CN107354516A - The method that porous silica Electrostatic spinning of fibres liquid and method of electrostatic spinning prepare porous silica silica fibre - Google Patents
The method that porous silica Electrostatic spinning of fibres liquid and method of electrostatic spinning prepare porous silica silica fibre Download PDFInfo
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- CN107354516A CN107354516A CN201710466042.8A CN201710466042A CN107354516A CN 107354516 A CN107354516 A CN 107354516A CN 201710466042 A CN201710466042 A CN 201710466042A CN 107354516 A CN107354516 A CN 107354516A
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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
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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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
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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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Nonwoven Fabrics (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention discloses a kind of method that porous silica Electrostatic spinning of fibres liquid and method of electrostatic spinning prepare porous silica silica fibre, electrostatic spinning liquid is made up of silicon dioxide gel, polyvinyl alcohol, pore creating material etc., pore creating material is Nano carbon balls, polymethyl methacrylate nano ball, polystyrene nanospheres, silica/pore creating material/polyvinyl alcohol composite fiber is prepared by electrostatic spinning, realize the oxidation Decomposition of pore creating material and polyvinyl alcohol simultaneously by high-temperature calcination, inorganic porous silicon dioxide fibre structure is prepared.The porous silica silica fibre that the present invention is prepared has high temperature resistant, corrosion resistant feature, it is rendered as flexibility, good endurance, available in multiple environment such as acid, alkali simultaneously, it can be applied to adsorption and separate, catalyst carrier, ionic adsorption, sewage disposal etc..
Description
Technical field
The invention belongs to the preparing technical field of functional fibre, is related to a kind of preparation method of inorganic porous fiber, specifically
It is related to a kind of preparation method of porous silica micro nanometer fiber.
Background technology
Electrostatic spinning technique is widely used in preparing one dimension fibre material, and the fiber of formation has that specific surface area is big, composition
The advantages that various, size adjustable, favored as bio-based bottom, electrode material, catalyst, environment filter membrane etc. by researcher.
Wherein, electrostatic spinning porous fibre is due to low-density, bigger serface, high adsorption capacity, big surface roughness etc.
Characteristic, the application field of electrospun fibers is expanded significantly, make its answering in association areas such as filtering, absorption, tissue growths
It is significantly improved with performance, the fibrous material that electrostatic spinning prepares loose structure will have vast potential for future development in future.
It is existing to prepare the method for porous fibrous material mainly by (the thermic phase point that is separated using electrostatic spinning technique
Be separated from the induction of, gas phase, non-solvent induction is separated) or post processing mode realize.Post processing mode passes through ultraviolet
Irradiation, heat treatment, washing etc. remove some compositions of fiber, form the fiber containing hole.But above method, it is on the one hand main
It is used to preparing the porous fibre that composition is high-molecular organic material, when inorganic materials prepare porous fibre, material soft in itself
Property be difficult to keep, and the fiber and size of pore structure is difficult to control thereon, on the other hand, last handling process needs more and cumbersome
Experimental procedure.
The content of the invention
Prepared it is an object of the invention to provide a kind of porous silica Electrostatic spinning of fibres liquid and method of electrostatic spinning more
The method of hole silicon dioxide fibre.
To reach above-mentioned purpose, present invention employs following technical scheme：
A kind of porous silica Electrostatic spinning of fibres liquid, the spinning solution are by silicon dioxide gel, pore creating material and matter
Polyvinyl alcohol (PVA) aqueous solution that amount fraction is 10~30% is dispersed through mixing manufactured homogeneous sol/pore creating material/polyvinyl alcohol
Be situated between steady system, the silicon dioxide gel:Pore creating material:The mass ratio of polyvinyl alcohol water solution is 1:(0.04~0.2):(0.8~
1.2), the pore creating material is the nano particle that heat decomposition temperature is less than 500 DEG C.
The pore creating material is selected from Nano carbon balls, polymethyl methacrylate (PMMA) nanosphere, polystyrene (PS) nanometer
One or two kinds of combination of the above in the organic nanometer granules such as ball.
