CN106517219A - Aerogel ball and preparation method thereof - Google Patents
Aerogel ball and preparation method thereof Download PDFInfo
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- CN106517219A CN106517219A CN201610160339.7A CN201610160339A CN106517219A CN 106517219 A CN106517219 A CN 106517219A CN 201610160339 A CN201610160339 A CN 201610160339A CN 106517219 A CN106517219 A CN 106517219A
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- aerogel
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- microscope carrier
- aeroge
- small ball
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/16—Preparation of silica xerogels
-
- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The present invention discloses an aerogel ball and a preparation method thereof. The preparation method comprises: uniformly mixing an aerogel powder material, an aqueous binder and an additive capable or incapable of selectively being added to prepare an aerogel slurry; uniformly dropping the aerogel slurry on a carrying table formed by mainly and uniformly paving the aerogel powder material so as to form small aerogel balls; and drying the small aerogel balls to obtain the aerogel ball. According to the present invention, the aerogel preparation process is simple, the complex operation is not required, the condition is mild, the method can be performed with the common equipment, the cost is low, the large scale production is easily achieved, and the obtained aerogel bass has advantages of nano-scale continuous pore structure, low density, high specific surface area, uniform mesopore distribution, wide application prospect, and the like.
Description
Technical field
The present invention relates to a kind of aerogel material, more particularly to a kind of airsetting glueballs and preparation method thereof, belong to nano-porous materials
Technical field.
Background technology
Aeroge is a kind of porous solid material being made up of nano-particle or high-polymer molecular, with density it is low, porosity is high,
The features such as pore size distribution is uniform.Its distinctive nano-scale hole structure causes it in the aspect table such as calorifics, acoustics, electricity, optics
Reveal the property of uniqueness, have broad application prospects in numerous areas.
In recent years, the preparation of microspheric functional material is one of hot issue of material circle, and it has been opened up perhaps for the application of functional material
More new field, but it is little to prepare the research report of airsetting glueballs so far, thus the preparation research of aeroge ball material have it is important
Meaning.
For example, CN1546225A discloses a kind of TiO2The preparation method of/aerosil ball, its balling technique is：Into
Ammoniacal liquor, surfactant and kerosene are housed in ball gel-forming container, solvent is added dropwise in gel-forming device.But the preparation work
Used in skill, ammonia vol is big, and colloidal sol is not easy balling-up, and oil phase is not easily recycled recycling.
Again for example, CN104163431A discloses a kind of method for preparing grade aerosil ball, its balling technique
For：Ammoniacal liquor and silica alcosol are entered static mixer by peristaltic pump to mix, then flow into from bottom fill soybean oil with
In the gel-forming device of ethanol, the other silica dioxide gel ball of grade is formed.But the supercritical drying process for adopting will to equipment
Ask high, condition is controlled and operating difficulties.
Again for example, CN104891510A discloses one kind and prepares grade SiO using constant pressure and dry2The method of airsetting glueballs, its
Balling technique is：The Ludox that pH value is 2～3 is stood after 12～24h of hydrolysis at room temperature, it is 4～6 to adjust pH value,
Then it is added drop-wise to the SiO of big 90 degree of hydrophobic angle2On aerogel powder, 1～2h of gelation is stood in air, is formed spherical wet
Gel；In absolute ethyl alcohol soak after, be repeatedly aged, burin-in process post-modification, drying, obtain grade SiO2Airsetting
Glueballs.But the complex operation, time are long, and obtained airsetting glueballs size is difficult to control to, and intensity is not high.
The content of the invention
Present invention is primarily targeted at a kind of airsetting glueballs preparation method of improvement and airsetting glueballs are provided, so as to overcome existing skill
Deficiency in art.
For realizing aforementioned invention purpose, the technical solution used in the present invention includes：
A kind of preparation method of airsetting glueballs is provided in certain embodiments, and which includes：
By aerogel powder material, aqueous binders and alternative addition or without additive be uniformly mixed and made into airsetting
Rubber cement material；
The aeroge slurry is uniformly dropped in mainly by the evenly laid out microscope carrier for being formed of aerogel powder material, airsetting is formed
Glue bead；
The gas gel small ball is dried, the airsetting glueballs is obtained.
