CN107758674A - Aerogel particle and preparation method thereof - Google Patents

Aerogel particle and preparation method thereof Download PDF

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CN107758674A
CN107758674A CN201610689630.3A CN201610689630A CN107758674A CN 107758674 A CN107758674 A CN 107758674A CN 201610689630 A CN201610689630 A CN 201610689630A CN 107758674 A CN107758674 A CN 107758674A
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aerogel particle
mixed solution
foregoing
aerogel
particle
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CN107758674B (en
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陈建宏
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/16Preparation of silica xerogels
    • C01B33/163Preparation of silica xerogels by hydrolysis of organosilicon compounds, e.g. ethyl orthosilicate
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/14Pore volume

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  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
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Abstract

The invention discloses a kind of aerogel particle and preparation method thereof, aerogel particle is via made by the following steps:Blend step:One silicone compounds are mixed into an organic solvent, to form a mixed solution;Hydrolysing step:One sour catalyst is added into the mixed solution, so that reaction is hydrolyzed;Condensation step:One alkali catalyst is added into the mixed solution, to carry out condensation reaction, and a hydrophobic dispersion solvent is added in the condensation reaction, and is stirred, make the mixed solution in whipping process gelation to produce more more homogeneous aerogel particles of structure.

Description

Aerogel particle and preparation method thereof
Technical field
The present invention relates to a kind of aerogel particle and preparation method thereof.
Background technology
Aeroge is a kind of mushy material with space network, has low-down thermal conductivity, main at present Applied to heat-insulating heat-preserving material.
The preparation method of aeroge is collosol and gel synthetic method, and main elder generation is by alcoxyl SiClx class (alkoxysilane) or just After the predecessors such as methyl silicate are mixed with organic solvent, and sour catalyst is added, so that reaction (hydrolysis) is hydrolyzed. After hydrolysis certain time, then alkali catalyst is added, to carry out condensation reaction (condensation), and condensation reaction In can gradually form colloidal sol.Molecule in colloidal sol continues condensation reaction bond, gradually forms the high-molecular gel of semisolid, Again through curing (age) after a while, colloidal sol is set to form Stability Analysis of Structures space network.Finally recycle supercritical drying The water of aeroge system and methanol equal solvent are extracted drying by technology, and obtain porous dry Monolithic aerogel.
The dry technology used due to the preparation method of above-mentioned aeroge can avoid airsetting for Supercritical Drying Technology Glue is ruptured in constant pressure and dry process by the effect of surface tension of moisture.But because Supercritical Drying Technology must be entered under high pressure OK, therefore atomic a small amount of aeroge drying is suitable only for, and is not easy volume production and reduces the production cost of aeroge.
On the other hand, above-mentioned aeroge would generally will above dry Monolithic aerogel in use and crush, but general grinding mode Easily cause that aerogel structure is uneven and outward appearance is broken (herein please refer to Fig. 9 to Figure 12), and be difficult to obtain it is excellent every Thermal property.
Another " porous material and its preparation side for having case such as TaiWan, China disclosure of the invention numbering the 200835648th before correlation Method ", mainly mixing alcoxyl SiClx class or silicate compound are synthesized with organic solvent with sol-gal process, and modified dose Modify and be made, so that the hydrophilic functional group on porous structure material surface is replaced into hydrophobic functional group whereby, aeroge is kept away Exempt from the effect of surface tension of moisture and rupture, therefore can be dried at room temperature, at a normal.
The hydrophobicity modification of case aeroge is to utilize the more echelon solvent replacement techniques of normal temperature and pressure, but such a hydrophobicity before this Modification program need to be performed for more than solvent displacement in 24 hours under normal temperature and pressure conditionses, and processing procedure required time too long, is not inconsistent cost effect Benefit.
Furthermore the aeroge of case is being crushed using above still needing to will first to dry Monolithic aerogel before this, therefore aeroge is same There is the problem of structure is uneven and outward appearance is broken.