A kind of method that method of electrostatic spinning prepares porous silica silica fibre, comprises the following steps：
Step 1: above-mentioned pore creating material is added into silicon dioxide gel, supersonic oscillations disperse 0.5~1.0h, obtain mixed
Compound, then the polyvinyl alcohol water solution that mass fraction is 10~30% is added into mixture, 2~6h is stirred, is prepared
Matter colloidal sol/pore creating material/steady system of polyvinyl alcohol Jie, as electrostatic spinning liquid, the silicon dioxide gel:Pore creating material:Polyethylene
The mass ratio of alcohol solution is 1:(0.04~0.2):(0.8~1.2)；
Step 2: the spinning solution obtains composite fibre through electrostatic spinning, made after composite fibre is dried using calcining removal
Hole agent and polyvinyl alcohol, obtain porous silica (SiO2) fiber.
The preparation method of the silicon dioxide gel, comprises the following steps：Titanium dioxide is used as using tetraethyl orthosilicate (TEOS)
Ludox presoma, using water as solvent, with H3PO4As catalyst, silica is made through hydrolytic condensation in tetraethyl orthosilicate
Colloidal sol, tetraethyl orthosilicate:Water:H3PO4Mass ratio be 1:(0.9~1.1):(0.01~0.02).
The reaction condition of the hydrolytic condensation is：By tetraethyl orthosilicate, water and H3PO4Mixing, H is controlled in mixing3PO4's
It is in being added in 30~60min to add speed, and 6~24h is then stirred at 20~30 DEG C.
The electrostatic spinning specifically includes following steps：The spinning solution is injected in the syringe of electrospinning device,
Composite fibre, syringe needle connection positive source are prepared into using electrospinning device, masking foil collects fiber as negative pole；
The distance of positive and negative interpolar is 10~15cm, and spinning voltage is 10~20kV, and syringe pump fltting speed is 200~400 μ L/min.
The drying condition of the composite fibre is：In 80~120 DEG C of 2~4h of oven drying.
The calcining specifically includes following steps：Dried composite fibre is placed in Muffle furnace, then with 5~10 DEG C/
Min programming rate is heated to 750~900 DEG C, and 2~4h of isothermal holding at such a temperature, you can it is fine to obtain porous silica
Dimension.
Beneficial effects of the present invention are embodied in：
The present invention first pass through the spinning solution containing nano particle pore creating material through electrostatic spinning prepare silica/nanosphere/
PVA composite fibres, then by high-temperature calcination, using pore creating material oxidation Decomposition under the high temperature conditions, hole is left in fibrous inside
Hole structure, a step are realized that the preparation of silicon dioxide fibre and the thermal decomposition of pore creating material and polymer (PVA) remove, are prepared more
Hole silicon dioxide fibre.By controlling silicon dioxide gel, pore creating material and the mass ratio of polyvinyl alcohol water solution, ensure the steady body that is situated between
System meets electrospun fibers synthesis and required, is uniformly distributed pore creating material, and the size of fiber central hole structure is regulated and controled difficulty reduces；
By regulating and controlling to the size of pore creating material, content in electrostatic spinning liquid, so as to adjust the size in fibrous inside aperture and
Distribution, raw material is easy to get, and method is simple and easy, available for quickly preparing porous silica silica fibre.The present invention prepare porous two
Silicon oxide fibre purity is high, and can give full play to silica has high temperature resistant, corrosion resistant feature, even if while after firing according to
Old to show flexibility, fiber size is controllable, good endurance, available in multiple environment such as acid, alkali, adsorption with separating,
There is good application prospect in the fields such as catalyst carrier, ionic adsorption, sewage disposal.
Further, by controlling H3PO4Addition speed regulation silicon dioxide gel prepare in tetraethyl orthosilicate hydrolysis
Degree, so as to by the size Control of silicon dioxide fibre in micro-nano scope.
Further, by controlling electrostatic spinning process parameter so that electrostatic spinning liquid forms answering for the film forming that is interweaved
Condensating fiber, and preferably keep the flexibility of silica.
Further, by the way that composite fibre is dried before calcination, the moisture content in fiber is removed, preferably keeps fine
The pattern of dimension.
Brief description of the drawings
Fig. 1 is the electron scanning micrograph of the porous silica silica fibre prepared in the embodiment of the present invention 1.
Fig. 2 is the infrared spectrogram of the porous silica silica fibre prepared in the embodiment of the present invention 1.
