Authority
- CN
- China
- Prior art keywords
- nano
- polyvinyl alcohol
- bead
- preparation
- ceramic bead
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
- C04B35/111—Fine ceramics
- C04B35/1115—Minute sintered entities, e.g. sintered abrasive grains or shaped particles such as platelets
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63416—Polyvinylalcohols [PVA]; Polyvinylacetates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0045—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by a process involving the formation of a sol or a gel, e.g. sol-gel or precipitation processes
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
Abstract
The invention discloses a kind of nano-porous alumina aeroge ceramic beads and preparation method thereof, are related to nano-hole aerogel ceramic technology field.The present invention includes the following steps：SS01 configures the Aluminum sol containing polyvinyl alcohol；SS02 prepares oil ammonia column solution；SS03 balling-up；SS04 agings, supercritical drying；SS05 is heat-treated.The present invention improves balling-up to improve surface tension effects by using addition polyvinyl alcohol with this, ensure the nano-pore structure of bead in combination with the gentle gel drying technology of sol-gel technique, it is obtained with some strength finally by thermal sintering, while remaining the alumina aerogels ceramic bead of nano-porous structure and high-specific surface area；The simple process and low cost is honest and clean, and sphericity is high, is conducive to large-scale production.
Description
Technical field
The invention belongs to nano-hole aerogel ceramic technology fields, more particularly to a kind of nano-porous alumina aeroge
Ceramic bead and preparation method thereof.
Background technology
Aeroge is a kind of solid-state material for the porous structure being mutually polymerized to by nano-particle, has porosity height, density
Many excellent properties such as low, large specific surface area, thermal conductivity are low, the velocity of sound is low, index of refraction is low.These excellent performances make aeroge
It is widely used in multiple fields, such as high efficiency heat insulation material, acoustic material, catalyst and catalyst carrier, boat
Empty space material and rechargeable battery carrier etc..It can be sent out when being used at relatively high temperatures using most silica aerogels at present
Raw burn knot cannot keep the architectural characteristic of its nanoporous, and temperature is used for a long time and is generally not more than 650 DEG C, while aeroge
Structural strength is relatively low, is difficult in some environments.In order to adapt to some special dimensions（Such as aerospace, high-temperature catalytic）
More operation at high temperature and in the case of having certain requirement to intensity seeks a kind of resistance to higher temperature, has nano-porous structure,
Simultaneously there is the nanoporous aerogel ceramic material of some strength to have become important one of developing direction.
In numerous material systems, aluminium oxide has higher temperature in use（Fusing point is up to 2054 DEG C, boiling point 2980
℃）, it is the ideal chose for preparing high temperature resistant aeroge ceramic material.If simultaneously by nanoporous aerogel ceramics macrostructure system
At spherical shape, its application range and efficiency in the fields such as heat-insulated, catalysis and chromatography filling will be expanded significantly.And aeroge is made pottery
Porcelain bead is easy to use and is easily recycled, it is easier to which the production cycle is shortened in exchange of solvent and rapid draing, is conducive to industrial metaplasia
Production.Finding no Patents documents prepares alumina aerogels ceramic bead at present, is more that silica aerogel is small
Ball and aluminium oxide ceramics bead, therefore nano-porous alumina aeroge ceramic bead has broad application prospects.
Invention content
Have the various aspects such as sphericity height, specific surface area height, intensity height excellent the purpose of the present invention is to provide a kind of
Woelm Alumina aeroge ceramic bead, at the same provide it is a kind of simple for process, manufacturing cost it is cheap quickly prepare aluminium oxide
The method of aeroge ceramic bead.To achieve the goals above, the invention discloses a kind of dexterous and quick techniques to obtain
The preparation method of alumina aerogels ceramic bead.
In order to solve the above technical problems, the present invention is achieved by the following technical solutions：
The present invention is a kind of nano-porous alumina aeroge ceramic bead, and the small ball's diameter is 0.2-2mm, aperture 5-
15nm, specific surface area are 200-500 m2/g；The bead is white or translucent color.
