CN108823790A - Centrifugal spinning porous micro nano rice tunica fibrosa and preparation method thereof - Google Patents
Centrifugal spinning porous micro nano rice tunica fibrosa and preparation method thereof Download PDFInfo
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- CN108823790A CN108823790A CN201810704471.9A CN201810704471A CN108823790A CN 108823790 A CN108823790 A CN 108823790A CN 201810704471 A CN201810704471 A CN 201810704471A CN 108823790 A CN108823790 A CN 108823790A
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4282—Addition polymers
- D04H1/4318—Fluorine series
-
- 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
- D01D5/18—Formation of filaments, threads, or the like by means of rotating spinnerets
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/425—Cellulose series
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4282—Addition polymers
- D04H1/43—Acrylonitrile series
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4282—Addition polymers
- D04H1/4309—Polyvinyl alcohol
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4326—Condensation or reaction polymers
- D04H1/435—Polyesters
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/188—Monocarboxylic acids; Anhydrides, halides or salts thereof
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
- D06M2101/08—Esters or ethers of cellulose
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/22—Polymers or copolymers of halogenated mono-olefins
Abstract
The present invention relates to a kind of centrifugal spinning porous micro nano rice tunica fibrosas and preparation method thereof, belong to functional nano technical field of fiber preparation.This method comprises the following steps：（1）The preparation of centrifugal spinning solution：It is in mass ratio 8 ~ 12 by polymer, solvent, inorganic nanoparticles:80~90:0 ~ 10 mixing, obtains finely dispersed centrifugal spinning solution after stirring；（2）Centrifugal spinning：Using step（1）Centrifugal spinning solution obtained carries out centrifugal spinning, centrifugal box-spinning machine revolving speed is controlled in 8000 ~ 12000rpm/min, it is irradiated in spinning process using power >=800W light source, obtains micro/nano-fibre film, vacuum drying obtains porous micro nano rice tunica fibrosa in the environment of then placing it in 25 ~ 35 DEG C.Film produced by the present invention can be directly used for water-oil separating, and the carrier that also can be used as so-gel film or catalyst separates or carry out catalysis reaction for gas.
Description
Technical field
The present invention relates to a kind of preparation method of tunica fibrosa, in particular to a kind of centrifugal spinning porous micro nano rice tunica fibrosa
And preparation method thereof, belong to functional nano technical field of fiber preparation.
Background technique
With the development of China's economic society, the processing such as traditional water purification process such as chlorination, flocculation sedimentation, ion exchange
Method has been unable to meet Low investment, low operating cost, high water quality and reliable and stable requirement, and new technology, the exploitation of new product are aobvious
It obtains particularly important.Porous micro nano rice fiber membrane technology is with low energy consumption, device volume is small, easy to operate, yield is high, does not generate two
The features such as secondary pollution, porous micro nano rice tunica fibrosa can be used for food, medicine, biology, environmental protection, water process, electronics and bionical etc.
Field, porous micro nano rice film have become energy-saving and emission-reduction, especially water treatment field core technology of greatest concern.
The method for preparing micro/nano-fibre has very much, including melt spinning, melt-spraying spinning method, liquid spray spin processes, Static Spinning
Silk method and centrifugal spinning etc..The method using electrostatic spinning, Static Spinning are concentrated mainly on to the preparation of micro/nano-fibre at present
Silk technology relatively simple can easily prepare nanofibers, however, electrostatic spinning is in cost, scale, controllability Study side
Face is from practical and application demand there are also with a distance from very big, and there is following inherent shortcomings to limit the party for electrostatic spinning at present
Method business large-scale use：（1）It needs to apply high voltage electric field in preparation process；（2）Production efficiency is low；（3）Solution needs certain
The pollution that the solvent of ratio generates solution with certain conductivity.Therefore in terms of cost, scale, controllability Study from
There are also very big distances for practical and application demand.
