CN108467276A - A kind of preparation method of electrostatic spinning nano fiber enhancing aerosil - Google Patents
A kind of preparation method of electrostatic spinning nano fiber enhancing aerosil Download PDFInfo
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- CN108467276A CN108467276A CN201810227701.7A CN201810227701A CN108467276A CN 108467276 A CN108467276 A CN 108467276A CN 201810227701 A CN201810227701 A CN 201810227701A CN 108467276 A CN108467276 A CN 108467276A
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- 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
- 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
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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- 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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
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Abstract
A kind of method that the enhanced aerosil block of electrostatic spinning nano fiber of excellent in mechanical performance is quickly prepared the present invention relates to constant pressure and dry.The advantages of used nanofiber is prepared using electrostatic spinning, and obtained nanofiber enhancing aerosil had not only maintained low-density, high porosity, but also overcome the big disadvantage of globality poor, brittleness.The silicon dioxide gel that the present invention is formed after being hydrolyzed using alkoxy silane and makes nanofiber be uniformly distributed therein as the receiving body of electrostatic spinning；So that silicon dioxide gel is formed gel by catalyst of ammonium hydroxide, then carry out aging and modification, electrostatic spinning nano fiber, which is made, enhances aerosil.The outstanding feature of this method is without dangerous and expensive supercritical drying, and easy to operate, process control, the period is short, at low cost, can be continuously produced, and obtained product physical property is excellent, and has excellent mechanical property.
Description
Technical field
The present invention relates to a kind of enhancing composite silicon dioxide aerogel block bodies, especially design with Electrospun nano-fibers
For reinforcement, by combination process, exchange of solvent, surface is modified and constant pressure and dry prepares the enhanced dioxy of electrostatic spinning nano fiber
The method of SiClx aeroge.
Background technology
Aerosil is a kind of novel porous functional material with nanometer scale solid phase particulates and hole, and
And its continuous three-dimensional net structure can also be controlled and be cut out on nanoscale.Aerosil has many unique
Performance, such as high porosity, high-specific surface area, low-density, ultralow dielectric and thermal coefficient.Aerosil has
Excellent properties be allowed in heat-insulation and heat-preservation, thermal insulation, aerospace, catalyst and its carrier, energy conservation and environmental protection, petrochemical industry, medicine
The fields such as object release have broad application prospects.
Currently, the main problem that aerosil industrialization and application face includes：
1. ripe easy preparation process not yet, aerosil is mainly the method by supercritical drying at present
It obtains, but this drying means is dangerous, condition is harsh, with high costs.The constant pressure and dry work of a large amount of mild conditions in recent years
The studied preparation applied to aerosil of skill, although aerosil and supercritical drying prepared by these methods
The physical property of the product of dry acquisition is closer to, but these methods preparation process complexity, long preparation period, solvent-oil ratio
Greatly, the modification by-product of a large amount of waste liquid and pollution is generated, therefore, it is difficult to be mass produced；
2. the poor mechanical property of aerosil, there are the low defect of brittleness height and intensity, especially constant pressure and dries to prepare
Product embrittlement is serious in the drying process, it is difficult to the material as single kind is applied in Practical Project；
Therefore, how aerosil is prepared in easy preparation process, while improving the whole of aerosil
Body and flexibility are of great immediate significance to extension aeroge industrialization and application, improve silica airsetting at present
In the mechanical property of glue and the method for globality, it is that one kind taking into account silica airsetting to prepare fiber-reinforcement silicon dioxide aerogel
The method of the porous property and mechanical property of glue, and currently solve the problems, such as this main path.
The preparation method for the fiber-reinforcement silicon dioxide aerogel reported in patent at present is mainly or using a diameter of micro-
The staple fiber or fibrofelt of meter level.Such as glass fibre is scattered in silicon dioxide gel, by aging, exchange of solvent and front three
The hydrophobically modified of base chlorosilane prepares fibre-reinforced aerosil block under the conditions of constant pressure and dry（Publication number：
CN101973752A）, this method prepare composite aerogel have certain globality, the porous excellent of aeroge, but
Composite aerogel is there are still larger brittleness, frangibility, mechanical property are poor, and preparation process is related to complicated constant pressure and dry
Technique is difficult to mass produce.Additionally by the method for infiltration by the three-dimensional framework of silicon dioxide gel infiltrated fiber felt, gas
Gel and fibrofelt or three-dimensional porous skeleton structure carry out compound preparing silicon dioxide composite aerogel（Such as publication number：
CN102701700A）, product physical property made from this method is poor, although mechanical strength increases, but composite aerogel
Flexibility can not still improve, easily cause aeroge substrate under flecition and the phenomenon that reinforcing material isolates and falls off.It is open
Mentioned in number patent for being CN1592651A the continuous fiber tire for using the fiber of low-titer to constitute prepared for reinforcing material it is compound
Aeroge, which has high-flexibility, but this method needs complicated craft woven to form fluffy fiber tire, and
And aeroge is combined with the filled type of batts so that the bond strength of composite material is limited.