Further, the preparation method of a kind of nano-porous alumina aeroge ceramic bead, including following step
Suddenly：
SS01 configures the Aluminum sol containing polyvinyl alcohol：
According to molar ratio by silicon source：Solvent：Chelating agent：Acid：Water=1：3-12：0.1-0.4：0.3-0.5：20-40 is added sequentially to
The water bath condition for being 65-85 DEG C in container and in temperature stirs 30-60min；Form the Aluminum sol of clear；Then it adds
Mass fraction is 0.2%-2%（Mass fraction of the polyvinyl alcohol than silicon source）Polyvinyl alcohol continue stir 30-60min；It waits gathering
Vinyl alcohol is fully immersed into vitreosol；It is cooled to room temperature；I.e. configuration obtains the Aluminum sol containing polyvinyl alcohol；
SSO2 prepares oil ammonia column solution：
Configuration concentration is the ammonia spirit of 5-15%（Water is solvent）In container；And be added a certain amount of paraffin oil or n-hexane in
In container；Make the control of paraffin oil height in 2-5cm；Due to the difference of density and compatibility；Paraffin oil or just is just formd in this way
Hexane is on upper layer；Oil ammonia column solution of the ammonia spirit in lower layer；
SS03 balling-up：
The syringe for being 0.4-2.2mm with bore is by the Aluminum sol containing polyvinyl alcohol prepared according to 60-100 drops/min
Rate is added drop-wise in oil ammonia column solution；Alumina gel bead can be prepared；
SS04 agings, supercritical drying：
Subsequent aging in ethanol and displacement 12-24h；An ethyl alcohol was replaced every 6 hours；It can most be made through supercritical drying afterwards
Obtain alumina aerogels bead；
SS05 is heat-treated：
The alumina aerogels bead prepared is first kept the temperature into 1-2h at 300-400 DEG C；Then heat to 1000-1200 DEG C
At a temperature of be heat-treated 2-4h；It can be obtained alumina aerogels ceramic bead.
Further, source of aluminium is any one of aluminium isopropoxide, aluminum nitrate, aluminium chloride and boehmite powder；It is preferred that different
Aluminium propoxide.
Further, the alcoholic solvent is any one of ethyl alcohol or methanol；Preferred alcohol.
Further, the chelating agent is any one of ethyl acetoacetate or acetylacetone,2,4-pentanedione；It is preferred that acetoacetate second
Ester.
Further, the acid is any one of hydrochloric acid, nitric acid, acetic acid or oxalic acid；It is preferred that nitric acid.
Further, the alcoholysis degree of the polyvinyl alcohol is in 86-90%；The polyvinyl alcohol molecule amount is in 100000-
170000。
Further, the supercritical fluid drying is using ethyl alcohol as dried medium；The pre- nitrogen for rushing 2-3 MPa；Again with
1-2 DEG C/min speed is heated to 260-270 DEG C；Heat preservation 1-3 hours；It is released stress again to normal with 200-300 kPa/min speed
Pressure；The process that bleeds off pressure keeps temperature constant；Nitrogen 20-30min is swept in most backlash；It is taken out after being cooled to room temperature.
The invention has the advantages that：
The present invention utilizes the crosslinking styling of polyvinyl alcohol by allocating the Aluminum sol containing polyvinyl alcohol so that more at spherical shape
It is good, while later stage removal is convenient, it can the quick large-scale continuous aluminium oxide gas for preparing high sphericity, high-ratio surface and high intensity
Gel ceramic bead, to meet the needs of various aspects.
Certainly, it implements any of the products of the present invention and does not necessarily require achieving all the advantages described above at the same time.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, will be described below to embodiment required
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is the alumina aerogels ceramic bead graph of pore diameter distribution after being heat-treated in embodiment 1.
Specific implementation mode
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
All other embodiment that technical staff is obtained without creative efforts belongs to the model that the present invention protects
It encloses.
Embodiment one
As shown in Figure 1, SS01 configures the Aluminum sol containing polyvinyl alcohol：
According to molar ratio by aluminium isopropoxide：Ethyl alcohol：Ethyl acetoacetate：Nitric acid：Water=1：8：0.2：0.2：30 are added sequentially to
The water bath condition for being 80 DEG C in container and in temperature stirs 30min, forms the Aluminum sol of clear.Then quality point is added
Number continues to stir 30min for 0.5% polyvinyl alcohol, waits for that polyvinyl alcohol is fully immersed into vitreosol, is cooled to room temperature, that is, matches
It sets to obtain the Aluminum sol containing polyvinyl alcohol；
SSO2 prepares oil ammonia column solution：
A certain amount of paraffin oil is added in container in container in the ammonia spirit that configuration concentration is 10%, makes paraffin oil height
Control, due to the difference of density and compatibility, just forms paraffin oil in upper layer, oil of the ammonia spirit in lower layer in this way in 5cm
Ammonia column solution；
SS03 balling-up：
The Aluminum sol containing polyvinyl alcohol prepared is dripped according to the rate of 60 drops/min with the syringe that bore is 1.0 mm
It is added in oil ammonia column solution, you can alumina gel bead is prepared；
SS04 agings, supercritical drying：
Then aging and displacement for 24 hours, were replaced an ethyl alcohol every 6 hours, most be can be prepared by afterwards through supercritical drying in ethanol
Alumina aerogels bead, wherein supercritical fluid drying are the pre- nitrogen for rushing 2 MPa using ethyl alcohol as dried medium, then with 1
DEG C/min speed is heated to 260 DEG C, 1 hour is kept the temperature, then release stress to normal pressure with 200 kPa/min speed, this bleeds off pressure process
Keep temperature constant, nitrogen 30min is swept in most backlash, is taken out after being cooled to room temperature；
SS05 is heat-treated：
The alumina aerogels bead prepared is first kept the temperature into 1h at 400 DEG C, at a temperature of then heating to 1100 DEG C at heat
Manage 2h, you can obtain alumina aerogels ceramic bead.