Embodiment
The present invention is described in further detail below in conjunction with drawings and examples.Embodiment is used to explain the present invention, but
It is not limited to protection scope of the present invention.
Embodiment 1
Step 1: taking 1g silicon dioxide gels to add the Nano carbon balls that 50mg average diameters are 110nm, ultrasonic wave is scattered equal
Even (0.5h), then thereto add mass fraction be 11% PVA aqueous solution 1g, be stirred until homogeneous (4h), obtain homogeneous sol/
Pore creating material/steady system of polyvinyl alcohol Jie, as electrostatic spinning liquid；
Wherein, silicon dioxide gel preparation method is：Using tetraethyl orthosilicate (TEOS) as silica precursor sol body,
Using water as solvent, H3PO4(85%) catalyst is used as, by tetraethyl orthosilicate:Water:H3PO4It is 1 in mass ratio:1:0.01 ratio
Example is mixed (wherein, H3PO4Need to drip in 30~60min), 6h is then stirred at room temperature, fills inorganic precursor
Divide hydrolysis, condensation, form silicon dioxide gel；
Wherein, the preparation of the PVA aqueous solution：PVA is added to the water, dissolves by heating and stirs, obtains the PVA aqueous solution,
It is standby.PVA alcoholysis degrees 87~89%.
Step 2: electrostatic spinning liquid is injected in the 1mL syringe with stainless steel syringe needle, control spinning speed is (i.e.
Syringe pump fltting speed) it is 200 μ L/min, regulation spinning voltage is 15kV, adjusting shower nozzle (i.e. stainless steel syringe needle) to receiver board
The distance of (being covered with masking foil) is 15cm, you can is collected on receiver board and obtains silicon/carbon dioxide nanosphere/PVA composite fibres
(fiber interweaving film forming).
Step 3: the composite fibre (film) of gained is placed in Muffle furnace after 80 DEG C of 2~4h of oven drying, in atmosphere
800 DEG C are heated to by 5 DEG C/min programming rate, and is incubated 2h at such a temperature, you can obtains porous silicon dioxide fibre (fiber
Intertexture film forming).
Referring to Fig. 1, silicon dioxide fibre manufactured in the present embodiment has a loose structure, and the diameter of fiber is distributed in 0.8~
1.2 μm, a diameter of 60~70nm in hole.Referring to Fig. 2, in the infrared spectrum of silicon dioxide fibre manufactured in the present embodiment, only exist
1078cm-1、790cm-1And 455cm-1There are obvious Si-O-Si absworption peaks, without other miscellaneous peaks.
Embodiment 2
Step 1: the silicon dioxide gel for taking 1g embodiments 1 to prepare adds the poly- methyl-prop that 75mg average diameters are 300nm
E pioic acid methyl ester nanosphere, ultrasonic wave are uniformly dispersed (0.5h), then add the PVA aqueous solution 1g that mass fraction is 11% thereto,
(4h) is stirred until homogeneous, obtains homogeneous sol/pore creating material/steady system of polyvinyl alcohol Jie, as electrostatic spinning liquid.
Step 2: the spinning speed will be controlled to be in the electrostatic spinning liquid injection 1mL syringe with stainless steel syringe needle
250 μ L/min, regulation spinning voltage are 10kV, adjusting shower nozzle (i.e. stainless steel syringe needle) to the distance of receiver board (being covered with masking foil)
For 15cm, you can collected on receiver board and obtain silica/PMMA nanospheres/PVA composite fibres (fiber interweaving film forming)
Step 3: the composite fibre (film) of gained is placed in Muffle furnace after 80 DEG C of 2~4h of oven drying, in atmosphere
850 DEG C are heated to by 10 DEG C/min programming rate, and is incubated 3h at such a temperature, you can it is (fine to obtain porous silicon dioxide fibre
Tie up intertexture film forming).
Silicon dioxide fibre manufactured in the present embodiment has loose structure, and the diameter of fiber is distributed in 0.8~1.2 μm, hole
A diameter of 100~110nm.
Embodiment 3
Step 1: 1g silicon dioxide gels are taken to add the polystyrene nanospheres that 100mg average diameters are 200nm, ultrasound
Ripple is uniformly dispersed (0.5h), then adds the PVA aqueous solution 1g that mass fraction is 11% thereto, is stirred until homogeneous (4h), obtains
Homogeneous sol/pore creating material/steady system of polyvinyl alcohol Jie, as electrostatic spinning liquid.
