CN106757528A - A kind of ultra-low density silicon dioxide fluffy fiber and preparation method thereof - Google Patents
A kind of ultra-low density silicon dioxide fluffy fiber and preparation method thereof Download PDFInfo
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- CN106757528A CN106757528A CN201610979677.3A CN201610979677A CN106757528A CN 106757528 A CN106757528 A CN 106757528A CN 201610979677 A CN201610979677 A CN 201610979677A CN 106757528 A CN106757528 A CN 106757528A
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- tetraethyl orthosilicate
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/10—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material by decomposition of organic substances
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
Abstract
The invention discloses a kind of ultra-low density silicon dioxide fluffy fiber and preparation method thereof.The preparation method is with tetraethyl orthosilicate as silicon source, with polyvinyl alcohol as polymer support, tetraethyl orthosilicate/poly-vinyl alcohol solution is set to possess specific character by crosslinking, collection fiber self assembly is set to stack to form three-dimensional fluff structure by common electrospinning device under room temperature environment, fiber high temperature calcification is obtained into silica fluffy fiber with Muffle furnace again.A diameter of 0.4 ~ 2 μm of obtained silica fluffy fiber, high temperature resistant, apparent density only has 0.016g/cm3, original three-dimensional fluff structure can be still kept after the water of 75 times of own wt, and reuse can be absorbed.Preparation method of the present invention is simple, economic, practical, without special material and equipment, easily low cost, popularization.
Description
Technical field
The invention belongs to inorganic oxide fibres preparing technical field, and in particular to a kind of ultra-low density silicon dioxide is fluffy
Fiber and preparation method thereof.
Background technology
Nanometer and micron-sized continuous fiber are obtained in that by electrostatic spinning, the Fiber Aspect Ratio is high, specific surface area big,
There is application potential very high in many fields.But using method of electrostatic spinning collect fiber be generally two dimensional surface film,
Fiber stack is fine and close, and making the high-specific surface area advantage of fiber cannot effectively play, so as to result in the porosity of fiber membrane, inhale
Attached property, gas permeability are relatively low, density defect higher.Therefore, the fluffy fiber with three-dimensional structure is prepared all to open all the time
Send out the important directions of high performance fibre material.
Blakeney etc. has prepared fluffy PCL three-dimensional fibers using the hemispherical collection device that internal row has fine needle
[Blakeney, B. A.; Tambralli, A.; Anderson, J. M., et al., Biomaterials. 2011,
32,1583-1590.], Jin etc. is prepared for fluffy fibre [Jin, the L. of PLA using similar collection device; Feng, Z. Q.;
Wang, T., et al., J Mater Chem B. 2014, 2, 129-136.].Bonino etc. is by PEO spinning solutions
Three wieners fibre [Bonino, C. A. has been prepared in repulsive interaction between middle addition sodium alginate particle increases fiber;
Efimenko, K.; Jeong, S. I., et al., Small. 2012, 8, 1928-1936.].These methods are
Prepared by the three-dimensional fiber based on polymeric material, and Part Methods need special external environment or the specific collection dress of needs
Put, thus it is relatively costly.In addition, polymeric material has the notable defect of poor heat resistance, typically when temperature is close to fusing point three
Dimension structure will completely lose.Therefore, resistant to elevated temperatures inorganic oxide three-dimensional fiber is developed significant.
Silicon is the element that nature is widely present, the spy such as silica has high temperature resistant, anticorrosive, biocompatibility good
Point.Silicon dioxide fibre and improved silica fiber can be used to separating, filter, oily waste treatment, carry that medicine, catalysis etc. are different to lead
Domain.But one kind can direct fabrics obtain three-dimensional in plane reception device by conventional electrostatic spinning equipment at present
The method of fluff structure silicon dioxide fibre.
The content of the invention
In view of conventional electrostatic spinning acquisition two dimensional surface pulp freeness is relatively low, and polymeric material heat resistance is poor
Problem, the invention provides a kind of succinct, silica fluffy fiber based on method of electrostatic spinning and preparation method thereof.
The preparation method is, with tetraethyl orthosilicate as silicon source, with polyvinyl alcohol as polymer support, positive silicon to be made by crosslinking
Acetoacetic ester/poly-vinyl alcohol solution possesses specific character, makes collection fine by common electrospinning device under room temperature environment
Dimension self assembly is stacked to form three-dimensional fluff structure, then fiber high temperature calcification is obtained into silica fluffy fiber with Muffle furnace.