Its aeroge ceramic bead diameter apertures 5-15nm, specific surface area 200-500 m2/g。
Embodiment two
SS01 configures the Aluminum sol containing polyvinyl alcohol：
According to molar ratio by aluminum nitrate：Ethyl alcohol：Ethyl acetoacetate：Nitric acid：Water=1：8：0.2：0.1：30 are added sequentially to hold
The water bath condition for being 80 DEG C in device and in temperature stirs 30min, forms the Aluminum sol of clear.Then mass fraction is added
Continue to stir 30min for 1% polyvinyl alcohol, waits for that polyvinyl alcohol is fully immersed into vitreosol, be cooled to room temperature, that is, be arranged to
To the Aluminum sol containing polyvinyl alcohol；
SSO2 prepares oil ammonia column solution：
A certain amount of paraffin oil is added in container in container in the ammonia spirit that configuration concentration is 10%, makes paraffin oil height
Control, due to the difference of density and compatibility, just forms paraffin oil in upper layer, oil of the ammonia spirit in lower layer in this way in 5cm
Ammonia column solution；
SS03 balling-up：
The Aluminum sol containing polyvinyl alcohol prepared is dripped according to the rate of 60 drops/min with the syringe that bore is 1.0 mm
It is added in oil ammonia column solution, you can alumina gel bead is prepared；
SS04 agings, supercritical drying：
Then aging and displacement for 24 hours, were replaced an ethyl alcohol every 6 hours, most be can be prepared by afterwards through supercritical drying in ethanol
Alumina aerogels bead, wherein supercritical fluid drying are the pre- nitrogen for rushing 2 MPa using ethyl alcohol as dried medium, then with 1
DEG C/min speed is heated to 260 DEG C, 1 hour is kept the temperature, then release stress to normal pressure with 200 kPa/min speed, this bleeds off pressure process
Keep temperature constant, nitrogen 30min is swept in most backlash, is taken out after being cooled to room temperature；
SS05 is heat-treated：
The alumina aerogels bead prepared is first kept the temperature into 1h at 400 DEG C, at a temperature of then heating to 1100 DEG C at heat
Manage 2h, you can obtain alumina aerogels ceramic bead.
Embodiment three
SS01 configures the Aluminum sol containing polyvinyl alcohol：
According to molar ratio by aluminium chloride：Ethyl alcohol：Ethyl acetoacetate：Nitric acid：Water=1：8：0.2：0.1：30 are added sequentially to hold
The water bath condition for being 80 DEG C in device and in temperature stirs 30min, forms the Aluminum sol of clear.Then mass fraction is added
Continue to stir 60min for 1% polyvinyl alcohol, waits for that polyvinyl alcohol is fully immersed into vitreosol, be cooled to room temperature, that is, be arranged to
To the Aluminum sol containing polyvinyl alcohol；
SSO2 prepares oil ammonia column solution：
A certain amount of paraffin oil is added in container in container in the ammonia spirit that configuration concentration is 10%, makes n-hexane height
Control, due to the difference of density and compatibility, just forms paraffin oil in upper layer, oil of the ammonia spirit in lower layer in this way in 5cm
Ammonia column solution；
SS03 balling-up：
The Aluminum sol containing polyvinyl alcohol prepared is dripped according to the rate of 60 drops/min with the syringe that bore is 1.0 mm
It is added in oil ammonia column solution, you can alumina gel bead is prepared；
SS04 agings, supercritical drying：
Then aging and displacement for 24 hours, were replaced an ethyl alcohol every 6 hours, most be can be prepared by afterwards through supercritical drying in ethanol
Alumina aerogels bead, wherein supercritical fluid drying are the pre- nitrogen for rushing 2 MPa using ethyl alcohol as dried medium, then with 1
DEG C/min speed is heated to 260 DEG C, 1 hour is kept the temperature, then release stress to normal pressure with 200 kPa/min speed, this bleeds off pressure process
Keep temperature constant, nitrogen 30min is swept in most backlash, is taken out after being cooled to room temperature；
SS05 is heat-treated：
The alumina aerogels bead prepared is first kept the temperature into 1h at 400 DEG C, at a temperature of then heating to 1100 DEG C at heat
Manage 2h, you can obtain alumina aerogels ceramic bead.