The content of the invention
Structure is more homogeneous it is an object of the invention to provide one kind production, effect of heat insulation more preferably aerogel particle and its Preparation method.
To achieve the above object, the present invention uses following technical proposal.
A kind of aerogel particle preparation method, is comprised the steps of:
Blend step:One silicone compounds are mixed into an organic solvent, to form a mixed solution;
Hydrolysing step:One sour catalyst is added into the mixed solution, so that reaction is hydrolyzed;
Condensation step:One alkali catalyst is added into the mixed solution, to carry out condensation reaction, and added in the condensation reaction One hydrophobic dispersion solvent, and being stirred, make the mixed solution in whipping process gelation and produce more aeroges Grain, wherein, in the condensation reaction, the mixed solution is stirred with 1200rpm to 2000rpm speed.
Further, the hydrophobic dispersion solvent is one or more solvents being selected from by following formed group:Ketone, Ethers, esters, the fragrant same clan, alkanes.
Further, post-processing step is also included after the condensation step:Foregoing aerogel particle is filtered out with a filter, connect And foregoing aerogel particle is cleaned with the mixed liquor of ethanol, water, before being dried in vacuo under 100 DEG C to 115 DEG C of temperature conditionss State aerogel particle.
Further, a hydrophobicity reforming step is also included after the condensation step:The mixed solution is heated up, and make foregoing Organic solvent vaporizes, and adds a chlorine and be acylated organic molecule, the chlorine is acylated a hydroxyl of organic molecule and foregoing aerogel particle Base reacts to each other, and foregoing aerogel particle is produced hydrophobicity, and avoids foregoing aeroge by the hydrophobic dispersion solvent Particle Breakage.
Further, the chlorine is acylated organic molecule and is formed group by following by one or more be selected from:Chlorination siloxanes, Chlorine acyl-alkane complexes species, chlorine acyl benzene class.
Further, the organic solvent includes ethanol, the water mutually mixed;In the hydrophobicity reforming step, make the mixing molten The temperature of liquid sequentially changes into one first temperature conditionss, a second temperature condition and one the 3rd temperature conditionss, first temperature strip Part is 78 DEG C to 82 DEG C, and the second temperature condition is 100 DEG C to 115 DEG C, and the 3rd temperature conditionss are 40 DEG C to 45 DEG C, this The chlorine is added during three temperature conditionss and is acylated organic molecule.
Further, a post-processing step is also included after the hydrophobicity reforming step:Foregoing airsetting is filtered out with a filter Glue particle, foregoing aerogel particle is then cleaned with toluene solvant, then be dried in vacuo foregoing aerogel particle.
A kind of aerogel particle, it is via made by the following steps:
Blend step:One silicone compounds are mixed into an organic solvent, to form a mixed solution;
Hydrolysing step:One sour catalyst is added into the mixed solution, so that reaction is hydrolyzed;
Condensation step:One alkali catalyst is added into the mixed solution, to carry out condensation reaction, and added in the condensation reaction One hydrophobic dispersion solvent, and being stirred, make the mixed solution in whipping process gelation and produce more aeroges Grain, the particle diameter of foregoing aerogel particle is 600nm ± 300nm, wherein, in the condensation reaction, with 1200rpm extremely 2000rpm speed stirs the mixed solution.
Preferably, the hydrophobic dispersion solvent is one or more solvents being selected from by following formed group:Ketone, Ethers, esters, the fragrant same clan, alkanes.
Aerogel particle of the present invention and preparation method thereof is by aforesaid operations, so as to have following effect.
1. the preparation method of the present invention, stirred during condensation step by a large amount of non-compatibility solvents, you can production The more homogeneous spherical particles shape aerogel particle of structure, to obtain effect of heat insulation more preferably aerogel particle, improves product Practicality.