Centrifugal spinning overcomes the limitation that the preparation method of electrostatic spinning micro/nano-fibre is encountered, and can be with height
Speed and low cost generate micro/nano-fibre.There is large specific surface area, hole by micro/nano-fibre film prepared by centrifugal spinning
The advantages that rate is high, aperture diameter the is small design be not required to apply high voltage electric field, can prepare the polymer not constrained by conductivity it is micro-/
Nano fibrous membrane, and its production efficiency greatly improves.Centrifugal spinning device structure is simple, mainly by motor, spinneret, collection
Stick etc. is constituted.For spinneret on motor shaft, the inside is equipped with polymer solution, has spinneret orifice on spinneret.When work, motor is logical
Electric rotary spinning head makes spinneret high speed rotation, and polymer solution is at spinneret orifice since centrifugal force effect is injected in collection stick
It moves to collect between spinneret orifice and forms orderly micro/nano-fibre on stick.Polymer solution formed at spinneret orifice it is micro-/receive
The rice main experienced three stages of fiber：1. polymer solution need to have certain viscosity, when rotation, which reaches, forms Taylor at spinneret orifice
Cone；2. polymer solution is acted on by surface tension and centrifugal force simultaneously, when centrifugal force is greater than surface tension, polymer is stretched
Form tiny micro/nano level fiber；3. fiber rotates between spinneret orifice and collection stick under the influence of centrifugal force, at this
Solvent volatilization in polymer solution in the process obtains fiber and rotates on collection stick.
Summary of the invention
The purpose of the present invention is to provide one kind can be directly used for water-oil separating, also can be used as so-gel film or catalysis
The carrier of agent separates or carries out the centrifugal spinning porous micro nano rice tunica fibrosa of catalysis reaction for gas.
The present invention provides the preparation method of centrifugal spinning porous micro nano rice tunica fibrosa described in one kind, and this method is fabricated to
This is low, manufacture craft is easy to control.
The technical solution adopted by the present invention to solve the technical problems is：
A kind of preparation method of centrifugal spinning porous micro nano rice tunica fibrosa, this method comprises the following steps：
（1）The preparation of centrifugal spinning solution：It is in mass ratio 8 ~ 12 by polymer, solvent, inorganic nanoparticles:80~90:0~10
Mixing, obtains finely dispersed centrifugal spinning solution after stirring；
（2）Centrifugal spinning：Using step（1）Centrifugal spinning solution obtained carries out centrifugal spinning, controls centrifugal box-spinning machine revolving speed
It is irradiated in 8000 ~ 12000rpm/min, spinning process using power >=800W light source, obtains micro/nano-fibre film, then
Vacuum drying obtains porous micro nano rice tunica fibrosa in the environment of placing it in 25 ~ 35 DEG C.
The principle of the present invention is:By polymer, solvent, inorganic nanoparticles mixing centrifugal spinning, quickly waved with solvent
Hair drilling or polymer are blended with polymer and polymer and inorganic particle blended drilling, obtains porous fiber film product.
It is irradiated in spinning process by high power light source, light source direct irradiation makes in irradiation process on spinning head and the fiber of ejection
Spinning environment temperature increases rapidly, accelerates the volatilization of solvent on fiber after forming fiber, is conducive to construct fiber multihole structure；
It is blended with polymer and preliminarily forms pore structure by illumination for polymer, then one of fiber is removed under the action of glacial acetic acid
To reach porous structure；Particle pore is mainly that inorganic particle does not dissolve in spin solvent, inorganic particulate during being spun to fibre
The random distribution of grain, to form cavernous structure.
The present invention spins standby composite fibre by centrifugation with polymer such as（Kynoar）As backing material, utilization is molten
Quickly volatilize drilling, polymer of agent is blended and polymer and inorganic particle blended by the porous micro-nano of centrifugal spinning with polymer
Rice tunica fibrosa.Polymer（Kynoar）It has a heat-resisting, corrosion-resistant, radiation hardness as backing material, and intensity it is high,
Good toughness.It is mainly used for carrying out catalysis reaction or the carrier as sol gel film as the carrier of catalyst for gas
Separation.