Invention content
The purpose of the present invention is to provide a kind of simple for process, with short production cycle, shape of product controllably, can be continuously produced
The preparation method of the electrostatic spinning nano fiber enhancing aerosil block materials of excellent in mechanical performance.
The technical scheme is that using electrostatic spinning nano fiber as reinforcement, by the preparation of composite material, pass through
The composite silicon dioxide aerogel block body material of excellent in mechanical performance is made in constant pressure and dry.
The specific preparation method of electrostatic spinning nano fiber enhancing aerosil of the present invention includes following step
Suddenly：
1）Alkoxy silane, absolute ethyl alcohol and deionized water are mixed, pH value of solution is adjusted to 3 ~ 4 using hydrochloric acid, magnetic agitation
12 ~ 24 h make silane be hydrolyzed, and obtain solution A；
2）It dissolves a polymer in and forms spinning solution in organic solvent, spinning solution is stretched under high voltage electrostatic field, is formed by curing
It is molten to obtain nanofiber composite silicon dioxide using solution A as the collection of liquid phase receiving body and evenly dispersed nanofiber for nanofiber
Glue；
3）The pH of dioxide composite Ludox is adjusted to 8 ~ 8.5 using ammonium hydroxide, obtains composite silicon dioxide wet gel；It will be wet solidifying
Glue is immersed in progress gel aging in ethanol solution, then the gel after aging is immersed in trim,ethylchlorosilane or hexamethyl
In the mixed solution of two silicon amine, absolute ethyl alcohol and n-hexane, surface modification is carried out, modified wet gel carries out constant pressure and dry,
Electrostatic spinning nano fiber enhancing aerosil is obtained, obtained electrostatic spinning nano fiber enhances aerosil
White bulk.
In step 1）In, the alkoxy silane is tetraethyl orthosilicate（TEOS）Or positive quanmethyl silicate（TMOS）, press
Molar ratio, alkoxy silane：Deionized water：Absolute ethyl alcohol=1：（0.2~0.6）：（10~20）；The time of the mixing is
12~24h；
In step 2）In, the type of the polymer includes polyacrylonitrile, polyamide, polymethyl methacrylate and acetate fiber
Element etc.；The spinning condition of the polymer can be：15 ~ 22 kV of voltage, 1 ~ 2 ml/h of flow velocity receive 10 ~ 15 cm of distance, spinning
0.5 ~ 3 h of time；The mass ratio of the electrostatic spinning nano fiber and silicon dioxide gel is preferably 1：（100~500）；
In step 3）In, the temperature of the aging can be 25 ~ 80 DEG C, and the time of aging can be 12 ~ 24 h；The compound dioxy
SiClx wet gel is soaked in trim,ethylchlorosilane（TMCS）Or hmds（HMDS）, absolute ethyl alcohol and n-hexane mixing
In solution, soaking time is 1 ~ 2 day；Trim,ethylchlorosilane or hmds by volume：Absolute ethyl alcohol：N-hexane can be
1：（1~3）：（6~12）, the soaking time is 12 ~ 24 h；The technological process of the constant pressure and dry is preferably：Modified answers
It closes silica wet gel and keeps the temperature 1 ~ 2 h at 40 ~ 60 DEG C, be then warming up to 110 ~ 130 DEG C of 4 ~ 6 h of heat preservation, heating rate is equal
For 1 ~ 10 DEG C/min.
The porosity of the electrostatic spinning nano fiber enhancing aerosil obtained is 90 ~ 96%, density is 0.1 ~
0.2 g/cm3, specific surface area is 500 ~ 1000 m2/ g, hydrophobic angle are 140 ~ 150 °, and aperture concentrates on 2 ~ 50 nm.