Example IV
SS01 configures the Aluminum sol containing polyvinyl alcohol：
According to molar ratio by aluminium isopropoxide：Ethyl alcohol：Ethyl acetoacetate：Nitric acid：Water=1：8：0.2：0.1：30 are added sequentially to
The water bath condition for being 80 DEG C in container and in temperature stirs 30min, forms the Aluminum sol of clear.Then quality point is added
Number continues to stir 60min for 1% polyvinyl alcohol, waits for that polyvinyl alcohol is fully immersed into vitreosol, is cooled to room temperature, that is, configures
Obtain the Aluminum sol containing polyvinyl alcohol；
SSO2 prepares oil ammonia column solution：
A certain amount of n-hexane is added in container in container in the ammonia spirit that configuration concentration is 10%, makes n-hexane height
Control, due to the difference of density and compatibility, just forms n-hexane in upper layer, oil of the ammonia spirit in lower layer in this way in 5cm
Ammonia column solution；
SS03 balling-up：
The Aluminum sol containing polyvinyl alcohol prepared is dripped according to the rate of 60 drops/min with the syringe that bore is 1.0 mm
It is added in oil ammonia column solution, you can alumina gel bead is prepared；
SS04 agings, supercritical drying：
Then aging and displacement for 24 hours, were replaced an ethyl alcohol every 6 hours, most be can be prepared by afterwards through supercritical drying in ethanol
Alumina aerogels bead, wherein supercritical fluid drying are the pre- nitrogen for rushing 2 MPa using ethyl alcohol as dried medium, then with 1
DEG C/min speed is heated to 260 DEG C, 1 hour is kept the temperature, then release stress to normal pressure with 200 kPa/min speed, this bleeds off pressure process
Keep temperature constant, nitrogen 30min is swept in most backlash, is taken out after being cooled to room temperature；
SS05 is heat-treated：
The alumina aerogels bead prepared is first kept the temperature into 1h at 400 DEG C, at a temperature of then heating to 1100 DEG C at heat
Manage 2h, you can obtain alumina aerogels ceramic bead.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the present invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described, are not limited the invention to the specific embodiments described.Obviously, according to the content of this specification,
It can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to preferably explain the present invention
Principle and practical application, to enable skilled artisan to be best understood by and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (8)
1. a kind of nano-porous alumina aeroge ceramic bead, it is characterised in that：The small ball's diameter is 0.2-2mm, aperture
For 5-15nm, specific surface area is 200-500 m2/g；The bead is white or translucent color.
2. a kind of preparation method of nano-porous alumina aeroge ceramic bead according to claim 1, feature exist
In including the following steps：
SS01 configures the Aluminum sol containing polyvinyl alcohol：
According to molar ratio by silicon source：Solvent：Chelating agent：Acid：Water=1：3-12：0.1-0.4：0.3-0.5：20-40 is added sequentially to
The water bath condition for being 65-85 DEG C in container and in temperature stirs 30-60min；Form the Aluminum sol of clear；Then it adds
Mass fraction is 0.2%-2%（Mass fraction of the polyvinyl alcohol than silicon source）Polyvinyl alcohol continue stir 30-60min；It waits gathering
Vinyl alcohol is fully immersed into vitreosol；It is cooled to room temperature；I.e. configuration obtains the Aluminum sol containing polyvinyl alcohol；
SSO2 prepares oil ammonia column solution：
Configuration concentration is the ammonia spirit of 5-15%（Water is solvent）In container；And be added a certain amount of paraffin oil or n-hexane in
In container；Make the control of paraffin oil height in 2-5cm；Due to the difference of density and compatibility；Paraffin oil or just is just formd in this way
Hexane is on upper layer；Oil ammonia column solution of the ammonia spirit in lower layer；
SS03 balling-up：
The syringe for being 0.4-2.2mm with bore is by the Aluminum sol containing polyvinyl alcohol prepared according to 60-100 drops/min
Rate is added drop-wise in oil ammonia column solution；Alumina gel bead can be prepared；
SS04 agings, supercritical drying：
Subsequent aging in ethanol and displacement 12-24h；An ethyl alcohol was replaced every 6 hours；It can most be made through supercritical drying afterwards
Obtain alumina aerogels bead；
SS05 is heat-treated：
The alumina aerogels bead prepared is first kept the temperature into 1-2h at 300-400 DEG C；Then heat to 1000-1200 DEG C
At a temperature of be heat-treated 2-4h；It can be obtained alumina aerogels ceramic bead.