Obtained silica fluffy fiber has a ultralow apparent density, and superelevation unit mass water absorption rate, energy
Three-dimensional fluff structure can be still kept after high temperature resistant, and multiple water suction.
A kind of preparation method of ultra-low density silicon dioxide fluffy fiber, comprises the following steps：
（1）By tetraethyl orthosilicate（TEOS）It is stirred at room temperature with deionized water after being well mixed, adds catalyst phosphoric acid
（H3PO4）Reacted, prepared tetraethyl orthosilicate precursor solution；
（2）By polyvinyl alcohol（PVA）It is dissolved in deionized water, obtains poly-vinyl alcohol solution；
（3）Poly-vinyl alcohol solution is uniformly mixed at room temperature with tetraethyl orthosilicate precursor solution, positive silicic acid second is obtained
Ester/polyvinyl alcohol precursor solution；
（4）It is aged after tetraethyl orthosilicate/polyvinyl alcohol precursor solution is stirred；
（5）Electrostatic spinning：Tetraethyl orthosilicate after ageing/polyvinyl alcohol precursor solution is loaded into needle tubing, by liquid pump come
Solution flow rate, solution is quantitatively controlled to flow into high voltage electric field by flat mouth syringe needle, the fiber stack for being formed in the electric field is in plane aluminium
On foil paper collecting board, three-dimensional fluffy tetraethyl orthosilicate/vinal is obtained；
（6）The three-dimensional fluffy tetraethyl orthosilicate/vinal collected is sintered into calcification in atmosphere by Muffle furnace, is obtained
The ultra-low density silicon dioxide fluffy fiber.
Further, step（1）In, the tetraethyl orthosilicate is 2h with the incorporation time of deionized water.
Further, step（1）In, the tetraethyl orthosilicate is 1 with deionized water molar ratio:7~12.
Further, step（1）In, the catalyst phosphoric acid is 1 with the molar ratio of tetraethyl orthosilicate:50~100.
Further, step（1）In, the reaction is carried out at room temperature, and the time is more than 10h, to ensure that TEOS's is complete
All-hydrolytic simultaneously prevents its excessive crosslinking.
Further, step（2）In, the molecular weight of the polyvinyl alcohol is 80000 g/mol ~ 130000 g/mol, is matched somebody with somebody
The poly-vinyl alcohol solution concentration put is 10% ~ 18%wt./vol..
Further, step（3）In, the tetraethyl orthosilicate precursor solution is pressed with the mixed proportion of poly-vinyl alcohol solution
Solvent volume ratio is 1：0.5 ~ 2 ratio mixing.
Further, step（4）In, the temperature of the ageing is 60 ~ 80 DEG C, to promote between silicone hydroxyl and alcoholic extract hydroxyl group
Dehydrating condensation, so that two kinds of materials form mixing cross-linked network, improves solution viscosity.
Further, step（4）In, the time of the stirring ageing is 1 ~ 5h.
Further, step（5）In, the technological parameter of the electrostatic spinning is：Voltage is 15 ~ 20 kV, and solution flow rate is
0.5 ~ 2ml/h, operating distance of the syringe needle away from collecting board is 15 ~ 20cm, and acquisition time is 30 ~ 90min.
Further, step（6）In, the technique of the sintering is：600 ~ 800 are warming up to the speed of 10 ~ 20 DEG C/min
After DEG C, 3 ~ 5h of constant temperature is finally naturally cooling to room temperature.
Ultra-low density silicon dioxide fluffy fiber obtained in the preparation method as described in any of the above-described.
A diameter of 0.4 ~ 2 μm of obtained ultra-low density silicon dioxide fluffy fiber, apparent density only has 0.016 g/
cm3, the water of 75 times of own wt, resistance to 800 can be absorbedoC high temperature, and reuse 5 times after can still keep original three-dimensional fluffy
Structure.
Traditional tetraethyl orthosilicate sol-gal process mainly regulates and controls molten by controlling the crosslinking degree of silester itself
The viscosity of glue, so as to obtain the colloidal sol of suitable electrostatic spinning.And currently invention addresses the tetraethyl orthosilicate and polyethylene after hydrolysis
Cross-linking reaction between alcohol, the spinning properties of TEOS are improved by the cross-linked network of TEOS and PVA, while acquisition can be formed
The appropriately crosslinked TEOS/PVA solution of three-dimensional fluffy fiber, the solution uses conventional electrospinning device and collection device
Self assembly is stacked and to form three-dimensional fiber under room temperature environment.