Preferably, the light source provides for news lamp, the colour temperature of news lamp is 2800k -5600k, power 1300W.
Preferably, the polymer can be the mixture of following one or more high-molecular organic materials:It is poly- inclined
Vinyl fluoride, cellulose acetate, polyethylene, polyacrylonitrile, polymethyl methacrylate, polyvinyl alcohol, poly terephthalic acid second two
Ester.
Preferably, the solvent is the mixture of following one or more solvents:Deionized water, acetone, N-N bis-
Methylformamide, N-N dimethyl acetamide, tetrahydrofuran, dimethyl sulfoxide, methylene chloride.
Preferably, the inorganic nanoparticles material is photosensitive selected from titanium dioxide, silica, silver orthophosphate, porphyrin
Agent or metal phthalocyanine.
Preferably, the centrifugal spinning device that centrifugal spinning uses includes motor, spinneret and collects stick, spinneret is installed
At the top of the shaft of motor and it is driven by a motor rotation, there is the cavity for accommodating spinning solution in spinneret, be equipped at the top of spinneret
Liquid injection port, spinneret side wall are equipped with the spinneret orifice being connected to the cavity, collect stick around the circle setting of spinneret one.
Preferably, spinning revolving speed is adjusted to 12000rpm/min, while shining by high power light source when centrifugal spinning
It penetrates, light source direct irradiation receives to obtain porous micro nano rice tunica fibrosa on spinning head and the fiber of ejection by collecting stick.According to
Spinning environment temperature is increased rapidly during penetrating, accelerates the volatilization of solvent on fiber after forming fiber, and it is fine to be conducive to construction
Tie up porous structure.
Preferably, since inorganic particle does not dissolve in spin solvent, random point of inorganic particle during being spun to fibre
Cloth receives to obtain the micro/nano-fibre film with pore structure by collecting stick.
Preferably, porous micro nano rice tunica fibrosa further constructs porous structure using glacial acetic acid dissolution few fibers.
Micro/nano-fibre membrane part can dissolve in acid, obtain porous micro nano rice tunica fibrosa by pickling.
Compared with prior art, the present invention its remarkable advantage is:Centrifugal spinning yield is high, and equipment is simple to operation, fiber
Regulation can be adjusted by controlling technological parameter；It is obtained such as revolving speed, concentration of dope, spinneret orifice diameter, collection stick distance
The diameter of required fiber and different specific surface areas, the tunica fibrosa can be directly used for water-oil separating, can also be used as catalysis
The carrier of agent is used to be catalyzed reaction or the carrier as so-gel film is separated for gas.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of centrifugal spinning device of the present invention；
Fig. 2 is the structural schematic diagram of spinneret in Fig. 1；
Label declaration：1 motor；2 spinnerets；3 collect stick；4 blades；5 fibers；6 liquid injection ports；7 spinneret orifices；8 spinning shells；9 circles
Shape sealing ring；10 annular edges；11 steps；
Fig. 3 is the spun fiber SEM of embodiment 1 figure（10000 times, 2000 times, 500 times）；
Fig. 4 is the spun fiber SEM of embodiment 2 figure（10000 times, 2000 times, 500 times）；
Fig. 5 is the spun fiber SEM of embodiment 3 figure（10000 times, 2000 times, 500 times）；
Fig. 6 is the spun fiber SEM of embodiment 4 figure（10000 times, 2000 times, 500 times）；
Fig. 7 is the spun fiber SEM of embodiment 5 figure（10000 times, 2000 times, 500 times）；
Fig. 8 is the spun fiber SEM of embodiment 6 figure（10000 times, 2000 times, 500 times）；
Fig. 9 is the spun fiber SEM of embodiment 7 figure（10000 times, 2000 times, 500 times）；
Figure 10 is illumination pore, acid processing pore, three kinds of pore method SEM figures of particle pore（10000 times, 2000 times, 500
Times）.
