CN109734413A - A kind of improved silica powder/silica nano fibrous aerogel composite and preparation method thereof - Google Patents
A kind of improved silica powder/silica nano fibrous aerogel composite and preparation method thereof Download PDFInfo
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Abstract
The present invention provides improved silica powder/silica nano fibrous intersection graded composite aerogel materials and preparation method thereof.The improved silica powder/silica nano fibrous intersection graded composite aerogel material, it is characterized in that, the silica nano fibrous 3 D stereo frame structure as aeroge, uniformly filled with modified nano silica powder inside the gap formed between single nanofiber, monolith composite material is divided into three layers of different nano silica powder packed densities on thickness, and the 3 D stereo frame of silica nano fibrous formation makes it have good compression resilience and intensity.Gained 3 D stereo silicon-dioxide powdery/silica nano fibrous aerogel material bulk density is 10~1000mg/cm3, average pore size is 0.05~1000 μm, and tensile strength is 20~50kPa, compression rebound rate >=85%.Gained aerogel material internal structure is in the mesh for the three-dimensional framework that silicon-dioxide powdery is dispersed in silicon dioxide fibre formation, it is interlaced between fiber to be formed there through hole, while improving the mechanical strength of the aerogel material, its high porosity, aperture gauge structure are imparted, it is made to have broad application prospects in fields such as heat-insulation warm keeping, absorbing sound and lowering noises.
Description
Technical field
The present invention relates to high temperature resistant heat insulation material technical fields, more particularly, to a kind of improved silica powder/dioxy
SiClx nanofiber aerogel composite and preparation method thereof.
Background technique
The critical material of high temperature resistant, fire-retardant, heat-barrier material as fields such as spacecraft, guided missile, fire-fighting, thermotransports, has
It is widely applied demand.Silicon dioxide aerogel powder is a kind of novel porous with nanometer scale solid phase particulates and hole
Functional material, and its continuous three-dimensional net structure can also be controlled and be cut out on nanoscale.Aerosil tool
There are many unique performances, such as high porosity, high-specific surface area, low-density, ultra-low thermal conductivity, are currently used the widest
One of general high temperature resistant, fire-retardant, heat-barrier material；And nanofiber aerogel material is the airsetting with three-dimensional network space structure
Glue material, since its is all made of nanometer and fiber, to make it have minimum aperture, and its three dimensional tortuous network knot
Structure can substantially reduce its thermal coefficient, be excellent high temperature resistant heat insulation material.
The current main preparation methods of aerogel material are to be combined by sol-gel technique with supercritical technology, are obtained
It obtains and the three-dimensional porous network shape material constructed is coalesced by colloid or high polymer particulate.But since its brittleness is big, mechanical strength
The disadvantages of difference, preparation process complexity, higher cost, keep its durability in actual application environment poor.Domestic patent
CN104911901A, which is disclosed, to be prepared a kind of Static Spinning SiO2 nano fibrous membrane/SiO2 colloidal sol and combines and prepared silica
Composite aerogel.Foreign literature [Synthesis of Flexible Aerogel Composites Reinforced with
Electrospun Nanofibers and Microparticles for Thermal Insulation.[J].Journal
Of Nanomaterials, 2013, (2013) 1~8] it reports a kind of by electrostatic spinning PVDF tunica fibrosa/SiO2Colloidal sol is mutually tied
Silicon dioxide composite aerogel has been prepared in conjunction.Domestic patent CN201010515083.X discloses a kind of by glass fibre and two
The enhancing aeroge of the compound preparation of silica aerogel.Above-mentioned material is using micrometer fibers or nanofiber as aeroge
Fiber, is then impregnated into wet gel by the frame of material, and is prepared by sol-gel technique and Supercritical Drying Technology
It arrives.Above-mentioned material is obtained by sol-gel process, though resulting aerogel composite improves it to a certain extent
Mechanical property, but still be corpuscular type structure, that there are still brittleness is big for gained aerogel material, and flexibility is poor, powder is caducous scarce
Point, and in preparation method there is also complex process, time-consuming, raw material range of choice is narrow the deficiencies of.Domestic patent
CN201310201999.1 disclose it is a kind of by one dimension fibre through three-dimensional network reconstructing method obtain three-dimensional fiber aerogel material
And preparation method thereof, this method is compared with sol-gel technique, simple process, and raw material range of choice is wide, prepared airsetting
Glue material has a fully fibrous structure, but the mechanical strength of the material only leans between fiber and is intertwined the bonding point to be formed and provided,
There are still biggish deficiencies for the tensile strength and shear strength for making material, so that it is restricted in actual application environment.