3. a kind of nano-porous alumina aeroge ceramic bead according to claim 2 and preparation method thereof, feature
It is, source of aluminium is any one of aluminium isopropoxide, aluminum nitrate, aluminium chloride and boehmite powder；It is preferred that aluminium isopropoxide.
4. a kind of nano-porous alumina aeroge ceramic bead according to claim 2 and preparation method thereof, feature
It is, the alcoholic solvent is any one of ethyl alcohol or methanol；Preferred alcohol.
5. a kind of nano-porous alumina aeroge ceramic bead according to claim 2 and preparation method thereof, feature
It is, the chelating agent is any one of ethyl acetoacetate or acetylacetone,2,4-pentanedione；It is preferred that ethyl acetoacetate.
6. a kind of nano-porous alumina aeroge ceramic bead according to claim 2 and preparation method thereof, feature
It is, the acid is any one of hydrochloric acid, nitric acid, acetic acid or oxalic acid；It is preferred that nitric acid.
7. a kind of nano-porous alumina aeroge ceramic bead according to claim 2 and preparation method thereof, feature
It is, the alcoholysis degree of the polyvinyl alcohol is in 86-90%；The polyvinyl alcohol molecule amount is in 100000-170000.
8. a kind of nano-porous alumina aeroge ceramic bead according to claim 2 and preparation method thereof, feature
It is, the supercritical fluid drying is using ethyl alcohol as dried medium；The pre- nitrogen for rushing 2-3 MPa；Again with 1-2 DEG C/min speed
Degree is heated to 260-270 DEG C；Heat preservation 1-3 hours；It is released stress again to normal pressure with 200-300 kPa/min speed；It is described to bleed off pressure
Process keeps temperature constant；Nitrogen 20-30min is swept in most backlash；It is taken out after being cooled to room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810438091.5A CN108585798B (en) | 2018-05-09 | 2018-05-09 | Nano porous alumina aerogel ceramic pellet and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810438091.5A CN108585798B (en) | 2018-05-09 | 2018-05-09 | Nano porous alumina aerogel ceramic pellet and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108585798A true CN108585798A (en) | 2018-09-28 |
| CN108585798B CN108585798B (en) | 2022-02-18 |
Family
ID=63636560
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810438091.5A Active CN108585798B (en) | 2018-05-09 | 2018-05-09 | Nano porous alumina aerogel ceramic pellet and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108585798B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109775739A (en) * | 2019-04-04 | 2019-05-21 | 江南大学 | A kind of classifying porous nano alumina material of gas defence and preparation method thereof |
| CN110482997A (en) * | 2019-08-26 | 2019-11-22 | 安徽科昂纳米科技有限公司 | A kind of preparation method of thermal insulation separation hot-bulb and thermal insulation separation hot-bulb obtained |
| CN110606736A (en) * | 2019-08-23 | 2019-12-24 | 广东工业大学 | Solvent-free synthesized ceramic microsphere and preparation method and application thereof |
| CN111517346A (en) * | 2020-03-16 | 2020-08-11 | 河北铭万精细化工有限公司 | Preparation method of high-purity nano aluminum oxide |
| CN113773063A (en) * | 2020-06-09 | 2021-12-10 | 萍乡学院 | Preparation method of porous ceramic |
| CN113773064A (en) * | 2020-06-09 | 2021-12-10 | 萍乡学院 | Porous ceramic with hierarchical pore structure |
| CN115872424A (en) * | 2022-12-30 | 2023-03-31 | 黄河三角洲京博化工研究院有限公司 | High-strength spherical alumina and preparation method thereof |
Citations (27)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1192096A (en) * | 1968-02-15 | 1970-05-20 | Atomic Energy Authority Uk | Improvements in or relating to ceramics |
| JPS4990694A (en) * | 1972-12-20 | 1974-08-29 | ||
| JPH07256100A (en) * | 1994-03-24 | 1995-10-09 | Agency Of Ind Science & Technol | Production of heat-resistant alumina carrier for catalytic combustion |
| CN1171094A (en) * | 1994-11-23 | 1998-01-21 | 赫彻斯特股份公司 | Composite material containing aerogel, process for manufacturing said material and use thereof |
| CN1202707A (en) * | 1997-06-14 | 1998-12-23 | 中国科学院山西煤炭化学研究所 | Method for preparing super fine barium ferrite powder |