Electrostatic spinning nano fiber prepared by the present invention enhances aerosil using electrostatic spinning nano fiber as dioxy
The reinforcement of SiClx aeroge, electrostatic spinning nano fiber have small fibre diameter, large specific surface area, distribution of fiber diameters uniform
The characteristics of, and nanofiber preferably can disperse to form fluffy three-dimensional net structure, Static Spinning in silicon dioxide gel
Nanofiber can be with nanometer grade silica aeroge skeleton in the microcosmic upper uniform compound structure of formation.The above feature has
Conducive to obtain mechanical property it is good and with preferably flexible aerosil block；In addition, nanofiber is compound right
The impact on physical properties of aerosil is small, therefore the porous property that aerosil is excellent, as high-specific surface area,
High porosity, high mesoporous pore volume will not be significantly affected, and the electrostatic spinning nano fiber obtained from enhances silica
Aeroge has excellent physical property.
The present invention prepares electrostatic spinning nano fiber enhancing aerosil by constant pressure and dry must regulate and control Nanowire
The composite construction of dimension and aerosil, forming nanofiber that is uniform, stablizing composite construction enhances silica airsetting
Glue also needs to the surface group of modified composite silicon dioxide wet gel in addition, avoid wet gel during constant pressure and dry substantially
Degree, which is shunk, obtains closely knit xerogel structure.Therefore, the homogeneity, dispersibility and rational solution of nanofiber are controlled
Proportioning, combination process and modifying process prepare electrostatic spinning nano fiber to constant pressure and dry enhances aerosil to closing weight
It wants.
Compared with the prior art, the present invention has following outstanding advantages：
The present invention prepares electrostatic spinning nano fiber using constant pressure and dry enhances aerosil, due to using constant pressure and dry work
Skill, therefore have the characteristics that at low cost, simple for process；Composite material maintains aerosil low-density, high ratio simultaneously
The excellent physical property such as surface area and high porosity；In addition electrostatic spinning nano fiber dispersion and mutually entanglement are distributed in titanium dioxide
In silica aerogel matrix, nanofiber is mutually interspersed with gel skeleton, enhances gel skeleton, forms dual network and intert mutually
Composite aerogel structure, the compound crack propagation for inhibiting aerosil in constant pressure and dry of nanofiber can
To obtain blockiness excellent dioxide composite silica aerogel；It is formd with aerosil additionally, due to nanofiber micro-
Uniform compound, the enhancing due to nanofiber and the toughening effect seen, obtained electrostatic spinning nano fiber enhancing titanium dioxide
There is silica aerogel excellent flexibility, silica aerogel particles will not there is the defect for the picking that falls off.In conclusion
By electrostatic spinning nano fiber enhance aerosil method, can be effectively improved aerosil intensity difference,
Brittleness is big, the easy fragmentation of the aeroge that constant pressure and dry obtains, can not material practical application as a whole defect.
Description of the drawings
Fig. 1 is the photo that electrostatic spinning nano fiber prepared by the present invention enhances aerosil block.
Fig. 2, which is the electrostatic spinning nano fiber of preparation example 1 of the present invention, enhances the stereoscan photograph of aerosil.
Fig. 3, which is the electrostatic spinning nano fiber of preparation example 1 of the present invention, enhances the N of aerosil2Adsorption and desorption isotherms.
In figure 3, abscissa is relative pressure（P/P0）, ordinate is adsorption volume（cm3/g）.
Fig. 4, which is the electrostatic spinning nano fiber of preparation example 1 of the present invention, enhances the graph of pore diameter distribution of aerosil.Scheming
In 4, abscissa is aperture（nm）, ordinate is pore volume（cm3/g）.
Fig. 5 is the flexibility photo of the flexible silica aerogel of preparation example 1 of the present invention.
Specific implementation mode
Below by embodiment combination attached drawing, the invention will be further described.
Embodiment 1
Material molar ratio：TEOS：Ethyl alcohol：Water=1：10：0.4, the absolute ethyl alcohol of the TEOS of 5 ml and 13 ml are mixed, then
1.8 ml water are added, the pH to 3 ~ 4 that hydrochloric acid solution adjusts mixed solution is added, persistently stirs 12 h to promote the hydrolysis of silicon source；
Polyacrylonitrile is dissolved with dimethylformamide, the spinning condition of Static Spinning polyacrylonitrile nanofiber：Voltage is 15 kV, flows
Speed is 1 ml/h, reception distance is 15 cm, the spinning time is 1 h, and the polyacrylonitrile nanofiber of Static Spinning is passed through titanium dioxide
Ludox is collected and dispersion, and a certain amount of ammonium hydroxide is added so that dioxide composite Ludox forms gel.Wet gel is placed in again
Aging is carried out in ethanol solution, aging temperature is 50 DEG C, and gel sample, which is immersed in solution batch volume ratio, after aging is
TMCS：Absolute ethyl alcohol：N-hexane=1：2：2 days modified in 8 mixed solution, wherein TMCS is 5 ml, is removed and is modified with n-hexane
Liquid and the drying that heats up in atmospheric conditions.