2. the aerogel particle of preparation method of the present invention, wherein void content and hole size can (solvent contains according to preparation condition Amount, solvent viscosity, sour catalyst and alkali catalyst content) regulated and controled.
3. preparation method of the present invention can control the preparation time of aerogel particle by allotment alkali catalyst content.
4. preparation method of the present invention can be by the content and mixing speed of control non-compatibility solvent, you can effectively control The size of micron aerogel particle, when non-compatibility solvent content is higher and mixing speed is faster, then aerogel particle is smaller; Relative, when non-compatibility solvent viscosity is smaller and mixing speed is slower, then aerogel particle is bigger.
5. the present invention utilizes the temperature conditionss controlled in reforming step, you can shortens the time needed for replacement technique, most soon The preparation of hydrophily or hydrophobic aerogel particle can be continuously finished in 4 hours to 5 hours, improves the life of aeroge whereby Produce efficiency.
Therefore, aerogel particle of the present invention and preparation method thereof improvement in the past aeroge have that structure is uneven, outward appearance is broken and The problem of being difficult to lift heat-insulating properties.
Brief description of the drawings
Fig. 1 is the step schematic flow sheet of the embodiment of the present invention.
Fig. 2 is the step schematic flow sheet of the modified step of the embodiment of the present invention.
Fig. 3 aerogel particle scanning electron micrographs prepared by stirring condition under the conditions of 1200rpm for the present invention.
Fig. 4 aerogel particle scanning electron micrographs prepared by stirring condition under the conditions of 1800rpm for the present invention.
Fig. 5 is aerogel particle penetration type electron microphoto of the present invention.
Fig. 6 is the micro- enlarged photograph of aerogel particle penetration type electron of the present invention.
Fig. 7 is absorption and desorption curve of the aerogel particle of the invention without hydrophobicity reforming step under logical nitrogen Figure.
Fig. 8 is the hole distribution map of the present invention aerogel particle converted according to Fig. 7.
Fig. 9 is current scanning electron micrograph of the aerogel powder under 500 multiplying powers on the market.
Figure 10 is current scanning electron micrograph of the aerogel powder under 1000 multiplying powers on the market.
Figure 11 is current scanning electron micrograph of the aerogel powder under 5,000 multiplying powers on the market.
Figure 12 is current scanning electron micrograph of the aerogel powder under 10,000 multiplying powers on the market.
【Symbol description】
(S1) blend step (S2) hydrolysing step
(S3) condensation step (S4) (S40) post-processing step
(S5) hydrophobicity reforming step.
Embodiment
The primary efficacy of summary technical characteristic, the aerogel particle of the embodiment of the present invention and preparation method thereof can be in Following embodiments clearly appear from.
Please referring initially to Fig. 1, aerogel particle preparation method of the embodiment of the present invention is disclosed, is comprised the steps of:Blend step (S1), hydrolysing step (S2), condensation step (S3) and post-processing step (S4), wherein:
The blend step (S1):One silicone compounds are mixed into an organic solvent, to form a mixed solution.The siliconization Compound (alkoxysilane) is, for example, tetramethyl siloxanes (tetramethoxysilane;) or tetraethyl siloxanes TMOS (tetraethoxysilane;TEOS), the predecessor such as methyl silicate, the forerunner such as the silicone compounds or methyl silicate The content of thing is 2.1 molar percentages between 12.5 molar percentages.The content of the organic solvent is 97.9 molar percentages To between 87.5 molar percentages.
The hydrolysing step (S2):One sour catalyst is added into the mixed solution, so that reaction (hydrolysis) is hydrolyzed.Its In, the silicone compounds are 1 with sour catalyst content ratio:0.3~1:0.001, reaction is hydrolyzed.