| DE19545346C2 (en) * | 1995-12-05 | 1999-10-14 | Univ Bayreuth Lehrstuhl Fuer K | Process for the production of ceramic nanocomposites |
| CN1293168A (en) * | 1999-10-18 | 2001-05-02 | 史啸鸣 | Process for preparing spherial porous alumina carrier |
| US6620458B2 (en) * | 2001-09-27 | 2003-09-16 | The Regents Of The University Of California | Method to produce alumina aerogels having porosities greater than 80 percent |
| CN101186512A (en) * | 2007-10-30 | 2008-05-28 | 哈尔滨工业大学 | Method for preparing heat insulation composite material by microwave |
| CN101306359A (en) * | 2008-07-01 | 2008-11-19 | 中国人民解放军第二炮兵工程学院 | Composite aerogel photocatalyst for recovering titanium dioxide/silicon dioxide |
| CN101429050A (en) * | 2008-12-04 | 2009-05-13 | 北京航空航天大学 | Method for producing porous ceramic with oriented structure by employing freeze dehydration |
| CN101525248A (en) * | 2009-04-22 | 2009-09-09 | 哈尔滨工业大学 | Ceramic aerogel and method for preparing the ceramic aerogel by gel injection moulding |
| CN102145994A (en) * | 2010-02-09 | 2011-08-10 | 航天材料及工艺研究所 | Block alumina aerogel with high temperature resistance and high specific surface area and preparation method thereof |
| CN102557710A (en) * | 2011-09-15 | 2012-07-11 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of corundum-mullite multiphase ceramic material with nano-pore structure |
| CN102584162A (en) * | 2012-02-20 | 2012-07-18 | 广东埃力生高新科技有限公司 | Unitary or polybasic aerogel thermal insulation material and preparation method thereof |
| CN102807357A (en) * | 2012-07-13 | 2012-12-05 | 中国科学院研究生院 | Block aerogel composite material and preparation method thereof |
| CN104096551A (en) * | 2013-04-08 | 2014-10-15 | 北京航空航天大学 | Aluminum-titanium oxide aerogel bead with high specific surface area and acid amount and preparation method thereof |
| CN105038496A (en) * | 2015-07-08 | 2015-11-11 | 当涂县科辉商贸有限公司 | Nanometer Al2O3 composite aerosil thermal-insulation heat-preserving paint and preparation method thereof |
| CN105688760A (en) * | 2016-01-18 | 2016-06-22 | 浙江大学 | Oxide composite aerogel of micro-nano porous structure with both micro-porosity and nano-porosity and preparing method of oxide composite aerogel |
| CN105801156A (en) * | 2016-02-19 | 2016-07-27 | 厦门纳美特新材料科技有限公司 | Porous alumina-silicon oxide aerogel balls and quick preparation method thereof |
| CN106000245A (en) * | 2015-08-26 | 2016-10-12 | 余煜玺 | Preparation method of bulk alumina aerogel |
| CN106007803A (en) * | 2016-05-16 | 2016-10-12 | 中国科学院兰州化学物理研究所 | High-temperature-resistant porous ceramic/alumina aerogel thermal insulation material |
| CN106517219A (en) * | 2015-12-02 | 2017-03-22 | 苏州同玄新材料有限公司 | Aerogel ball and preparation method thereof |
| CN106673703A (en) * | 2016-11-29 | 2017-05-17 | 清华大学 | Preparation method of light-weight and high-strength zirconium oxide-reinforced porous aluminum oxide ceramic |
| CN106865586A (en) * | 2017-02-24 | 2017-06-20 | 西北农林科技大学 | A kind of method for preparing alumina type aeroge |
| CN107098352A (en) * | 2016-02-20 | 2017-08-29 | 金承黎 | A kind of preparation method of high temperature resistant aeroge and aerogel type porous ceramics |
| CN107973592A (en) * | 2016-10-24 | 2018-05-01 | 天津工业大学 | A kind of γ-Al of even aperture distribution2O3Ceramic micro filter film and preparation method thereof |
-
2018
- 2018-05-09 CN CN201810438091.5A patent/CN108585798B/en active Active
Patent Citations (27)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1192096A (en) * | 1968-02-15 | 1970-05-20 | Atomic Energy Authority Uk | Improvements in or relating to ceramics |
| JPS4990694A (en) * | 1972-12-20 | 1974-08-29 | ||
| JPH07256100A (en) * | 1994-03-24 | 1995-10-09 | Agency Of Ind Science & Technol | Production of heat-resistant alumina carrier for catalytic combustion |
| CN1171094A (en) * | 1994-11-23 | 1998-01-21 | 赫彻斯特股份公司 | Composite material containing aerogel, process for manufacturing said material and use thereof |
| DE19545346C2 (en) * | 1995-12-05 | 1999-10-14 | Univ Bayreuth Lehrstuhl Fuer K | Process for the production of ceramic nanocomposites |