Among some embodiments, described preparation method can include：The aeroge slurry is made because of self gravitation effect,
Uniformly it is dropped on the microscope carrier and forms gas gel small ball.
Among some embodiments, described preparation method can include：The initial velocity for making the aeroge slurry to set from
Eject in container and be uniformly dropped on the microscope carrier and form gas gel small ball.
Among some preferred embodiments, described preparation method can include：Make the aeroge slurry setting thrust and
Uniformly it is dropped under the collective effect of self gravitation on the microscope carrier and forms gas gel small ball.
Among some embodiments, the spacing between the two neighboring described gas gel small ball formed on the microscope carrier is more than
2mm.Cause the adhesion of adjacent gas gel small ball to prevent spacing too small.
Among some embodiments, preferably the aeroge slurry is placed in the container that can be rotated around own axes, and makes institute
State aeroge slurry to drop on the microscope carrier during the container is rotated in the speed with 1r/s～10r/s and form airsetting
Glue bead, the axis vertical of wherein described container are arranged.
In some embodiments, to contain the aeroge slurry and can allow its drippage container be it is conventional with drip hole,
The equipment such as all kinds of containers of spray orifice, or syringe, shower nozzle.Wherein, by adjusting drip hole, aperture of spray orifice etc.,
Size of aeroge slurry gob (or slurry group) of drippage etc. is can adjust, and then the gas gel small ball size for making to be formed is controllable.
Among some embodiments, 0.1～2mm is preferably by the thickness of the evenly laid out microscope carrier for being formed of aerogel powder material.
More preferred, the aeroge coating includes 10～50wt% aerogel powder materials.
Further, the density of the aerogel powder material is 0.05g/ml～0.3g/ml, and particle diameter is 0.1 μm～2mm, than
Surface is 500m2/ g～1200m2/ g, thermal conductivity are 0.01W/m.k～0.04W/m.k.
Wherein, the hydrophilicity and hydrophobicity of the aerogel powder material can need according to application and adjust.
Further, the aerogel powder material is at least preferably from aerosil, titania aerogel, graphite
Any one in alkene aeroge, but not limited to this.
More preferred, the aeroge coating includes 10～50wt% aqueous binders.
Further, the aqueous binders are at least selected from aqueous pure-acrylic emulsion, aqueous acrylate and vinyl acetate emulsion, waterborne styrene-acrylic emulsion, water
Any one in property acrylic acid ester emulsion, aqueous polyurethane emulsion, aqueous epoxy resin emulsion, waterborne organic silicon emulsion, but
Not limited to this.
Further, the aeroge coating is comprising optionally addition or without additive.
Further, the additive at least selected from defoamer, dispersant, levelling agent, thickener, wetting agent, coalescents,
Any one in pigment, but not limited to this.
Among some preferred embodiments, described preparation method includes：In normal pressure and temperature be 30～70 DEG C under conditions of will
The gas gel small ball is dried, and obtains the airsetting glueballs.
In certain embodiments there is provided the airsetting glueballs prepared by aforesaid any one method.
A kind of airsetting glueballs is provided in certain embodiments, and its a diameter of 0.1～10mm, specific surface area are 500～1200m2/ g,
Density is 0.10～0.20g/cm3, and include the continuous pore space structure with nano-scale, in the network loose structure for wherein being formed
The aperture of hole is 2～30nm,.
Compared with prior art, advantages of the present invention includes：
(1) the airsetting glueballs preparation process is simple for providing, without the need for complex operations, mild condition can be by common conventional equipment
Implement, it is with low cost, beneficial to large-scale production；
(2) the airsetting glueballs preparation technology for providing can be obtained the continuous pore space structure with nano-scale, and density is low, specific surface
High, the mesoporous airsetting glueballs being evenly distributed of product, such as the diameter of prepared airsetting glueballs can be adjusted to 0.1 as needed～
10mm, specific surface area are 500～1200m2/ g, the continuous pore space structure with nano-scale, the network loose structure for being formed
Aperture size is 2～30nm or so, and density is 0.10～0.20g/cm3Internal structure is typical mesoporous nano material, can be with
The hydrophilic and hydrophobic of airsetting glueballs is adjusted according to applied environment, density is low, specific surface area is high, it is mesoporous be evenly distributed, and gained
Airsetting glueballs is the grade orbicule of profile rule and size tunable, and rolling characteristics is high, heat-insulated, catalysis, chromatogram filling with
And the field such as absorption is easy to application, can significantly expand the range of application and efficiency of aeroge, compensate for existing airsetting glueballs and prepare skill
Deficiency in art, it is significant.