Compared with prior art, the invention has the advantages that and beneficial effect：
（1）Preparation method of the present invention is simple, economic, practical, without special material and equipment, easily low cost, popularization；
（2）Silica fluffy fiber prepared by the present invention can be resistant to 800 DEG C of high temperature, and apparent density only has 0.016 g/cm3, it is
13 times of atmospheric density, the 45% of only common cotton density；The silica fluffy fiber of preparation can absorb own wt 75
Times water, and reuse 5 times after can still keep original three-dimensional fluff structure；
（3）The present invention prepare silica fluffy fiber specific surface area it is big, corrosion-resistant, with biocompatibility, can be used to inhale
Many fields such as attached, separation, load medicine, catalysis, fluorescence, organizational project.
Brief description of the drawings
Fig. 1 is silica fluffy fiber and silicon dioxide fibre film and the apparent density of cotton prepared by the present invention
Test result is contrasted；
Fig. 2 is silica fluffy fiber and silicon dioxide fibre film and the water absorption rate test knot of cotton prepared by the present invention
Fruit contrasts；
Fig. 3 is the silica fluffy fiber electron micrograph after being sintered in embodiment 1；
Fig. 4 is the silica fluffy fiber electron micrograph after being sintered in embodiment 2；
Fig. 5 is the silica fluffy fiber electron micrograph after being sintered in embodiment 3；
Fig. 6 be embodiment 2 prepare silica fluffy fiber repeat water suction 5 times after electron micrograph；
Fig. 7 is silica fluffy fiber and cotton prepared by embodiment 2 and silicon dioxide fibre film repeats the suction of water suction 5 times
Water rate result.
Specific embodiment
With reference to specific embodiment and accompanying drawing, the present invention is further elaborated, but this patent protection domain is not limited
In following examples.
Fig. 1 is the apparent close of silica fluffy fiber and silicon dioxide fibre film prepared by the present invention and cotton
Degree test result contrast；As shown in Figure 1, the apparent density of silica fluffy fiber prepared by the present invention is 0.016g/cm3,
Far below 0.035 g/cm of cotton3With 0.028 g/cm of silicon dioxide fibre film3。
Fig. 2 is silica fluffy fiber and silicon dioxide fibre film and the water absorption rate of cotton prepared by the present invention
Test result is contrasted；As shown in Figure 2, the water absorption rate of silica fluffy fiber prepared by the present invention is 7700%, far above cotton
3800% and silicon dioxide fibre film 3250%.
Embodiment 1
（1）80mmol tetraethyl orthosilicates are blended in 10.9ml deionized waters and are stirred at room temperature, 0.8mmol phosphorus is added after 2h
Acid stirs 10 hours prepared tetraethyl orthosilicate precursor solutions at room temperature as catalyst；
（2）It is molten by 1 g molecular weight for the polyvinyl alcohol of 100000g/mol is completely dissolved in 10ml deionized waters at 90 DEG C
The solution time is 3h, and 10%wt./vol. poly-vinyl alcohol solutions are obtained, and treats that solution is cooled to room temperature；
（3）Tetraethyl orthosilicate precursor solution and poly-vinyl alcohol solution are mixed and stirred for 3 hours, tetraethyl orthosilicate presoma is molten
Liquid is 1 by solvent volume ratio with the mixed proportion of poly-vinyl alcohol solution：2, tetraethyl orthosilicate/polyvinyl alcohol presoma is obtained molten
Liquid；
（4）It is aged 5 hours after being stirred at tetraethyl orthosilicate/polyvinyl alcohol precursor solution is placed in into 60 DEG C, obtains and be adapted to electrostatic
Tetraethyl orthosilicate/the poly-vinyl alcohol solution of spinning；
（5）The tetraethyl orthosilicate of suitable electrostatic spinning/poly-vinyl alcohol solution is loaded into needle tubing, is quantitatively controlled by liquid pump molten
Flow velocity, solution flows into high voltage electric field by flat mouth syringe needle, and the fiber stack for being formed in the electric field is in plane aluminium-foil paper collecting board
On；The technological parameter selected in electrostatic spinning is：Voltage is 20kV, and solution flow rate is 2ml/h, working distance of the syringe needle away from collecting board
From being 15cm, fiber acquisition time is 90min；
（6）Tetraethyl orthosilicate/the vinal of collection is sintered into calcification so as to obtain dioxy in atmosphere by Muffle furnace
SiClx fluffy fiber；Sintering process is：800 DEG C of constant temperature is warming up to 3 hours with the speed of 10 DEG C/min, room is finally naturally cooling to
Temperature, obtains silica fluffy fiber.