The another silicone compounds are 1 with sour catalyst content ratio:0.001 to 1:0.3.When the silicone compounds and the acid The content ratio of catalyst is 1:When 0.001, then the time of the hydrolysis need to be up to 300 minutes, when the silicone compounds and the acid The content ratio of catalyst is 1:Hydrolysis time need to reach 10min when 0.3.It can thus be appreciated that the time needed for hydrolysis can be with the sour catalyst The increase of content and decline.
The condensation step (S3):One alkali catalyst is added into the mixed solution, to carry out condensation reaction (condensation). The mol ratio of the sour catalyst and the alcohol mixed solution and alkali catalyst water and alcohol mixed solution is, for example, 10:10 to 10:40.Should The mol ratio of alkali catalyst and the sour catalyst is, for example, 1.0:1.0 to 3.0:1.0.
In the alkali catalyst and alcohol mixed solution, the alkali catalyst content increase will substantially shorten condensation reaction time (i.e. The gelation time of aeroge).(alkali catalyst:Sour catalyst ratio is 1.0:Gelation about 1600 minutes when 1.0;Alkali catalyst:Acid touches Matchmaker's ratio is 3.0:Gelation is fallen to approximately 5 minutes when 1.0, therefore adjustable alkali catalyst content is with respect to the ratio of the sour catalyst content Example is with the time required to adjusting processing procedure.
Before the condensation reaction in the condensation step (S3) is nearly completed, the mixed solution can be initially formed colloidal sol shape (sol).The mixed solution is controlled in the hydrophobic dispersion solvent that a large amount of non-conforming systems are added under conditions of colloidal sol shape, gone forward side by side Row 1200rpm to 2000rpm quick stirring, make mixed solution under rapid mixing conditions by the hydrophobic dispersion solvent repulsion Influence, and gelation forms pearl shape or spherical aerogel particle, particle diameter about 600nm ± 300nm of foregoing aerogel particle.
So-called hydrophobic dispersion solvent can be C6 ~ C16 ketones, C6 ~ C16 ethers, C6 ~ C16 esters, C7 ~ C16 aromatic series Class, C8 ~ C20 alkanes, halogenation ethers, halogenation esters, halogenated aromatic class and halogenation alkanes etc..Specifically such as toluene, coal Oil, remove stain oil etc..
The post-processing step (S4):Foregoing aerogel particle is filtered out with a filter, it is then clear with the mixed liquor of ethanol, water Wash foregoing aerogel particle 3 to 4 times, foregoing aeroge is dried with after being vacuumized under 100 DEG C to 115 DEG C of temperature conditionss Grain, you can obtain spherical aerogel particle.
Continue please refer to Fig. 2, it is preferable that above-mentioned aerogel particle can further carry out hydrophobicity modification, mainly at this Also include a hydrophobicity reforming step (S5) after condensation step:The temperature of the mixed solution is set sequentially to change into one first temperature strip Part, a second temperature condition and one the 3rd temperature conditionss, first temperature conditionss are 78 DEG C to 82 DEG C, make the second of the mixed solution Alcohol is vaporized (ethyl alcohol boiling point is 78 DEG C), and the second temperature condition is 100 DEG C to 115 DEG C (boiling point of water is 100 DEG C), makes this The water of mixed solution is vaporized, and the 3rd temperature conditionss are 40 DEG C to 45 DEG C.
A chlorine is added in three temperature conditionss and is acylated organic molecule, the chlorine is acylated organic molecule and selected to be one or more From in by following formed group:Chlorination siloxanes, chlorine acyl-alkane complexes species, chlorine acyl benzene class.
Whereby, make the chlorine be acylated the monohydroxy of organic molecule and foregoing aerogel particle to react to each other, and make foregoing airsetting Glue particle produces hydrophobicity, and by the repulsive force between the hydrophobic dispersion solvent and foregoing aerogel particle, avoids foregoing gas Gel particle crushes.If above-mentioned aerogel particle changes with toluene through hydrophobicity reforming step (S5), the post-processing step (S40) Solvent cleans foregoing aerogel particle, with the acylated organic molecule that goes to dechlorinate, then vacuumizes again and dries foregoing aerogel particle.