Step 2: the spinning speed will be controlled to be in the electrostatic spinning liquid injection 1mL syringe with stainless steel syringe needle
250 μ L/min, regulation spinning voltage are 10kV, adjusting shower nozzle (i.e. stainless steel syringe needle) to the distance of receiver board (being covered with masking foil)
For 15cm, you can collected on receiver board and obtain silica/PS nanospheres/PVA composite fibres (fiber interweaving film forming).
Step 3: the composite fibre (film) of gained is placed in Muffle furnace after 80 DEG C of 2~4h of oven drying, in atmosphere
750 DEG C are heated to by 10 DEG C/min programming rate, and is incubated 2h at such a temperature, you can it is (fine to obtain porous silicon dioxide fibre
Tie up intertexture film forming).
Silicon dioxide fibre manufactured in the present embodiment has loose structure, and the diameter of fiber is distributed in 0.8~1.2 μm, hole
A diameter of 80~90nm.
The present invention has advantages below：
1. porous silica silica fibre prepared by the present invention has high temperature resistant, corrosion resistant feature, while through electrostatic spinning
And calcining after be still rendered as flexible silicon dioxide fiber film, rollable to be folded without being broken, good endurance, available for acid,
In multiple environment such as alkali；
2. realizing the decomposition of pore creating material and the removal of polymer (PVA) simultaneously by high-temperature calcination, stayed in fibrous inside
Lower pore space structure, step is simple, and the preparation method of porous silica silica fibre is simple, can be achieved to produce in enormous quantities；
3. porous silica fiber pore size is adjustable, there is the big three-dimensional porous structure of specific surface area, can be applied to
Adsorption is with separating, catalyst carrier, ionic adsorption, sewage disposal etc..
Claims (9)
- A kind of 1. porous silica Electrostatic spinning of fibres liquid, it is characterised in that：The spinning solution is by silicon dioxide gel, pore-creating Agent and the polyvinyl alcohol water solution that mass fraction is 10~30% are dispersed through mixing manufactured homogeneous sol/pore creating material/poly- second The steady system of enol Jie, the silicon dioxide gel:Pore creating material:The mass ratio of polyvinyl alcohol water solution is 1:(0.04~0.2): (0.8~1.2), the pore creating material are the nano particle that heat decomposition temperature is less than 500 DEG C.
- A kind of 2. porous silica Electrostatic spinning of fibres liquid according to claim 1, it is characterised in that：The pore creating material choosing One or two kinds of combination of the above from Nano carbon balls, polymethyl methacrylate nano ball, polystyrene nanospheres.
- 3. a kind of method that method of electrostatic spinning prepares porous silica silica fibre, it is characterised in that：Comprise the following steps：Step 1: pore creating material is added into silicon dioxide gel, supersonic oscillations disperse 0.5~1.0h, obtain mixture, then to The polyvinyl alcohol water solution that mass fraction is 10~30% is added in mixture, stirs 2~6h, homogeneous sol/make is prepared Hole agent/steady system of polyvinyl alcohol Jie, as electrostatic spinning liquid, the silicon dioxide gel:Pore creating material:Polyvinyl alcohol water solution Mass ratio is 1:(0.04~0.2):(0.8~1.2)；The pore creating material is the nano particle that heat decomposition temperature is less than 500 DEG C；Step 2: the spinning solution obtains composite fibre through electrostatic spinning, pore creating material is removed using calcining after composite fibre is dried And polyvinyl alcohol, obtain porous silica silica fibre.
- 4. a kind of method that method of electrostatic spinning prepares porous silica silica fibre according to claim 3, it is characterised in that：Institute The preparation method of silicon dioxide gel is stated, is comprised the following steps：Using tetraethyl orthosilicate as silica precursor sol body, with water As solvent, with H3PO4As catalyst, silicon dioxide gel, tetraethyl orthosilicate is made through hydrolytic condensation in tetraethyl orthosilicate: Water:H3PO4Mass ratio be 1:(0.9~1.1):(0.01~0.02).