Fig. 3 is the electron micrograph of obtained silica fluffy fiber, silica fluffy fiber it is average straight
Footpath is 0.4 μm.
Embodiment 2
（1）50mmol tetraethyl orthosilicates and 10.8ml deionized waters are blended in after 2h is stirred at room temperature and add 1mmol phosphoric acid
As catalyst, 10 hours prepared tetraethyl orthosilicate precursor solutions are stirred at room temperature；
（2）It is molten by 1.5g molecular weight for the polyvinyl alcohol of 80000g/mol is completely dissolved in 10ml deionized waters at 90 DEG C
The solution time is 4h, and 15%wt./vol. poly-vinyl alcohol solutions are obtained, and treats that solution is cooled to room temperature；
（3）Tetraethyl orthosilicate precursor solution and poly-vinyl alcohol solution are mixed and stirred for 3 hours, tetraethyl orthosilicate presoma is molten
Liquid is 1 by solvent volume ratio with the mixed proportion of poly-vinyl alcohol solution：1, tetraethyl orthosilicate/polyvinyl alcohol presoma is obtained molten
Liquid；
（4）It is aged 1 hour after being stirred at tetraethyl orthosilicate/polyvinyl alcohol precursor solution is placed in into 80 DEG C, obtains and be adapted to electrostatic
Tetraethyl orthosilicate/the poly-vinyl alcohol solution of spinning；
（5）The tetraethyl orthosilicate of suitable electrostatic spinning/poly-vinyl alcohol solution is loaded into needle tubing, is quantitatively controlled by liquid pump molten
Flow velocity, solution flows into high voltage electric field by flat mouth syringe needle, and the fiber stack for being formed in the electric field is in plane aluminium-foil paper collecting board
On.The technological parameter selected in electrostatic spinning is：Voltage is 18kV, and solution flow rate is 1ml/h, working distance of the syringe needle away from collecting board
From being 18cm, acquisition time is 60min；
（6）Tetraethyl orthosilicate/the vinal of collection is sintered into calcification so as to obtain dioxy in atmosphere by Muffle furnace
SiClx fluffy fiber；Sintering process is：600 DEG C of constant temperature is warming up to 5 hours with 20 DEG C/min of speed, is finally naturally cooling to
Room temperature, obtains silica fluffy fiber.
Fig. 4 is the electron micrograph of obtained silica fluffy fiber, silica fluffy fiber it is average straight
Footpath is 0.6 μm.
Embodiment 3
（1）50mmol tetraethyl orthosilicates are blended in 10.8ml deionized waters and are stirred at room temperature, 0.5mmol phosphorus is added after 2h
Acid stirs 10 hours prepared tetraethyl orthosilicate precursor solutions at room temperature as catalyst；
（2）By 1.8g molecular weight for the polyvinyl alcohol of 130000g/mol is completely dissolved in 10ml deionized waters at 90 DEG C,
Dissolution time is 5h, and 18%wt./vol. poly-vinyl alcohol solutions are obtained, and treats that solution is cooled to room temperature；
（3）Tetraethyl orthosilicate precursor solution and poly-vinyl alcohol solution are mixed and stirred for 3 hours, tetraethyl orthosilicate presoma is molten
Liquid is 1 by solvent volume ratio with the mixed proportion of poly-vinyl alcohol solution：0.5, tetraethyl orthosilicate/polyvinyl alcohol presoma is obtained molten
Liquid；
（4）It is aged 3 hours after being stirred at tetraethyl orthosilicate/polyvinyl alcohol precursor solution is placed in into 60 DEG C, obtains and be adapted to electrostatic
Tetraethyl orthosilicate/the poly-vinyl alcohol solution of spinning；
（5）The tetraethyl orthosilicate of suitable electrostatic spinning/poly-vinyl alcohol solution is loaded into needle tubing, is quantitatively controlled by liquid pump molten
Flow velocity, solution flows into high voltage electric field by flat mouth syringe needle, and the fiber stack for being formed in the electric field is in plane aluminium-foil paper collecting board
On；The technological parameter selected in electrostatic spinning is：Voltage is 15kV, and solution flow rate is 0.5ml/h, work of the syringe needle away from collecting board
Distance is 20cm, and acquisition time is 60min；
（6）Tetraethyl orthosilicate/the vinal of collection is sintered into calcification so as to obtain dioxy in atmosphere by Muffle furnace
SiClx fluffy fiber；Sintering process is：700 DEG C of constant temperature is warming up to 4 hours with 15 DEG C/min of speed, is finally naturally cooling to
Room temperature, obtains silica fluffy fiber.