Specific embodiment
In the present invention, if not refering in particular to, all parts, percentage are unit of weight, used equipment and raw material etc.
It is commercially available or commonly used in the art.Method in following embodiments is unless otherwise instructed the normal of this field
Rule method.
Embodiment 1
The preparation method of centrifugal spinning porous micro nano rice tunica fibrosa, specific step is as follows：
（1）Polymer is accurately weighed with assay balance：0.54g Kynoar（PVDF）（Wherein the molal weight M of PVDF=
600000g/mol）With 0.06g cellulose acetate（CA）（Wherein molal weight M=100000g/mol of CA）, solvent：3.24g third
Ketone and 2.16g dimethyl sulfoxide（DMSO）, it being placed in 20mL sample bottle, sample bottle is sealed with raw material band, it is heated to 40-60 DEG C,
The finely dispersed centrifugal spinning solution of PVDF/CA is finally made in stirring 24 hours.
（2）Centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1 and Fig. 2, setting revolving speed is 12000rpm/min, is received
Integrate stick distance as 12cm, orifice diameter 0.4mm takes 5mL spinning solution sample in spinneret, opens motor, opens simultaneously
Open news lamp（800w, similarly hereinafter）It is radiated at spinneret and collects on stick, light source is made to cover all fibres, directly obtained by collecting stick
To porous PVDF/CA micro/nano-fibre film.
The centrifugal spinning device that centrifugal spinning uses is as depicted in figs. 1 and 2, including motor 1, spinneret 2 and collection stick 3,
Spinneret is mounted at the top of the shaft of motor and is driven by a motor rotation, has the cavity for accommodating spinning solution, spinning in spinneret
Overhead is equipped with liquid injection port 6, and spinneret side wall is equipped with the spinneret orifice 7 being connected to the cavity, collects stick and encloses around spinneret one
Setting.
Distance controlling is 0.4mm in 10cm ± 2cm, diameter the present embodiment of spinneret orifice between spinneret and collection stick,
0.3 ~ 0.6mm is adjustable in actual production.To guarantee preferably to collect tunica fibrosa, spinneret and the difference in height for collecting stick top
It is 1-2cm.It is that axis is centrosymmetric distribution that stick, which is collected, using spinneret, and the number for collecting stick is 8.
Spinneret is made of polytetrafluoroethylene (PTFE).Spinneret is made of spinning shell 8 and circular seal ring 9, and spinning shell is
The cylinder-like structure of bottom opening, the bottom end of spinning shell extend outward to form annular along 10, and step is arranged in the middle part on annular edge
11, the circular seal ring and step cooperation seal the opening of spinning shell, and the bottom of circular seal ring and annular edge
Bottom plane it is concordant.Spinneret orifice is located at position of the spinneret bottom surface at top surface general 2/3, and symmetrical in the same plane
Setting 8.A pair of of blade 4 is also set up in the horizontal direction along upper in annular, and when spinning, which forms upward air-flow, makes spun fiber
It collects and is collecting stick top half without depositing to bottom.
When centrifugal spinning, spinneret is driven by a motor rotation, and spinning solution is sprayed from the spinneret orifice of spinneret, in spinneret orifice
Move and is stretched between stick collecting, while solvent volatilizees, form micro/nano-fibre, by collection stick receive to obtain it is micro-/receive
Rice tunica fibrosa.Motor speed is generally 5000-15000 rpm/min.
Compared with electrostatic spinning, centrifugal spinning equipment is simple, at low cost, can spinning solution more higher than Static Spinning silk spinning it is dense
Degree, it is more secure when used using this centrifugal spinning device, it is high-efficient；The yield of one-jet electrostatic spinning apparatus is 1-
Two orders of magnitude at least can be improved in 100mg/h, the productivity ratio electrostatic spinning of centrifugal spinning.