- 5. a kind of method that method of electrostatic spinning prepares porous silica silica fibre according to claim 4, it is characterised in that：Institute The reaction condition for stating hydrolytic condensation is：By tetraethyl orthosilicate, water and H3PO4Mixing, H is controlled in mixing3PO4Addition speed be In being added in 30~60min, 6~24h is then stirred at 20~30 DEG C.
- 6. a kind of method that method of electrostatic spinning prepares porous silica silica fibre according to claim 3, it is characterised in that：Institute State electrostatic spinning and specifically include following steps：By in the syringe of spinning solution injection electrospinning device, Static Spinning is utilized Silk equipment is prepared into composite fibre, syringe needle connection positive source, and masking foil collects fiber as negative pole；Positive and negative interpolar Distance is 10~15cm, and spinning voltage is 10~20kV, and syringe pump fltting speed is 200~400 μ L/min.
- 7. a kind of method that method of electrostatic spinning prepares porous silica silica fibre according to claim 3, it is characterised in that：Institute The drying condition for stating composite fibre is：In 80~120 DEG C of 2~4h of oven drying.
- 8. a kind of method that method of electrostatic spinning prepares porous silica silica fibre according to claim 3, it is characterised in that：Institute State calcining and specifically include following steps：Dried composite fibre is placed in Muffle furnace, then with 5~10 DEG C/min heating speed Degree is heated to 750~900 DEG C, and 2~4h of isothermal holding at such a temperature, you can obtains porous silicon dioxide fibre.
- 9. a kind of method that method of electrostatic spinning prepares porous silica silica fibre according to claim 3, it is characterised in that：Institute State a kind of either two kinds of pore creating material in Nano carbon balls, polymethyl methacrylate nano ball, polystyrene nanospheres Combination of the above.
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| CN108823790A (en) * | 2018-07-01 | 2018-11-16 | 浙江理工大学 | Centrifugal spinning porous micro nano rice tunica fibrosa and preparation method thereof |
| CN108998841A (en) * | 2017-06-07 | 2018-12-14 | 南京理工大学 | A kind of preparation method of porous polypropylene nitrile nanofibre |
| CN109825899A (en) * | 2019-03-05 | 2019-05-31 | 山东大学 | A kind of method that electrostatic spinning directly prepares mesoporous silicon Magnesium coumpoud oxide fiber |
| CN111389396A (en) * | 2020-03-10 | 2020-07-10 | 中国海洋大学 | Carbon smoke removing catalyst and preparation method and application thereof |
| 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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| CN108998841A (en) * | 2017-06-07 | 2018-12-14 | 南京理工大学 | A kind of preparation method of porous polypropylene nitrile nanofibre |
| US11652201B2 (en) | 2017-09-13 | 2023-05-16 | Unifrax I Llc | Silicon-based anode material for lithium ion battery |
| US11069885B2 (en) | 2017-09-13 | 2021-07-20 | Unifrax I Llc | Silicon-based anode material for lithium ion battery |
| CN108823790A (en) * | 2018-07-01 | 2018-11-16 | 浙江理工大学 | Centrifugal spinning porous micro nano rice tunica fibrosa and preparation method thereof |
| CN109825899A (en) * | 2019-03-05 | 2019-05-31 | 山东大学 | A kind of method that electrostatic spinning directly prepares mesoporous silicon Magnesium coumpoud oxide fiber |
| CN109825899B (en) * | 2019-03-05 | 2021-06-25 | 山东大学 | Method for directly preparing mesoporous silicon-magnesium composite oxide fiber through electrostatic spinning |
| CN111389396A (en) * | 2020-03-10 | 2020-07-10 | 中国海洋大学 | Carbon smoke removing catalyst and preparation method and application thereof |
| CN111389396B (en) * | 2020-03-10 | 2023-07-25 | 中国海洋大学 | Carbon smoke removing catalyst and preparation method and application thereof |
| 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 |
| CN112695413A (en) * | 2020-12-18 | 2021-04-23 | 广东工业大学 | MXene/porous carbon nanofiber composite material and preparation method and application thereof |
| CN113698188A (en) * | 2021-08-20 | 2021-11-26 | 南京理工大学 | Method for preparing silicon dioxide fiber with rectangular cross section by taking silica sol as raw material |
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Application publication date: 20171117 |