Nanofiber is as a kind of novel superfine fibre with fibre diameter is small, fiber membrane aperture is small, large specific surface area
Etc. numerous advantages.Silica nano fibrous membrane has both ceramic and nanofiber dual as a kind of novel inorfil film
Advantage has the advantages such as high temperature resistant, heat-proof quality be good, in the heat-insulated field of inorganic high-temperature resistant with huge application prospect.It is inorganic
Nano silica aerogel powder equally has excellent heat-proof quality, but answers since its powder characteristics significantly limits it
With.It combines, silicon dioxide aerogel powder can be filled in silicon dioxide aerogel powder by silica nano fibrous
In the interfibrous hole of aerosil, the high temperature resistant heat insulation performance of significant increase entirety.But consider silicon dioxide powder
The caducous characteristic of body, by the way of intersecting graded composite, by the maximum of silicon-dioxide powdery as innermost layer, greatly
Loading of the silicon dioxide aerogel powder in silica nano fibrous is improved, whole thermal insulation is greatly improved
Can, while guaranteeing that silicon dioxide aerogel powder is not fallen off, performance is much better than other aeroges.
Summary of the invention
1. a kind of improved silica powder/silica nano fibrous production side for intersecting graded composite aerogel material
Method, which comprises the following steps:
1) slurries of the modified silicon dioxide aerogel powder of preparation:
Step 1: by mass fraction be 2~20% surfactant and 50~90% solvent with 700~1000 turns/
The speed divided stirs 30-40 minutes, keeps surfactant evenly dispersed in a solvent；
Add step 2: the aerosil of 3-15% is spaced 5 minutes equal equivalent (each one third) in three times
Add, is added in the surfactant being stirred and solvent mixed liquor, is dispersed；
Step 3: 5% modifying agent is added, into finely dispersed aerosil slurry with 500-800 revs/min
Speed stir 20-30 minutes, prepare modified aerosil slurry；
2) silicon-dioxide powdery/silica nano fibrous aerogel composite is prepared:
A: polymer, ethyl orthosilicate are dissolved in the first solvent, precursor solution is obtained；
B: precursor solution is subjected to electrostatic spinning, obtains presoma silica nano fibrous membrane；
C: presoma nano fibrous membrane is calcined, silica nano fibrous membrane is obtained；
D: silica nano fibrous membrane is dispersed in the second solvent, obtains silica nano fibrous membrane dispersion liquid,
Then by the slurries of the silicon dioxide aerogel powder of above-mentioned preparation and silica nano fibrous dispersion liquid 1:1,2:1,3:1,
2:1,1:1 mixing obtain five kinds of different mixed dispersion liquids, bonding are then added in the dispersion liquid of five kinds of different mixing proportions
Agent, and using segmentation freeze-drying curing molding, obtain silicon-dioxide powdery/silica nano fibrous composite dispersion liquid solidification
Body；
E: the second solvent in silicon-dioxide powdery/silica nano fibrous composite dispersion liquid solidified body is removed, is obtained
To silicon-dioxide powdery/silica nano fibrous composite aerogel.
2. improved silica powder according to claim 1/silica nano fibrous aerogel composite
Preparation method, which is characterized in that the surfactant includes anionic surfactant and cationic surfactant；It is described
Anionic surfactant includes at least one of stearic acid, neopelex；Preferably, the cationic surface
Activating agent packet quaternary ammonium compound.
3. preparation method according to claim 1, which is characterized in that the solvent is methanol, ethyl alcohol, propyl alcohol, fourth
One of alcohol, ethylene glycol are a variety of.
4. preparation method according to claim 1, which is characterized in that the modifying agent be Silane coupling agent KH550,
One of KH560 or KH570 or a variety of.