Drying process is：Modified composite silicon dioxide wet gel keeps the temperature 2 h at 40 DEG C, is then warming up to 130 °
C keeps the temperature 6 h, and heating rate is 1 DEG C/min.
The density of the Static Spinning polyacrylonitrile nanofiber enhancing aerosil of the preparation is 0. 15 g/
cm3, specific surface area is 890 m2/ g, average pore size are 9.7 nm, and pore volume is 2.15 cm3/g。
Embodiment 2
Material molar ratio：TEOS：Ethyl alcohol：Water=1：15：0.6, the absolute ethyl alcohol of the TEOS of 5 ml and 19.5 ml are mixed,
2.7 ml water are added, hydrochloric acid solution is added and adjusts mixed solution pH to 3 ~ 4, lasting stirring is for 24 hours to promote the hydrolysis of silicon source；It will
Polymethyl methacrylate is dissolved with dimethylformamide, the spinning condition of Static Spinning polymethyl methacrylate nano fiber：
Voltage is 18 kV, flow velocity is 1 ml/h, reception distance is 15 cm, the spinning time is 3 h, by the polymethylacrylic acid of Static Spinning
Methyl esters nanofiber is collected and is disperseed by silicon dioxide gel, a certain amount of ammonium hydroxide is added so that dioxide composite Ludox
Form gel.Wet gel is placed in ethanol solution again and carries out aging, aging temperature is 50 DEG C, by gel sample after aging
It is HMDS that product, which are immersed in solution batch volume ratio,：Absolute ethyl alcohol：N-hexane=1：1：It is 2 days modified in 8 mixed solution, wherein
HMDS is 5 ml, and modification liquid and the drying that heats up in atmospheric conditions are removed with n-hexane.
Drying process is：Modified composite silicon dioxide wet gel keeps the temperature 1 h at 60 DEG C, is then warming up to 110
DEG C heat preservation 6 h, heating rate is 5 DEG C/min.
The density of the Static Spinning polymethyl methacrylate nano fiber-reinforcement silicon dioxide aerogel of the preparation is 0.
2 g/cm3, specific surface area is 950 m2/ g, average pore size are 7.5 nm, and pore volume is 1.80 cm3/g。
Embodiment 3
Material molar ratio：TMOS：Ethyl alcohol：Water=1：10：0.4, the absolute ethyl alcohol of the TMOS of 3.3 ml and 13 ml are mixed,
1.8 ml water are added, hydrochloric acid solution is added and adjusts mixed solution pH to 3 ~ 4, lasting stirring is for 24 hours to promote the hydrolysis of silicon source；It will
Polyamide is dissolved with dimethylformamide, the spinning condition of Static Spinning polyamide nanofiber：Voltage is 18 kV, flow velocity 2
Ml/h, distance is received as 15 cm, the spinning time is 1 h, and Static Spinning polyamide nanofiber is collected by silicon dioxide gel
And dispersion, a certain amount of ammonium hydroxide is added so that dioxide composite Ludox forms gel.It is molten that wet gel is placed in absolute ethyl alcohol again
Aging is carried out in liquid, aging temperature is 60 DEG C, and it is TMCS that gel sample, which is immersed in solution batch volume ratio, after aging：It is anhydrous
Ethyl alcohol：N-hexane=1：3：1 day modified in 8 mixed solution, wherein TMCS is 5 ml, removes modification liquid with n-hexane and normal
Heat up drying under the conditions of pressure.
Drying process is the same as embodiment 1.