| CN1202707A (en) * | 1997-06-14 | 1998-12-23 | 中国科学院山西煤炭化学研究所 | Method for preparing super fine barium ferrite powder |
| CN1293168A (en) * | 1999-10-18 | 2001-05-02 | 史啸鸣 | Process for preparing spherial porous alumina carrier |
| US6620458B2 (en) * | 2001-09-27 | 2003-09-16 | The Regents Of The University Of California | Method to produce alumina aerogels having porosities greater than 80 percent |
| CN101186512A (en) * | 2007-10-30 | 2008-05-28 | 哈尔滨工业大学 | Method for preparing heat insulation composite material by microwave |
| CN101306359A (en) * | 2008-07-01 | 2008-11-19 | 中国人民解放军第二炮兵工程学院 | Composite aerogel photocatalyst for recovering titanium dioxide/silicon dioxide |
| CN101429050A (en) * | 2008-12-04 | 2009-05-13 | 北京航空航天大学 | Method for producing porous ceramic with oriented structure by employing freeze dehydration |
| CN101525248A (en) * | 2009-04-22 | 2009-09-09 | 哈尔滨工业大学 | Ceramic aerogel and method for preparing the ceramic aerogel by gel injection moulding |
| CN102145994A (en) * | 2010-02-09 | 2011-08-10 | 航天材料及工艺研究所 | Block alumina aerogel with high temperature resistance and high specific surface area and preparation method thereof |
| CN102557710A (en) * | 2011-09-15 | 2012-07-11 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of corundum-mullite multiphase ceramic material with nano-pore structure |
| CN102584162A (en) * | 2012-02-20 | 2012-07-18 | 广东埃力生高新科技有限公司 | Unitary or polybasic aerogel thermal insulation material and preparation method thereof |
| CN102807357A (en) * | 2012-07-13 | 2012-12-05 | 中国科学院研究生院 | Block aerogel composite material and preparation method thereof |
| CN104096551A (en) * | 2013-04-08 | 2014-10-15 | 北京航空航天大学 | Aluminum-titanium oxide aerogel bead with high specific surface area and acid amount and preparation method thereof |
| CN105038496A (en) * | 2015-07-08 | 2015-11-11 | 当涂县科辉商贸有限公司 | Nanometer Al2O3 composite aerosil thermal-insulation heat-preserving paint and preparation method thereof |
| CN106000245A (en) * | 2015-08-26 | 2016-10-12 | 余煜玺 | Preparation method of bulk alumina aerogel |
| CN106517219A (en) * | 2015-12-02 | 2017-03-22 | 苏州同玄新材料有限公司 | Aerogel ball and preparation method thereof |
| CN105688760A (en) * | 2016-01-18 | 2016-06-22 | 浙江大学 | Oxide composite aerogel of micro-nano porous structure with both micro-porosity and nano-porosity and preparing method of oxide composite aerogel |
| CN105801156A (en) * | 2016-02-19 | 2016-07-27 | 厦门纳美特新材料科技有限公司 | Porous alumina-silicon oxide aerogel balls and quick preparation method thereof |
| CN107098352A (en) * | 2016-02-20 | 2017-08-29 | 金承黎 | A kind of preparation method of high temperature resistant aeroge and aerogel type porous ceramics |
| CN106007803A (en) * | 2016-05-16 | 2016-10-12 | 中国科学院兰州化学物理研究所 | High-temperature-resistant porous ceramic/alumina aerogel thermal insulation material |
| CN107973592A (en) * | 2016-10-24 | 2018-05-01 | 天津工业大学 | A kind of γ-Al of even aperture distribution2O3Ceramic micro filter film and preparation method thereof |
| CN106673703A (en) * | 2016-11-29 | 2017-05-17 | 清华大学 | Preparation method of light-weight and high-strength zirconium oxide-reinforced porous aluminum oxide ceramic |
| CN106865586A (en) * | 2017-02-24 | 2017-06-20 | 西北农林科技大学 | A kind of method for preparing alumina type aeroge |
Non-Patent Citations (2)
| Title |
|---|
| A. YAMUNA等: "Processing and Property Evaluatiuon of Alumina Aerogel Based Ceramic Nanocomposites", 《THE SCIENCE OF ENGINEERING CERAMICS III》 * |
| 潘永康等: "《现代干燥技术》", 31 December 2006, 化学工业出版社 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109775739A (en) * | 2019-04-04 | 2019-05-21 | 江南大学 | A kind of classifying porous nano alumina material of gas defence and preparation method thereof |
| CN109775739B (en) * | 2019-04-04 | 2020-06-23 | 江南大学 | Anti-poison graded porous nano aluminum oxide material and preparation method thereof |
| CN110606736A (en) * | 2019-08-23 | 2019-12-24 | 广东工业大学 | Solvent-free synthesized ceramic microsphere and preparation method and application thereof |