Embodiment 2：
The preparation method of centrifugal spinning porous micro nano rice tunica fibrosa, specific step is as follows：
（1）The preparation method of centrifugal spinning porous micro nano rice tunica fibrosa, the specific steps are the same as those in embodiment 1, and difference is：With point
Analysis balance accurately weighs polymer：0.42g Kynoar（PVDF）（Wherein molal weight M=600000g/mol of PVDF）With
0.18g cellulose acetate（CA）（Wherein molal weight M=100000g/mol of CA）, solvent：3.24g acetone and 2.16g diformazan
Base sulfoxide（DMSO）, it is placed in 20mL sample bottle, sample bottle is sealed with raw material band, is heated to 40-60 DEG C, stirs 24 hours, most
The obtained finely dispersed centrifugal spinning solution of PVDF/CA eventually.
（2）Centrifugal spinning is carried out using Fig. 1 shown device, setting revolving speed is 12000rpm/min, collects stick distance and is
12cm, orifice diameter 0.4mm take 5mL spinning solution sample in spinneret, open motor, while opening news lamp photograph
It penetrates, directly obtains porous PVDF/CA micro/nano-fibre film by collecting stick.
Embodiment 3：
The preparation method of centrifugal spinning porous micro nano rice tunica fibrosa, specific step is as follows：
（1）The preparation method of centrifugal spinning porous micro nano rice tunica fibrosa, the specific steps are the same as those in embodiment 1, and difference is：With point
Analysis balance accurately weighs polymer：0.30g Kynoar（PVDF）（Wherein molal weight M=600000g/mol of PVDF）With
0.30g cellulose acetate（CA）（Wherein molal weight M=100000g/mol of CA）, solvent：3.24g acetone and 2.16g diformazan
Base sulfoxide（DMSO）, it is placed in 20mL sample bottle, sample bottle is sealed with raw material band, is heated to 40-60 DEG C, stirs 24 hours, most
The obtained finely dispersed centrifugal spinning solution of PVDF/CA eventually.
（2）Centrifugal spinning is carried out using Fig. 1 shown device, setting revolving speed is 12000rpm/min, collects stick distance and is
12cm, orifice diameter 0.4mm take 5mL spinning solution sample in spinneret, open motor, while opening news lamp photograph
It penetrates, directly obtains porous PVDF/CA micro/nano-fibre film by collecting stick.
Embodiment 4：
The preparation method of centrifugal spinning porous micro nano rice tunica fibrosa, specific step is as follows：
（1）The preparation method of centrifugal spinning porous micro nano rice tunica fibrosa, the specific steps are the same as those in embodiment 1, and difference is：With point
Analysis balance accurately weighs polymer：0.30g Kynoar（PVDF）（Wherein molal weight M=600000g/mol of PVDF）With
0.30g cellulose acetate（CA）（Wherein molal weight M=100000g/mol of CA）, solvent：3.24g acetone and 2.16gN-N bis-
Methylacetamide（DMAC）, it is placed in 20mL sample bottle, sample bottle is sealed with raw material band, is heated to 40-60 DEG C, stirring 24 is small
When, the finely dispersed centrifugal spinning solution of PVDF/CA is finally made.
（2）Centrifugal spinning is carried out using Fig. 1 shown device, setting revolving speed is 12000rpm/min, collects stick distance and is
12cm, orifice diameter 0.4mm take 5mL spinning solution sample in spinneret, open motor, while opening news lamp photograph
It penetrates, directly obtains porous PVDF/CA micro/nano-fibre film by collecting stick.
Embodiment 5：
The preparation method of centrifugal spinning porous micro nano rice tunica fibrosa, specific step is as follows：
（1）The preparation method of centrifugal spinning porous micro nano rice tunica fibrosa, the specific steps are the same as those in embodiment 1, and difference is：With point
Analysis balance accurately weighs polymer：0.42g Kynoar（PVDF）（Wherein molal weight M=600000g/mol of PVDF）With
0.18g cellulose acetate（CA）（Wherein molal weight M=100000g/mol of CA）, solvent：3.168g acetone and 2.112g bis-
Methyl sulfoxide（DMSO）, inorganic nanoparticles：0.12g P25 type titanium dioxide（TiO2）It is placed in 20mL sample bottle, sample bottle
It is sealed with raw material band, is heated to 40-60 DEG C, stirred 24 hours, TiO is finally made2The finely dispersed centrifugal spinning of/PVDF/CA
Solution.