The density of the Static Spinning polyamide nanofiber enhancing aerosil of the preparation is 0. 12 g/cm3,
Specific surface area is 800 m2/ g, average pore size are 10.8 nm, and pore volume is 2.16 cm3/g。
Embodiment 4
Material molar ratio：TMOS：Ethyl alcohol：Water=1：20：0.4, the absolute ethyl alcohol of the TMOS of 3.3 ml and 26 ml are mixed,
1.8 ml water are added, hydrochloric acid solution is added and adjusts mixed solution pH to 3 ~ 4, persistently stir 12h to promote the hydrolysis of silicon source；It will
Polyacrylonitrile is dissolved with dimethylformamide, and the spinning condition of Static Spinning polyacrylonitrile nanofiber is：Voltage is 18 kV, flows
Speed is 1 ml/h, reception distance is 15 cm, the spinning time is 0.5 h, and the polyacrylonitrile nanofiber of Static Spinning is passed through dioxy
SiClx colloidal sol is collected and dispersion, and a certain amount of ammonium hydroxide is added so that dioxide composite Ludox forms gel.Wet gel is set again
Aging is carried out in ethanol solution, aging temperature is 40 DEG C, and gel sample is immersed in solution batch volume ratio after aging
For HMDS：Absolute ethyl alcohol：N-hexane=1：3：1 day modified in 8 mixed solution, wherein HMDS is 6 ml, is changed with n-hexane washout
Property liquid and the drying that heats up in atmospheric conditions.
Drying process is the same as embodiment 1.
The density of the Static Spinning polyacrylonitrile nanofiber enhancing aerosil of the preparation is 0. 12 g/
cm3, specific surface area is 908 m2/ g, average pore size are 10.2 nm, and pore volume is 2.32 cm3/g。
Embodiment 5
Material molar ratio：TEOS：Ethyl alcohol：Water=1：15：0.2, the absolute ethyl alcohol of the TEOS of 5 ml and 19.5 ml are mixed,
0.9 ml water is added, hydrochloric acid solution is added and adjusts mixed solution pH to 3 ~ 4, lasting stirring is for 24 hours to promote the hydrolysis of silicon source；It will
Cellulose acetate acetone solution, the spinning condition of Static Spinning cellulose acetate nanofiber：Voltage is 20 kV, flow velocity 1
Ml/h, it receives apart from being 1 h for 15 cm, spinning time, Static Spinning cellulose acetate nanofiber is passed through into silicon dioxide gel
It collects and disperses, a certain amount of ammonium hydroxide is added so that dioxide composite Ludox forms gel.Wet gel is placed in anhydrous second again
Aging is carried out in alcoholic solution, aging temperature is 60 DEG C, and it is TMCS that gel sample, which is immersed in solution batch volume ratio, after aging：
Absolute ethyl alcohol：N-hexane=1：1：2 days modified in 8 mixed solution, wherein TMCS is 6 ml, and modification liquid is removed simultaneously with n-hexane
Heat up drying in atmospheric conditions.
Drying process is：Modified composite silicon dioxide wet gel keeps the temperature 1 h at 60 DEG C, is then warming up to 130
DEG C heat preservation 4 h, heating rate is 10 DEG C/min.
The density of the Static Spinning cellulose acetate nanofiber enhancing aerosil of the preparation is 0.15 g/
cm3, specific surface area is 785 m2/ g, average pore size are 10.7 nm, and pore volume is 2.10 cm3/g。
Embodiment 6
Material molar ratio：TEOS：Ethyl alcohol：Water=1：20：0.6, the absolute ethyl alcohol of the TEOS of 5 ml and 26 ml are mixed, then
2.7 ml water are added, hydrochloric acid solution is added and adjusts mixed solution pH to 3 ~ 4, lasting stirring is for 24 hours to promote the hydrolysis of silicon source；It will gather
Acrylonitrile acetone solution, the spinning condition of electrostatic spinning polyacrylonitrile nanofiber：Voltage is 15 kV, flow velocity be 1 ml/h,
It is 2 h that distance, which is received, as 10 cm, spinning time, and the polyacrylonitrile nanofiber of Static Spinning is collected by silicon dioxide gel
And dispersion, a certain amount of ammonium hydroxide is added so that dioxide composite Ludox forms gel.It is molten that wet gel is placed in absolute ethyl alcohol again
Aging is carried out in liquid, aging temperature is 60 DEG C, and it is TMCS that gel sample, which is immersed in solution batch volume ratio, after aging：It is anhydrous
Ethyl alcohol：N-hexane=1：3：2 days modified in 12 mixed solution, wherein TMCS is 5 ml, removes modification liquid with n-hexane and normal
Heat up drying under the conditions of pressure.
Drying process is the same as embodiment 1.