Description of the drawings
Fig. 1 is the photo of 1 obtained airsetting glueballs of the embodiment of the present invention；
Fig. 2 is the adsorption effect figure of 1 obtained airsetting glueballs of the embodiment of the present invention；
Fig. 3 is the grain size distribution of aerosil powder in the embodiment of the present invention 1；
Fig. 4 is the transmission electron microscope picture of aerosil powder in the embodiment of the present invention 1.
Specific embodiment
Embody feature of present invention to describe in detail in the following description with the exemplary embodiments of advantage.It should be understood that energy of the present invention
Enough to have various changes in different embodiments, which neither departs from the scope of the present invention, and explanation therein and is shown in this
Purposes of discussion is treated as in matter, and is not used to limit the present invention.
The present invention is described in detail with some embodiments below in conjunction with the accompanying drawings.
Embodiment 1
1) by silicon dioxide aerogel powder (its particle diameter distribution and pattern see Fig. 3-Fig. 4) and aqueous polyurethane is in mass ratio
1:3 mixing, and the hydroxyethyl cellulose of about 0.1wt% is added, it is prepared into water paste；
2) water paste is added in a container that can make slurry extruding drippage, described container bore about 2mm or so；
3) silicon-dioxide powdery is laid on flat board and forms microscope carrier, aerogel powder thickness about 1mm on flat board；
4) water paste in the container is dropped on the microscope carrier, that is, obtains gas gel small ball, the container rotation turns
Speed is 5r/s (axis vertical is arranged, and Open Side Down), and the particle size range of airsetting glueballs is 2mm or so.
5) by step 4) the airsetting glueballs for preparing is placed on 30～70 DEG C of dryings of normal pressure in baking oven, that is, obtain dry airsetting glueballs,
Its specific surface area is 700m2/ g, the continuous pore space structure with nano-scale, the network loose structure aperture size for being formed is
15nm or so, density are 0.15g/cm3Internal structure is typical mesoporous nano material, and the gas gel small ball can be used to adsorb
Organic solvent.
Embodiment 2
1) by silicon dioxide aerogel powder and aqueous polyurethane in mass ratio 1:4, add the hydroxypropyl cellulose of 0.5wt%, system
For into water paste；
2) by the water paste of above-mentioned preparation, it is added in a container that can make slurry extruding drippage, the container bore scope
For 3mm or so；
3) silicon-dioxide powdery is laid on a microscope carrier, on flat board, aerogel powder thickness is 1.5mm；
4) by the slurry in container be dropped in 3) described in be paved with the microscope carrier of silicon-dioxide powdery, that is, obtain gas gel small ball,
The rotation rotating speed 7r/s (axis vertical is arranged, and Open Side Down) of the container, the particle size range of airsetting glueballs is 3mm or so；
5) by step 4) the airsetting glueballs for preparing is placed on 30～70 DEG C of dryings of normal pressure in baking oven, that is, obtain dry airsetting glueballs,
Its particle size range is 3mm or so, and specific surface area is 800m2/ g, the continuous pore space structure with nano-scale, the net for being formed
Network loose structure aperture size is 20nm or so, and density is 0.17g/cm3, internal structure is typical mesoporous nano material.