Fig. 5 is the electron micrograph of obtained silica fluffy fiber, as shown in Figure 5, the fluffy fibre of silica
The average diameter of dimension is 1 μm.The three-dimensional fluff structure of the fiber sample prepared in the embodiment is optimal, therefore in photo only
Few fibers focusing is accurate, and the fiber more remote apart from focusing plane is fuzzyyer.
Embodiment 4
（1）80mmol tetraethyl orthosilicates are blended in 15ml deionized waters and are stirred at room temperature, 0.8mmol phosphoric acid is added after 2h
As catalyst, 10 hours prepared tetraethyl orthosilicate precursor solutions are stirred at room temperature；
（2）The polyvinyl alcohol that 1.8g molecular weight is 80000 g/mol is completely dissolved in 10ml deionized waters at 90 DEG C, it is molten
The solution time is 5h, and 18%wt./vol. poly-vinyl alcohol solutions are obtained, and treats that solution is cooled to room temperature；
（3）Tetraethyl orthosilicate precursor solution and poly-vinyl alcohol solution are mixed and stirred for 3 hours, tetraethyl orthosilicate presoma is molten
Liquid is 2 by solvent volume ratio with the mixed proportion of poly-vinyl alcohol solution：1, tetraethyl orthosilicate/polyvinyl alcohol presoma is obtained molten
Liquid；
（4）It is aged 3 hours after being stirred at tetraethyl orthosilicate/polyvinyl alcohol precursor solution is placed in into 60 DEG C, obtains and be adapted to electrostatic
Tetraethyl orthosilicate/the poly-vinyl alcohol solution of spinning；
（5）The tetraethyl orthosilicate of suitable electrostatic spinning/poly-vinyl alcohol solution is loaded into needle tubing, is quantitatively controlled by liquid pump molten
Flow velocity, solution flows into high voltage electric field by flat mouth syringe needle, and the fiber stack for being formed in the electric field is in plane aluminium-foil paper collecting board
On；The technological parameter selected in electrostatic spinning is：Voltage is 15kV, and solution flow rate is 2ml/h, working distance of the syringe needle away from collecting board
From being 20cm, acquisition time is 60min；
（6）Tetraethyl orthosilicate/the vinal of collection is sintered into calcification so as to obtain dioxy in atmosphere by Muffle furnace
SiClx fluffy fiber；Sintering process is：800 DEG C of constant temperature is warming up to 3 hours with 10 DEG C/min of speed, is finally naturally cooling to
Room temperature, obtains silica fluffy fiber.
Learn that the average diameter of silica fluffy fiber is 2 μm by SEM observations.
Embodiment 5
Silica fluffy fiber prepared by embodiment 2 carries out water suction experiment.
The electron micrograph of silica fluffy fiber obtained after water suction 5 times is reused as shown in fig. 6, by scheming
6 understand, reuse water suction 5 times after silica fluffy fiber still keep original three-dimensional fluff structure.
Fig. 7 show repetition and absorbs water 5 times, the water absorption rate of cotton, silicon dioxide fibre film and silica fluffy fiber
As a result, as shown in Figure 7, the water absorption rate of the silica fluffy fiber of preparation is far above cotton and silicon dioxide fibre film.