5. preparation method according to claim 1, which is characterized in that the binder includes organic binder and nothing
Machine binder；Preferably, the organic binder includes at least one in polyethylene oxide, polypropylene oxide and polyvinyl acetate
Kind；The inorganic binder includes silica solution.
6. preparation method according to claim 1, which is characterized in that the polymer is selected from polyvinyl alcohol, gathers partially
At least one of vinyl fluoride, polyethylene glycol oxide, polyvinyl acetate, polyvinyl butyral, polyvinylpyrrolidone；With/
Or, first solvent and second solvent are each independently selected from water, ethyl alcohol, ethylene glycol, isopropanol, glycerine, second
Acyl acetone, at least one of glacial acetic acid and n,N-Dimethylformamide.
7. preparation method according to claim 1, which is characterized in that in step (b), using electrospinning device
Carry out electrostatic spinning, the parameter of electrostatic spinning are as follows: humidity 20%-70%, rate of flooding 0.1-10mL/h, voltage 8-50kV connect
Receiving apparatus distance 10-30cm between spinning nozzle；And/or in step (c), when calcining, calcination temperature is stepped up from room temperature
To 600-1000 DEG C, heating rate is 0.5-10 DEG C/min, and keeps the temperature 0-480min；And/or in step (d), using mashing
Silica nano fibrous membrane is dispersed in the second solvent by method, beating rate 3000-20000rpm.
8. preparation method according to claim 1, which is characterized in that in step (d), the stage curing molding
Selected from least one of freezing curing molding, colloidal sol curing molding and gel solidification molding, it is shaped to point wherein stage curing
Not by the slurries and silica nano fibrous dispersion liquid of 1:1,2:1,3:1,2:1,1:1 silicon dioxide aerogel powder mixed
After being refrigerated to g., jelly-like, the mixing dispersion g., jelly-like substance of 2:1,3:1,2:1,1:1 are being sequentially placed to the mixing dispersion in 1:1
On g., jelly-like, freeze forming is further played；In step (e), the second solvent is removed using dry, the drying is dry selected from normal pressure
Dry, supercritical drying is freeze-dried, is dried under reduced pressure, being dried in vacuo, at least one of infra-red drying and spray drying.
9. preparation method according to claim 1-8, which is characterized in that molten by second in step (e)
Bonding intensive treatment is carried out after agent removal, to improve the adhesion strength of binder and ceramic nanofibers film；Preferably, described viscous
It ties intensive treatment and is selected from least one of radiation treatment, high-temperature process, ultraviolet irradiation processing, microwave treatment and ultrasonic treatment.
10. a kind of improved silica powder/silica nano fibrous aerogel composite, which is characterized in that root
It is obtained according to the described in any item preparation methods of claim 1-8；Preferably, the improved silica powder/silica is received
Rice fiber composite aerogel material bulk density is 0.9-450mg/cm3, specific surface area 0.1-1500m/g.
Beneficial effect:
1. the present invention is with silicon dioxide aerogel powder by combining electrostatic spinning is silica nano fibrous, so that
Nano silica aerogel powder is firmly locked in the slight void of nanofiber formation, and traditional glass fibre is overcome
It ties up that aeroge brittleness is big, the caducous problem of powder, is greatly improved the actual use performance of aeroge.
2. the present invention is by overcoming nanoscale aerogel powder uniform stable dispersion inside nanofiber aeroge
The big deficiency of air draught convection current caused by hole is greatly improved the heat-proof quality of simple nanofiber aeroge.
3. by the way of intersecting graded composite, by the maximum of silicon dioxide aerogel powder as innermost layer, greatly
Improve loading of the silicon dioxide aerogel powder in silica nano fibrous, be greatly improved whole heat-insulated
Performance, while guaranteeing that silicon dioxide aerogel powder is not fallen off, performance is much better than other aeroges.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, art technology
Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Fixed range.