Embodiment 3
1) by silicon-dioxide powdery and water-base epoxy resin in mass ratio 1:4, the hydroxypropyl cellulose of 0.5wt% is added, is prepared
Into water paste；
2) by the water paste of above-mentioned preparation, it is added in a container that can make slurry extruding drippage, described container bore is
5mm；
3) silicon-dioxide powdery is laid on a microscope carrier, on flat board, aerogel powder thickness is 1.8mm；
4) by the slurry in container be dropped in 3) described in be paved with the microscope carrier of silicon-dioxide powdery, that is, obtain gas gel small ball,
The rotation rotating speed of the container is 4r/s (axis vertical settings), bead particle diameter can by the slurry outlet of regulation container controlling,
The particle size range of airsetting glueballs is 5mm or so；
5) the airsetting glueballs of preparation is placed on into 30～70 DEG C of dryings of normal pressure in baking oven, that is, obtains dry gas gel small ball, its particle diameter
Scope is 5mm, and specific surface area is 100m2/ g, the continuous pore space structure with nano-scale, the network loose structure for being formed
Aperture size is 10nm or so, and density is 0.18g/cm3Internal structure is typical mesoporous nano material.
Reference examples：
1) with industrial-grade sodium silicate as silicon source, it is 1 by volume by industrial-grade sodium silicate and deionized water：4 are well mixed,
It is 2～3 that solution Jing strong-acid type styrene type cation exchange resin ion exchanges after being well mixed prepare pH value
Ludox, then stands hydrolysis 12h at room temperature.
2) ammonia spirit of 1mol/L is slowly added dropwise in the Ludox after hydrolysis, is adjusted its pH value to 6, is obtained prefabricated
Ludox.
3) hydrophobic angle is about 126 ° of SiO2Aerogel powder it is evenly laid out on flat board as microscope carrier.
4) prefabricated Ludox is dropwise added drop-wise on microscope carrier using syringe, forms stable spherical droplets, stood in air
Gelation 1h is so that the surface strength of spherical droplet overcomes the surface tension of ethanol solution, the spherical wet gel of formation enough.
5) spherical wet gel is obtained into gas gel small ball in 50 DEG C of dryings of normal pressure.But the unadjustable control of its particle diameter distribution, airsetting
Glue bead intensity difference, whole complex technical process, time-consuming, and cannot adjust the hydrophilicity and hydrophobicity of gas gel small ball.
It should be understood that embodiment described in the invention is merely for exemplary purpose, and it is not used to limit the protection of the present invention
Scope, those skilled in the art can be made within the scope of the invention various other replacements, changes and improvements, thus, the present invention
Above-mentioned embodiment is not limited to, and is only defined by the claims.
Claims (9)
1. a kind of preparation method of airsetting glueballs, it is characterised in that include：
By aerogel powder material, aqueous binders and alternative addition or without additive be uniformly mixed and made into airsetting
Rubber cement material；
The aeroge slurry is uniformly dropped in mainly by the evenly laid out microscope carrier for being formed of aerogel powder material, airsetting is formed
Glue bead；
The gas gel small ball is dried, the airsetting glueballs is obtained.
2. preparation method according to claim 1, it is characterised in that include：
The aeroge slurry is made uniformly to be dropped on the microscope carrier because of self gravitation effect, and form gas gel small ball；
Or, the initial velocity for making the aeroge slurry to set is ejected from container and is uniformly dropped on the microscope carrier and shape
Into gas gel small ball；
Or, make the aeroge slurry setting thrust and self gravitation collective effect under be uniformly dropped on the microscope carrier and
Form gas gel small ball.
3. preparation method according to claim 1 and 2, it is characterised in that include：
Spacing between the two neighboring described gas gel small ball formed on the microscope carrier is more than 2mm；
And/or, the aeroge slurry is placed in the container that can be rotated around own axes, and makes the aeroge slurry exist
The container is dropped to during the speed with 1r/s～10r/s rotates on the microscope carrier and forms gas gel small ball, wherein described
The axis vertical of container is arranged；And/or, it is 0.1～2mm by the thickness of the evenly laid out microscope carrier for being formed of aerogel powder material.
4. preparation method according to claim 1, it is characterised in that：
The aeroge coating includes 10～50wt% aerogel powder materials；
And/or, the density of the aerogel powder material is 0.05g/ml～0.3g/ml, and particle diameter is 0.1 μm～2mm, specific surface
For 500m2/ g～1200m2/ g, thermal conductivity are 0.01W/m.k～0.04W/m.k；
And/or, the aerogel powder material is at least selected from aerosil, titania aerogel, graphene aerogel
In any one.