（2）Centrifugal spinning is carried out using Fig. 1 shown device, setting revolving speed is 12000rpm/min, collects stick distance and is
12cm, orifice diameter 0.4mm take 5mL spinning solution sample in spinneret, open motor, while opening news lamp photograph
It penetrates, directly obtains porous TiO by collecting stick2/ PVDF/CA micro/nano-fibre film.
Embodiment 6：
The preparation method of centrifugal spinning porous micro nano rice tunica fibrosa, specific step is as follows：
（1）The preparation method of centrifugal spinning porous micro nano rice tunica fibrosa, the specific steps are the same as those in embodiment 1, and difference is：With point
Analysis balance accurately weighs polymer：0.42g Kynoar（PVDF）（Wherein molal weight M=600000g/mol of PVDF）With
0.18g cellulose acetate（CA）（Wherein molal weight M=100000g/mol of CA）, solvent：3.168g acetone and 2.112g bis-
Methyl sulfoxide（DMSO）, inorganic nanoparticles：0.12g anatase titanium dioxide（TiO2）It is placed in 20mL sample bottle, sample
Bottle is sealed with raw material band, is heated to 40-60 DEG C, stirs 24 hours, TiO is finally made2The finely dispersed centrifugation of/PVDF/CA is spun
Silk solution.
（2）Centrifugal spinning is carried out using Fig. 1 shown device, setting revolving speed is 12000rpm/min, collects stick distance and is
12cm, orifice diameter 0.4mm take 5mL spinning solution sample in spinneret, open motor, while opening news lamp photograph
It penetrates, directly obtains porous TiO by collecting stick2/ PVDF/CA micro/nano-fibre film.
Embodiment 7：
The preparation method of centrifugal spinning porous micro nano rice tunica fibrosa, specific step is as follows：
（1）The preparation method of centrifugal spinning porous micro nano rice tunica fibrosa, the specific steps are the same as those in embodiment 1, and difference is：With point
Analysis balance accurately weighs polymer：0.42g Kynoar（PVDF）（Wherein molal weight M=600000g/mol of PVDF）With
0.18g cellulose acetate（CA）（Wherein molal weight M=100000g/mol of CA）, solvent：3.24g acetone and 2.16g diformazan
Base sulfoxide（DMSO）, inorganic nanoparticles：0.12g anatase titanium dioxide（TiO2）It is placed in 20mL sample bottle, sample bottle
It is sealed with raw material band, is heated to 40-60 DEG C, stirred 24 hours, finally the obtained finely dispersed centrifugal spinning solution of PVDF/CA.
（2）Centrifugal spinning is carried out using Fig. 1 shown device, setting revolving speed is 12000rpm/min, collects stick distance and is
12cm, orifice diameter 0.4mm take 5mL spinning solution sample in spinneret, open motor, are obtained by collecting stick
PVDF/CA micro/nano-fibre film is placed on glacial acetic acid by PVDF/CA micro/nano-fibre film（Three hawk chemical reagent of Hangzhou is limited
Company）Middle processing dissolves few fibers in two hours, obtains porous micro nano rice fiber.
It is taken small respectively after the micro/nano-fibre film vacuum drying prepared in embodiment 1,2,3,4,5,6,7 for verification the verifying results
Block sample field emission scanning electron microscope（SEM）Test fiber surface morphology, scanning electron microscope（SEM）As a result see Fig. 3,4,5,6,7,8,
9.Embodiment 1.2.3.4 is illumination pore respectively, and it is particle pore that embodiment, which is 5,6, and embodiment 7 is acid processing pore.Finally
In conjunction with illumination pore, acid processing pore, the sectional view of particle pore（Figure 10）, three kinds of equal effects of pore method are bright as the result is shown
It is aobvious.