| CN110482997A (en) * | 2019-08-26 | 2019-11-22 | 安徽科昂纳米科技有限公司 | A kind of preparation method of thermal insulation separation hot-bulb and thermal insulation separation hot-bulb obtained |
| CN110482997B (en) * | 2019-08-26 | 2021-10-22 | 安徽科昂纳米科技有限公司 | Preparation method of heat preservation and insulation ball and prepared heat preservation and insulation ball |
| CN111517346A (en) * | 2020-03-16 | 2020-08-11 | 河北铭万精细化工有限公司 | Preparation method of high-purity nano aluminum oxide |
| CN113773063A (en) * | 2020-06-09 | 2021-12-10 | 萍乡学院 | Preparation method of porous ceramic |
| CN113773064A (en) * | 2020-06-09 | 2021-12-10 | 萍乡学院 | Porous ceramic with hierarchical pore structure |
| CN115872424A (en) * | 2022-12-30 | 2023-03-31 | 黄河三角洲京博化工研究院有限公司 | High-strength spherical alumina and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108585798B (en) | 2022-02-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108585798A (en) | A kind of nano-porous alumina aeroge ceramic bead and preparation method thereof | |
| CN106629750B (en) | A kind of atmospheric preparation method of transparent silicon dioxide block aeroge | |
| CN103086692B (en) | Preparation method of blocky SiO2-Y2O3 compound aerogel | |
| CN102701700B (en) | SiO2 aerogel/inorganic cotton compound thermal insulation felt and preparation method thereof | |
| Suh et al. | Sol− gel strategies for pore size control of high-surface-area transition-metal oxide aerogels | |
| CN105801156B (en) | A kind of porous aluminas-silica aerogel bead and its fast preparation method | |
| CN101698592B (en) | Silicon-aluminium aerogel composite material and manufacturing method thereof | |
| JP4855582B2 (en) | Mesoporous silica, mesoporous silica composite and production method thereof | |
| CN107973592B (en) | Gamma-Al with evenly distributed aperture2O3Ceramic microfiltration membrane and preparation method thereof | |
| CN103769016A (en) | Atmospheric-pressure preparation method for hydrophobic SiO2-TiO2 composite aerogel | |
| JPH07187846A (en) | Reticular ceramic article | |
| CN104402397A (en) | Preparation method of high-temperature-resistant block-shaped SiO2-Al2O3 composite aerogel thermal insulation material | |
| CN103551091A (en) | Method for drying aerogel | |
| CN105780126B (en) | A kind of preparation method of the porous mullite formed by generated in-situ whisker overlap joint | |
| CN106007803A (en) | High-temperature-resistant porous ceramic/alumina aerogel thermal insulation material | |
| CN110510617B (en) | Normal-pressure drying preparation method of large-size alumina-silica aerogel | |
| CN104163444A (en) | Alpha-alumina hollow ball preparation method | |
| CN108249901A (en) | A kind of preparation method of high temperature resistant aeroge material | |
| CN109437816A (en) | A kind of preparation method of aluminium silica aerogel composite plate | |
| CN111362664B (en) | Preparation method of aluminum-titanium doped silicon dioxide aerogel/fiber composite material | |
| CN103130271B (en) | Ultra-low density block-shaped fully stabilized zirconia gel and preparing method thereof | |
| CN103496738B (en) | Preparation method of titanium oxide aerogel with high specific surface area and high controllability | |
| CN107973615B (en) | Mesoporous gamma-Al2O3Ceramic membrane and preparation method thereof | |
| CN1189459A (en) | Nanometre titanium dioxide/silicon dioxide mesic hole compound and prepn. thereof | |
| CN104073918A (en) | Method for synthesizing polycrystalline mullite fibers under low temperature condition |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20220207 Address after: 238000 advanced manufacturing industrial park north of Zhenxing road and west of Huashan Road, Chaohu Economic Development Zone, Hefei, Anhui Province Applicant after: Anhui Honghui Technology Co.,Ltd. Address before: 230000 room 406, North 4th floor, management committee of Chaohu Economic Development Zone, Hefei, Anhui Applicant before: ANHUI ZHONGHANG MINGKUN NEW MATERIAL TECHNOLOGY Co.,Ltd. Applicant before: Zhu Mengwei |
|
| TA01 | Transfer of patent application right |