5. preparation method according to claim 1, it is characterised in that：
The aeroge coating includes 10～50wt% aqueous binders；
And/or, the aqueous binders at least selected from aqueous pure-acrylic emulsion, aqueous acrylate and vinyl acetate emulsion, waterborne styrene-acrylic emulsion, aqueous third
Any one in olefin(e) acid ester emulsion, aqueous polyurethane emulsion, aqueous epoxy resin emulsion, waterborne organic silicon emulsion.
6. preparation method according to claim 1, it is characterised in that：
The aeroge coating is comprising optionally addition or without additive；
And/or, the additive is at least selected from defoamer, dispersant, levelling agent, thickener, wetting agent, coalescents, face
Any one in material.
7. preparation method according to claim 1, it is characterised in that include：In normal pressure and temperature is 30～70 DEG C of condition
It is lower that the gas gel small ball is dried, obtain the airsetting glueballs.
8. the airsetting glueballs that prepared by the method by any one of claim 1-7.
9. a kind of airsetting glueballs, its a diameter of 0.1～10mm, specific surface area are 500～1200m2/ g, and include have receive
The continuous pore space structure of meter ruler cun, the aperture of the network loose structure Hole for wherein being formed is 2～30nm, and sphericity is 0.7～1,
Density is 0.10～0.20g/cm3。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2015209883310 | 2015-12-02 | ||
| CN201520988331 | 2015-12-02 |
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| CN106517219A true CN106517219A (en) | 2017-03-22 |
| CN106517219B CN106517219B (en) | 2019-02-12 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107128934A (en) * | 2017-06-28 | 2017-09-05 | 武汉理工大学 | Light hollow aeroge ball forming method and its mould used |
| CN108585798A (en) * | 2018-05-09 | 2018-09-28 | 安徽中航名坤新材料科技有限公司 | A kind of nano-porous alumina aeroge ceramic bead 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 |
| CN117229678A (en) * | 2023-11-15 | 2023-12-15 | 四川赛尔科美新材料科技有限公司 | Inorganic silicon sound insulation and heat preservation gel and manufacturing method thereof |
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| JP2007244993A (en) * | 2006-03-15 | 2007-09-27 | National Institute Of Advanced Industrial & Technology | Ceramic carrier, ceramic catalytic body and methods for manufacturing them |
| CN104497729A (en) * | 2014-12-15 | 2015-04-08 | 苏州同玄新材料有限公司 | Aerogel anti-dewing paint, and preparation method and application thereof |
| CN104891510A (en) * | 2015-05-28 | 2015-09-09 | 长安大学 | Method for preparing millimeter SiO2 aerogel ball by drying under normal pressure |
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| JP2007244993A (en) * | 2006-03-15 | 2007-09-27 | National Institute Of Advanced Industrial & Technology | Ceramic carrier, ceramic catalytic body and methods for manufacturing them |
| CN104497729A (en) * | 2014-12-15 | 2015-04-08 | 苏州同玄新材料有限公司 | Aerogel anti-dewing paint, and preparation method and application thereof |
| CN104891510A (en) * | 2015-05-28 | 2015-09-09 | 长安大学 | Method for preparing millimeter SiO2 aerogel ball by drying under normal pressure |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107128934A (en) * | 2017-06-28 | 2017-09-05 | 武汉理工大学 | Light hollow aeroge ball forming method and its mould used |
| CN107128934B (en) * | 2017-06-28 | 2019-04-30 | 武汉理工大学 | Light hollow aeroge ball forming method and its mold used |
| CN108585798A (en) * | 2018-05-09 | 2018-09-28 | 安徽中航名坤新材料科技有限公司 | A kind of nano-porous alumina aeroge ceramic bead and preparation method thereof |
| CN108585798B (en) * | 2018-05-09 | 2022-02-18 | 安徽弘徽科技有限公司 | Nano porous alumina aerogel ceramic pellet 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 |
| 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 |
| CN117229678A (en) * | 2023-11-15 | 2023-12-15 | 四川赛尔科美新材料科技有限公司 | Inorganic silicon sound insulation and heat preservation gel and manufacturing method thereof |
| CN117229678B (en) * | 2023-11-15 | 2024-01-26 | 四川赛尔科美新材料科技有限公司 | Inorganic silicon sound insulation and heat preservation gel and manufacturing method thereof |
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