Embodiment one:
1) slurries of the modified silicon dioxide aerogel powder of preparation:
Step 1: being 10% surfactant and 60% solvent with 800 revs/min of speed stirring 35 by mass fraction
Minute, keep surfactant evenly dispersed in a solvent；
Step 2: 5% aerosil is added to the surfactant being stirred and solvent mixes according to segmentation
It closes in liquid, is dispersed；
Step 3: 5% modifying agent is added, into finely dispersed aerosil slurry with 600 revs/min of speed
Degree stirring 20 minutes, prepares modified aerosil slurry；
2) silicon-dioxide powdery/silica nano fibrous aerogel composite is prepared:
A: polymer, ethyl orthosilicate are dissolved in the first solvent, precursor solution is obtained；
B: precursor solution is subjected to electrostatic spinning, obtains presoma silica nano fibrous membrane；
C: presoma nano fibrous membrane is calcined, silica nano fibrous membrane is obtained；
D: silica nano fibrous membrane is dispersed in the second solvent, obtains silica nano fibrous membrane dispersion liquid,
Then by the slurries of the silicon dioxide aerogel powder of above-mentioned preparation and silica nano fibrous dispersion liquid 1:1,2:1,3:1,
2:1,1:1 mixing obtain five kinds of different mixed dispersion liquids, bonding are then added in the dispersion liquid of five kinds of different mixing proportions
Agent, and using segmentation freeze-drying curing molding, obtain silicon-dioxide powdery/silica nano fibrous composite dispersion liquid solidification
Body；
E: the second solvent in silicon-dioxide powdery/silica nano fibrous composite dispersion liquid solidified body is removed, is obtained
To silicon-dioxide powdery/silica nano fibrous composite aerogel.
Claims (10)
1. a kind of improved silica powder/silica nano fibrous production method for intersecting graded composite aerogel material,
Characterized by comprising the following steps:
1) slurries of the modified silicon dioxide aerogel powder of preparation:
Step 1: being 2~20% surfactant and 50~90% solvent with 700~1000 revs/min by mass fraction
Speed stirs 30-40 minutes, keeps surfactant evenly dispersed in a solvent；
It adds, adds step 2: the aerosil of 3-15% is spaced 5 minutes equal equivalent (each one third) in three times
It is added in the surfactant being stirred and solvent mixed liquor, is dispersed；
Step 3: 5% modifying agent is added, into finely dispersed aerosil slurry with 500-800 revs/min of speed
Degree stirring 20-30 minutes, prepares modified aerosil slurry；
2) silicon-dioxide powdery/silica nano fibrous aerogel composite is prepared:
A: polymer, ethyl orthosilicate are dissolved in the first solvent, precursor solution is obtained；
B: precursor solution is subjected to electrostatic spinning, obtains presoma silica nano fibrous membrane；
C: presoma nano fibrous membrane is calcined, silica nano fibrous membrane is obtained；
D: silica nano fibrous membrane is dispersed in the second solvent, obtains silica nano fibrous membrane dispersion liquid, then
By the slurries of the silicon dioxide aerogel powder of above-mentioned preparation and silica nano fibrous dispersion liquid 1:1,2:1,3:1,2:1,
1:1 mixing obtains five kinds of different mixed dispersion liquids, binder is then added in the dispersion liquid of five kinds of different mixing proportions, and
Curing molding is freeze-dried using segmentation, obtains silicon-dioxide powdery/silica nano fibrous composite dispersion liquid solidified body；
E: the second solvent in silicon-dioxide powdery/silica nano fibrous composite dispersion liquid solidified body is removed, obtains two
Silica powder/silica nano fibrous composite aerogel.
2. improved silica powder according to claim 1/silica nano fibrous aerogel composite preparation
Method, which is characterized in that the surfactant includes anionic surfactant and cationic surfactant；It is described yin from
Sub- surfactant includes at least one of stearic acid, neopelex；Preferably, the cation surface activating
Agent packet quaternary ammonium compound.
3. preparation method according to claim 1, which is characterized in that the solvent is methanol, ethyl alcohol, propyl alcohol, butanol, second
One of glycol is a variety of.
4. preparation method according to claim 1, which is characterized in that the modifying agent be Silane coupling agent KH550,
One of KH560 or KH570 or a variety of.
5. preparation method according to claim 1, which is characterized in that the binder includes organic binder and inorganic viscous
Tie agent；Preferably, the organic binder includes at least one of polyethylene oxide, polypropylene oxide and polyvinyl acetate；
The inorganic binder includes silica solution.