The density of the Static Spinning polyacrylonitrile nanofiber enhancing aerosil of the preparation is 0.2 g/cm3,
Specific surface area is 750 m2/ g, average pore size are 10.4 nm, and pore volume is 1.95 cm3/g。
Claims (6)
1. a kind of preparation method of electrostatic spinning nano fiber enhancing aerosil, it is characterised in that by following steps system
It is standby：
1）The preparation and hydrolysis of silicon dioxide gel
Alkoxy silane, deionized water and absolute ethyl alcohol are mixed, pH value of solution is adjusted to 3 ~ 4 using hydrochloric acid, magnetic agitation 12 ~
24 h make silane hydrolyzate, obtain solution A；In molar ratio, alkoxy silane：Deionized water：Absolute ethyl alcohol=1：（0.2~0.6）：
（10~20）；The alkoxy silane is ethyl orthosilicate or methyl orthosilicate；
2）The dispersion of electrostatic spinning and nanofiber
It dissolves a polymer in and forms spinning solution in organic solvent, polymer nanocomposite fibre is prepared by the method for high-voltage electrostatic spinning
Dimension, the type of the polymer includes polyacrylonitrile, polyamide, polymethyl methacrylate and cellulose acetate etc.；Using step
Rapid 1）The colloidal sol of preparation is collected as receiving body and evenly dispersed nanofiber forms nanofiber dioxide composite Ludox；
3）Preparation, aging, modification and the constant pressure and dry of dioxide composite Silica hydrogel
In step 2）It is 8 ~ 8.5 to get to silica that ammonia water conditioning system pH is added in obtained dioxide composite Ludox
Wet gel is immersed in progress gel aging in ethanol solution, then the wet gel after aging is immersed in front three by wet gel
Base chlorosilane or hmds, absolute ethyl alcohol and n-hexane mixed solution in, carry out surface modification, it is modified wet solidifying
Glue carries out constant pressure and dry, obtains electrostatic spinning nano fiber enhancing aerosil block.
2. a kind of preparation method of electrostatic spinning nano fiber enhancing aerosil as described in claim 1, feature
It is in step 2）In, the technique of the electrostatic spinning is：Spinning flow velocity is 1 ~ 2 ml/h, and it is 10 ~ 15 cm to receive distance,
The spinning time is 0.5 ~ 3 h.
3. a kind of preparation method of electrostatic spinning nano fiber enhancing aerosil as described in claim 1, feature
It is in step 2）In, the mass ratio of the nanofiber and silicon dioxide gel is 1：（100~500）.
4. a kind of preparation method of electrostatic spinning nano fiber enhancing aerosil as described in claim 1, feature
It is in step 3）In, the temperature of the aging is 25 ~ 80 DEG C, and the time of aging is 12 ~ 24 h.
5. a kind of preparation method of electrostatic spinning nano fiber enhancing aerosil as described in claim 1, feature
It is in step 3）In, the composite silicon dioxide wet gel is soaked in trim,ethylchlorosilane or hmds, anhydrous second
In the mixed solution of alcohol and n-hexane, trim,ethylchlorosilane or hmds by volume：Absolute ethyl alcohol：N-hexane 1：（1
~3）：（6~12）, soaking time is 12 ~ 24 h.
6. a kind of preparation method of electrostatic spinning nano fiber enhancing aerosil as described in claim 1, feature
It is in step 3）In, the technological process of the constant pressure and dry is：Modified composite silicon dioxide wet gel is at 40 ~ 60 DEG C
1 ~ 2 h is kept the temperature, is then warming up to 110 ~ 130 DEG C of 4 ~ 6 h of heat preservation, heating rate is 1 ~ 10 DEG C/min.
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| CN114180984A (en) * | 2021-11-10 | 2022-03-15 | 安徽壹石通材料科学研究院有限公司 | Hydroxyapatite/silicon oxide composite aerogel and preparation method thereof |
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| CN114044667A (en) * | 2021-11-23 | 2022-02-15 | 广州市香港科大霍英东研究院 | Mesoporous inorganic fiber composite material and preparation method and application thereof |
| CN114436624A (en) * | 2022-01-05 | 2022-05-06 | 江苏恒科新材料有限公司 | Polyester nanofiber/silicon dioxide composite aerogel film and preparation method thereof |
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| CN114934394A (en) * | 2022-05-31 | 2022-08-23 | 广东宜纳新材料科技有限公司 | Preparation method of fiber composite gel flexible membrane |
| CN116252529A (en) * | 2022-09-08 | 2023-06-13 | 浙江美盾防护技术有限公司 | Bulletproof glass and processing method thereof |
| CN117511219A (en) * | 2024-01-05 | 2024-02-06 | 中铁建设集团有限公司 | Flexible fiber reinforced nano microporous aerogel and preparation method thereof |
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