Whereby, you can the aerogel particle of the high secondary um porous of spherical shape, size homogeneity is prepared, on the one hand can be with Outward appearance, the homogeneity of structure of aerogel particle are improved, improves application.In addition, it is acylated by heating vaporization and chlorine organic The addition of molecule, can rapid, high volume prepare hydrophobicity modification aeroge technology, make aeroge be easier to be expanded by volume production Big industry application scale.
Table one is referred to below, aerogel particle prepared by display this case embodiment, is utilized specific surface area analysis instrument (BET) The front and rear parameter comparison sheet of analysis modification:
In tableS BETFor the specific surface area of BET measurements;V poreFor the pore volume of BET measurements;D pFor the hole diameter of BET measurements;S microFor micropore specific area;V microFor micro pore volume.
Data is at ambient temperature, aerogel particle utilize specific surface area before being modified with Unit Weight and after modification in table Analyzer, under conditions of P/Po=0 is evacuated to, contained solvent in aerogel particle or the impurity of absorption are desorbed removal Afterwards, logical nitrogen (N2) make into aerogel particle aerogel particle absorption nitrogen (N2) to pressure reach saturation conditions under (P/Po= 1), then vacuumize carry out desorption process once again, make adsorption saturation nitrogen aerogel particle carry out nitrogen desorption, when desorption extremely The pressure of nitrogen (N2) reaches the condition of P/Po=0.At this in absorption and desorption process, absorption and the desorption of aerogel particle are measured Curve, and carry out analysis and can obtain above specific surface area related data.
It is continuous to refer to Fig. 3 and Fig. 4, utilize sweep electron microscope (SEM, scanning electron Microscope the microphoto of distribution and apparent size of the aerogel particle under different micro-scales) is captured, display is made The surface structure of standby aerogel particle has uniform, the spherical shape outward appearance of high homogeneity.
It is continuous to refer to Fig. 5 and Fig. 6, utilize sweep electron microscope (SEM, scanning electron Microscope internal structure and its hole distribution of the aerogel particle under different micro-scales) are captured.Show aeroge point Sub mutually aggregation forms nanoscale aerogel structure.
Continue referring to Fig. 7, in the display embodiment of the present invention, the aerogel particle without hydrophobicity reforming step is in logical nitrogen Under absorption and desorption curve;And Fig. 8 then shows absorption and the desorption curve of the aerogel particle without hydrophobicity reforming step It is converted into hole distribution map.
The explanation of summary embodiment, when can be fully understood by the present invention operation, use and the present invention produce the effect of, Embodiment described above is only presently preferred embodiments of the present invention, when can not limit the scope implemented of the present invention, i.e. Yi Benfa with this Bright claims and description of the invention content makees simple equivalent changes and modifications, in the range of all the category present invention covers.

Claims (9)

1. a kind of aerogel particle preparation method, it is characterised in that comprise the steps of:Blend step:By a silicone compound Thing mixes an organic solvent, to form a mixed solution;Hydrolysing step:One sour catalyst is added into the mixed solution, to enter water-filling Solution reaction;Condensation step:One alkali catalyst is added into the mixed solution, to carry out condensation reaction, and in the condensation reaction Add a hydrophobic dispersion solvent, and stirred, make the mixed solution in whipping process gelation and produce more airsettings Glue particle, wherein, in the condensation reaction, the mixed solution is stirred with 1200rpm to 2000rpm speed.
2. aerogel particle preparation method as claimed in claim 1, it is characterised in that:The hydrophobic dispersion solvent to be a kind of or A variety of solvents being selected from by following formed group:Ketone, ethers, esters, the fragrant same clan, alkanes.