6. preparation method according to claim 1, which is characterized in that the polymer is selected from polyvinyl alcohol, polyvinylidene fluoride
At least one of alkene, polyethylene glycol oxide, polyvinyl acetate, polyvinyl butyral, polyvinylpyrrolidone；And/or institute
It states the first solvent and second solvent is each independently selected from water, ethyl alcohol, ethylene glycol, isopropanol, glycerine, levulinic
Ketone, at least one of glacial acetic acid and n,N-Dimethylformamide.
7. preparation method according to claim 1, which is characterized in that in step (b), carried out using electrospinning device
Electrostatic spinning, the parameter of electrostatic spinning are as follows: humidity 20%-70%, rate of flooding 0.1-10mL/h, voltage 8-50kV receive dress
Set the distance 10-30cm between spinning nozzle；And/or in step (c), when calcining, calcination temperature from room temperature be stepped up to
600-1000 DEG C, heating rate is 0.5-10 DEG C/min, and keeps the temperature 0-480min；And/or in step (d), using beating method
Silica nano fibrous membrane is dispersed in the second solvent, beating rate 3000-20000rpm.
8. preparation method according to claim 1, which is characterized in that in step (d), the stage curing molding is selected from
At least one of curing molding, colloidal sol curing molding and gel solidification molding are freezed, wherein stage curing be shaped to respectively to
The slurries and silica nano fibrous dispersion liquid of the silicon dioxide aerogel powder of 1:1,2:1,3:1,2:1,1:1 mixing freeze
To g., jelly-like, the mixing dispersion g., jelly-like substance of 2:1,3:1,2:1,1:1 are being sequentially placed to the mixing dispersion jelly in 1:1
On shape, freeze forming is further played；In step (e), remove the second solvent using dry, the drying be selected from constant pressure and dry,
Supercritical drying is freeze-dried, is dried under reduced pressure, being dried in vacuo, at least one of infra-red drying and spray drying.
9. preparation method according to claim 1-8, which is characterized in that in step (e), the second solvent is gone
Bonding intensive treatment is carried out after removing, to improve the adhesion strength of binder and ceramic nanofibers film；Preferably, the bonding is strong
Change processing selected from least one of radiation treatment, high-temperature process, ultraviolet irradiation processing, microwave treatment and ultrasonic treatment.
10. a kind of improved silica powder/silica nano fibrous aerogel composite, which is characterized in that according to power
Benefit requires the described in any item preparation methods of 1-8 to obtain；Preferably, the improved silica powder/silica nanometer is fine
Dimension aerogel composite bulk density is 0.9-450mg/cm3, specific surface area 0.1-1500m/g.
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| CN110424067A (en) * | 2019-07-08 | 2019-11-08 | 清华大学 | A kind of flexibility silicon dioxide fibre aerogel material and preparation method thereof |
| CN110656443A (en) * | 2019-08-26 | 2020-01-07 | 深圳市大毛牛新材料科技有限公司 | Soft, light, thin and super-thermal aerogel filling material for shoes, clothes, bedding and manufacturing method thereof |
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| CN111268995A (en) * | 2019-11-19 | 2020-06-12 | 重庆文理学院 | Honeycomb nano-pore structure composite heat insulation material and preparation method thereof |
| CN111840880A (en) * | 2020-08-03 | 2020-10-30 | 安华消防新材料科技（江苏）有限公司 | Aerogel fire extinguishing agent and preparation method thereof |
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| CN112661482A (en) * | 2021-01-11 | 2021-04-16 | 中广核研究院有限公司 | Fiber composite aerogel material and preparation method and application thereof |
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| CN113277831A (en) * | 2021-04-12 | 2021-08-20 | 南京睿扬光电技术有限公司 | Preparation method of modified composite silicon dioxide aerogel |
| CN113277831B (en) * | 2021-04-12 | 2022-05-17 | 南京睿扬光电技术有限公司 | Preparation method of modified composite silicon dioxide aerogel |
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| CN115322502B (en) * | 2022-07-14 | 2023-10-13 | 中国科学院上海硅酸盐研究所 | Silica aerogel reinforced polyvinyl alcohol composite material and preparation method thereof |
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