Claims (8)
1. a kind of preparation method of ultra-low density silicon dioxide fluffy fiber, it is characterised in that comprise the following steps：
（1）Tetraethyl orthosilicate is stirred with deionized water at room temperature after being well mixed, adds catalyst phosphoric acid to carry out instead
Should, prepare tetraethyl orthosilicate precursor solution；
（2）Polyvinyl alcohol is dissolved in deionized water, poly-vinyl alcohol solution is obtained；
（3）Poly-vinyl alcohol solution is uniformly mixed at room temperature with tetraethyl orthosilicate precursor solution, positive silicic acid second is obtained
Ester/polyvinyl alcohol precursor solution；
（4）It is aged after tetraethyl orthosilicate/polyvinyl alcohol precursor solution is stirred；
（5）Electrostatic spinning：Tetraethyl orthosilicate after ageing/polyvinyl alcohol precursor solution is loaded into needle tubing, by liquid pump come
Solution flow rate, solution is quantitatively controlled to flow into high voltage electric field by flat mouth syringe needle, the fiber stack for being formed in the electric field is in plane aluminium
On foil paper collecting board, three-dimensional fluffy tetraethyl orthosilicate/vinal is obtained；
（6）The three-dimensional fluffy tetraethyl orthosilicate/vinal collected is sintered into calcification in atmosphere by Muffle furnace, is obtained
The ultra-low density silicon dioxide fluffy fiber.
2. the preparation method of a kind of ultra-low density silicon dioxide fluffy fiber according to claims 1, it is characterised in that：
Step（1）In, the tetraethyl orthosilicate is 2h with the incorporation time of deionized water；The tetraethyl orthosilicate and deionized water mole
Ratio is 1:7~12；The catalyst phosphoric acid is 1 with the molar ratio of tetraethyl orthosilicate:50~100；The reaction is at room temperature
Carry out, the time is more than 10 hours.
3. the preparation method of a kind of ultra-low density silicon dioxide fluffy fiber according to claim 1, it is characterised in that：Step
Suddenly（2）In, the molecular weight of the polyvinyl alcohol is 80000g/mol ~ 130000g/mol, and the poly-vinyl alcohol solution concentration of configuration is
10%~18%wt./vol.。
4. the preparation method of a kind of ultra-low density silicon dioxide fluffy fiber according to claim 1, it is characterised in that：Step
Suddenly（3）In, the tetraethyl orthosilicate precursor solution is 1 by solvent volume ratio with the mixed proportion of poly-vinyl alcohol solution：0.5~2
Ratio mixing.
5. the preparation method of a kind of ultra-low density silicon dioxide fluffy fiber according to claim 1, it is characterised in that：Step
Suddenly（4）In, the temperature of the ageing is 60 ~ 80 DEG C, and the time is 1 ~ 5h.
6. the preparation method of a kind of ultra-low density silicon dioxide fluffy fiber according to claim 1, it is characterised in that：Step
Suddenly（5）In, the technological parameter of the electrostatic spinning is：Voltage is 15 ~ 20 kV, and solution flow rate is 0.5 ~ 2ml/h, and syringe needle is away from receipts
The operating distance for collecting plate is 15 ~ 20cm, and acquisition time is 30 ~ 90min.
7. the preparation method of a kind of ultra-low density silicon dioxide fluffy fiber according to claim 1, it is characterised in that：Step
Suddenly（6）In, the technique of the sintering is：After 600 ~ 800 DEG C being warming up to the speed of 10 ~ 20 DEG C/min, 3 ~ 5h of constant temperature, finally
It is naturally cooling to room temperature.
8. ultra-low density silicon dioxide fluffy fiber obtained in the preparation method as described in any one of claim 1 ~ 7, its feature exists
In：A diameter of 0.4 ~ 2 μm, apparent density only has 0.016 g/cm3, the water of 75 times of own wt can be absorbed, resistance to 800 DEG C are high
Temperature, and reuse 5 times after can still keep original three-dimensional fluff structure.
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| CN107354516A (en) * | 2017-06-19 | 2017-11-17 | 西安科技大学 | The method that porous silica Electrostatic spinning of fibres liquid and method of electrostatic spinning prepare porous silica silica fibre |
| CN109837610A (en) * | 2019-02-26 | 2019-06-04 | 湘潭大学 | A kind of Na2TiSiO5The electrostatic spinning preparation method of C nano fiber |
| 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 |
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| CN112626641A (en) * | 2020-12-10 | 2021-04-09 | 新疆理工学院 | Method for preparing fluffy flexible three-dimensional silicon dioxide nano-fibers in one step by template-free method |
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