3. aerogel particle preparation method as claimed in claim 2, it is characterised in that:Locate after also including after the condensation step Manage step:Foregoing aerogel particle is filtered out with a filter, foregoing aerogel particle is then cleaned with the mixed liquor of ethanol, water, Foregoing aerogel particle is dried in vacuo under 100 DEG C to 115 DEG C of temperature conditionss.
4. aerogel particle preparation method as claimed in claim 2, it is characterised in that:Also include one after the condensation step to dredge Water-based reforming step:The mixed solution is heated up, and vaporize aforementioned organic solvents, and add a chlorine and be acylated organic molecule, make The monohydroxy that the chlorine is acylated organic molecule and foregoing aerogel particle reacts to each other, and it is hydrophobic to produce foregoing aerogel particle Property, and avoid foregoing aerogel particle from crushing by the hydrophobic dispersion solvent.
5. aerogel particle preparation method as claimed in claim 4, it is characterised in that:The chlorine be acylated organic molecule to be a kind of or It is a variety of to be selected from by following formed group:Chlorination siloxanes, chlorine acyl-alkane complexes species, chlorine acyl benzene class.
6. aerogel particle preparation method as claimed in claim 4, it is characterised in that:The organic solvent includes what is mutually mixed Ethanol, water;In the hydrophobicity reforming step, the temperature of the mixed solution is set sequentially to change into one first temperature conditionss, one second Temperature conditionss and one the 3rd temperature conditionss, first temperature conditionss be 78 DEG C to 82 DEG C, the second temperature condition be 100 DEG C extremely 115 DEG C, the 3rd temperature conditionss are 40 DEG C to 45 DEG C, and the chlorine is added in three temperature conditionss and is acylated organic molecule.
7. aerogel particle preparation method as claimed in claim 4, it is characterised in that:Also wrapped after the hydrophobicity reforming step Include a post-processing step:Foregoing aerogel particle is filtered out with a filter, foregoing aerogel particle is then cleaned with toluene solvant, Foregoing aerogel particle is dried in vacuo again.
8. a kind of aerogel particle, it is characterised in that via made by the following steps:Blend step:By a silicone compounds An organic solvent is mixed, to form a mixed solution;Hydrolysing step:One sour catalyst is added into the mixed solution, to be hydrolyzed Reaction;Condensation step:One alkali catalyst is added into the mixed solution, to carry out condensation reaction, and added in the condensation reaction Enter a hydrophobic dispersion solvent, and stirred, make the mixed solution in whipping process gelation and produce more aeroges Particle, the particle diameter of foregoing aerogel particle is 600nm ± 300nm, wherein, in the condensation reaction, with 1200rpm extremely 2000rpm speed stirs the mixed solution.
9. aerogel particle as claimed in claim 8, it is characterised in that:The hydrophobic dispersion solvent is selected from for one or more In the solvent by following formed group:Ketone, ethers, esters, the fragrant same clan, alkanes.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110894167A (en) * 2019-09-26 2020-03-20 上海稀点新材料科技有限公司 Nano porous heat insulation material and preparation method thereof
CN111218024A (en) * 2018-11-27 2020-06-02 台湾气凝胶科技材料开发股份有限公司 Method for continuously preparing core-shell hydrophilic-hydrophobic bipolar composite aerogel powder
CN113563012A (en) * 2020-04-29 2021-10-29 台湾气凝胶科技材料开发股份有限公司 Preparation method of cold-resisting and heat-insulating hydrophobic aerogel composite jelly and related product thereof