The embodiment of the present invention is only used for that the present invention is further illustrated, not exhaustive, does not constitute to claim
The restriction of protection scope, there are also other variations and modifications are equal on the premise of not exceeding the technical scheme recorded in the claims
In the scope of the present invention.
Claims (10)
1. a kind of preparation method of centrifugal spinning porous micro nano rice tunica fibrosa, it is characterised in that this method comprises the following steps：
（1）The preparation of centrifugal spinning solution：It is in mass ratio 8 ~ 12 by polymer, solvent, inorganic nanoparticles:80~90:0~10
Mixing, obtains finely dispersed centrifugal spinning solution after stirring；
（2）Centrifugal spinning：Using step（1）Centrifugal spinning solution obtained carries out centrifugal spinning, controls centrifugal box-spinning machine revolving speed
It is irradiated in 8000 ~ 12000rpm/min, spinning process using power >=800W light source, obtains micro/nano-fibre film, then
Vacuum drying obtains porous micro nano rice tunica fibrosa in the environment of placing it in 25 ~ 35 DEG C.
2. the preparation method of centrifugal spinning porous micro nano rice tunica fibrosa according to claim 1, which is characterized in that described
Light source provides for news lamp, and the colour temperature of news lamp is 2800k -5600k, power 1300W.
3. the preparation method of centrifugal spinning porous micro nano rice tunica fibrosa according to claim 1, which is characterized in that described
Polymer can be following one or more high-molecular organic materials mixture:Kynoar, cellulose acetate, poly- second
Alkene, polyacrylonitrile, polymethyl methacrylate, polyvinyl alcohol, polyethylene terephthalate.
4. the preparation method of centrifugal spinning porous micro nano rice tunica fibrosa according to claim 1, which is characterized in that described
Solvent be following one or more solvents mixture:Deionized water, acetone, N-N dimethylformamide, N-N dimethyl
Acetamide, tetrahydrofuran, dimethyl sulfoxide, methylene chloride.
5. the preparation method of centrifugal spinning porous micro nano rice tunica fibrosa according to claim 1, which is characterized in that described
Inorganic nanoparticles material be selected from titanium dioxide, silica, silver orthophosphate, porphyrin photosensitizer or metal phthalocyanine.
6. the preparation method of centrifugal spinning porous micro nano rice tunica fibrosa according to claim 1, which is characterized in that centrifugation
The centrifugal spinning device that spinning uses includes motor, spinneret and collects stick, spinneret be mounted at the top of the shaft of motor and by
Motor drives rotation, has the cavity for accommodating spinning solution in spinneret, is equipped with liquid injection port at the top of spinneret, spinneret side wall is equipped with
The spinneret orifice being connected to the cavity collects stick around the circle setting of spinneret one.
7. the preparation method of centrifugal spinning porous micro nano rice tunica fibrosa according to claim 1, it is characterised in that：Centrifugation
When spinning, spinning revolving speed is adjusted to 12000rpm/min, while irradiating by high power light source, light source direct irradiation is in spinning head
And on the fiber sprayed, receive to obtain porous micro nano rice tunica fibrosa by collecting stick.
8. the preparation method of centrifugal spinning porous micro nano rice tunica fibrosa according to claim 7, it is characterised in that：Due to
Inorganic particle does not dissolve in spin solvent, and the random distribution of inorganic particle during being spun to fibre receives to obtain by collecting stick
Micro/nano-fibre film with pore structure.
9. the preparation method of centrifugal spinning porous micro nano rice tunica fibrosa according to claim 1, it is characterised in that：It is porous
Micro/nano-fibre film further constructs porous structure using glacial acetic acid dissolution few fibers.
10. fiber made of a kind of preparation method of centrifugal spinning porous micro nano rice tunica fibrosa according to claim 1
Film.
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