CN113563046A (en) * 2020-04-29 2021-10-29 台湾气凝胶科技材料开发股份有限公司 Preparation method of high-temperature-resistant, heat-insulating and fireproof aerogel/inorganic fiber composite adhesive material and application of product thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007115860A1 (en) * 2006-04-12 2007-10-18 Bio-Ker Srl Sol-gel derived silica polymers for the sustained release of proteins
CN102341188A (en) * 2009-01-30 2012-02-01 阿力泽有限公司 Method for Attachment of Silicon-Containing Compounds to a Surface and for Synthesis of Hypervalent Silicon-Compounds
CN102448883A (en) * 2009-05-29 2012-05-09 赢创德固赛有限公司 Process for the preparation of an aerogel in pellets
CN102781977A (en) * 2010-02-18 2012-11-14 道康宁公司 Siloxane surface-modified hydrogel and hydrogel microparticle compositions
CN103328382A (en) * 2011-01-21 2013-09-25 Dic株式会社 Process for producing porous silica particles, resin composition for antireflection coatings, article with antireflection coating, and antireflection film
CN103570030A (en) * 2012-08-08 2014-02-12 佳能株式会社 Method for manufacturing a dispersion of hollow particles, an antireflective film, and an optical element
CN105271260A (en) * 2014-06-11 2016-01-27 中国科学院苏州纳米技术与纳米仿生研究所 Method for preparing hydrophobic silica aerogel through normal-pressure drying process

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007115860A1 (en) * 2006-04-12 2007-10-18 Bio-Ker Srl Sol-gel derived silica polymers for the sustained release of proteins
CN102341188A (en) * 2009-01-30 2012-02-01 阿力泽有限公司 Method for Attachment of Silicon-Containing Compounds to a Surface and for Synthesis of Hypervalent Silicon-Compounds
CN102448883A (en) * 2009-05-29 2012-05-09 赢创德固赛有限公司 Process for the preparation of an aerogel in pellets
CN102781977A (en) * 2010-02-18 2012-11-14 道康宁公司 Siloxane surface-modified hydrogel and hydrogel microparticle compositions
CN103328382A (en) * 2011-01-21 2013-09-25 Dic株式会社 Process for producing porous silica particles, resin composition for antireflection coatings, article with antireflection coating, and antireflection film
CN103570030A (en) * 2012-08-08 2014-02-12 佳能株式会社 Method for manufacturing a dispersion of hollow particles, an antireflective film, and an optical element
CN105271260A (en) * 2014-06-11 2016-01-27 中国科学院苏州纳米技术与纳米仿生研究所 Method for preparing hydrophobic silica aerogel through normal-pressure drying process

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
J.D. WELLS ET AL: ""Monodisperse, nonporous, spherical silica particles"", 《COLLOIDS AND SURFACES A: PHYSICOCHEMICAL AND ENGINEERING ASPECTS 》 *
汪多仁编: "《绿色化工助剂》", 31 January 2006, 科学技术文献出版社 *
蔡龙 等: ""酸碱催化剂浓度对柔性硅气凝胶性能和结构的影响"", 《化工学报》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111218024A (en) * 2018-11-27 2020-06-02 台湾气凝胶科技材料开发股份有限公司 Method for continuously preparing core-shell hydrophilic-hydrophobic bipolar composite aerogel powder
CN111218024B (en) * 2018-11-27 2022-05-13 台湾气凝胶科技材料开发股份有限公司 Method for continuously preparing core-shell hydrophilic-hydrophobic bipolar composite aerogel powder
CN110894167A (en) * 2019-09-26 2020-03-20 上海稀点新材料科技有限公司 Nano porous heat insulation material and preparation method thereof
CN113563012A (en) * 2020-04-29 2021-10-29 台湾气凝胶科技材料开发股份有限公司 Preparation method of cold-resisting and heat-insulating hydrophobic aerogel composite jelly and related product thereof
CN113563046A (en) * 2020-04-29 2021-10-29 台湾气凝胶科技材料开发股份有限公司 Preparation method of high-temperature-resistant, heat-insulating and fireproof aerogel/inorganic fiber composite adhesive material and application of product thereof
CN113563046B (en) * 2020-04-29 2023-03-14 台湾气凝胶科技材料开发股份有限公司 Preparation method of high-temperature-resistant, heat-insulating and fireproof aerogel/inorganic fiber composite adhesive material and application of product thereof

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