CN106087109A - Pore-size regulatable polysulfones polylactic acid nano porous superfine fibre - Google Patents
Pore-size regulatable polysulfones polylactic acid nano porous superfine fibre Download PDFInfo
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- CN106087109A CN106087109A CN201610647258.XA CN201610647258A CN106087109A CN 106087109 A CN106087109 A CN 106087109A CN 201610647258 A CN201610647258 A CN 201610647258A CN 106087109 A CN106087109 A CN 106087109A
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- Prior art keywords
- polysulfones
- polylactic acid
- superfine fibre
- pore
- size
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
-
- 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
- D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
- D01D5/247—Discontinuous hollow structure or microporous structure
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Nonwoven Fabrics (AREA)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention discloses a kind of regulatable polysulfones of pore-size/polylactic acid nano porous superfine fibre, by polysulfones and polylactic acid blend are dissolved in dichloromethane/dimethylformamide, or dichloromethane/dimethyl acetylamide, or the binary mixed solvent such as dichloromethane/acetone, prepare electrostatic spinning solution, then electrospinning device is used to carry out electrostatic spinning, a step can prepare surface there is the porous superfine fibre of nanometer micropore, and the present invention can be by regulation and control polysulfones and the blending ratio of polylactic acid, prepare the nanoporous ultrafine fiber with different aperture size.The polysulfones of the present invention/polylactic acid nano porous superfine fibre surface has the pore structure of prosperity, and surface pore size adjustable, fibre diameter reaches submicron order, there is high-specific surface area and surface adsorption energy, may be used for the fine dust in the Organic substance in absorption effluent, absorption air and toxic gas.
Description
Technical field
The present invention relates to a kind of surface pore size adjustable nanoporous ultrafine fiber, particularly a kind of polylactic acid/
Polysulfones is blended nanoporous ultrafine fiber.
Background technology
Use electrostatic spinning technique can prepare the fibre diameter superfine fibre at submicron order, be to prepare ultra-fine fibre at present
Dimension is the simplest, most straightforward approach.Nanoporous ultrafine fiber refers to that fiber surface has the superfine fibre of nanoaperture structure.
High molecular polymer is dissolved in the binary mixed solvent system being made up of volatile solvent and non-solvent, prepares electrostatic spinning molten
Liquid, during electrostatic spinning, owing to solvent volatilization makes polymer rich phase and solvent phase occur to be separated, thus at fiber table
Face produces loose structure.This kind of method a step can prepare nanoporous ultrafine fiber, have easy and simple to handle, that flow process is short etc. is excellent
Point.The nanoporous ultrafine fiber of preparation has high-specific surface area and surface adsorption energy, is a kind of excellent adsorbing material and load
Body material, has broad application prospects in air cleaning, sewage disposal, biological medicine, sensor and electrode material field.
That has reported at present can prepare the polymer of nanoporous ultrafine fiber less by a step method of electrostatic spinning
Number is several, such as polylactic acid, polyacrylonitrile, polystyrene and cellulose acetate etc., and prepared by the kind difference of material
The pore structure of fiber surface is the most different.
Polysulfones is widely used in Water filter material with its excellent chemical stability and heat stability, but polysulfones is difficult to
Prepare fiber surface by electrostatic spinning technique and there is the porous superfine fibre of flourishing nanoaperture structure, and polylactic acid can be adopted
Obtain surface with electrostatic spinning technique and there is the porous superfine fibre of flourishing nanoaperture structure, but its chemical stability and heat
Less stable so that it is application is restricted.
Summary of the invention
The present invention provides a kind of regulatable polysulfones of pore-size/polylactic acid nano porous superfine fibre, existing to solve
Drawbacks described above present in technology.
Polysulfones and polylactic acid blend are dissolved in dichloromethane/dimethylformamide or dichloromethane/dimethyl second by the present invention
Amide, or the binary mixed solvent such as dichloromethane/acetone, prepare electrostatic spinning solution, then use electrospinning device
Carry out electrostatic spinning, a step can prepare surface there is the porous superfine fibre of nanometer micropore, and the present invention can be by adjusting
Control polysulfones and the blending ratio of polylactic acid, prepare the nanoporous ultrafine fiber with different aperture size.This product surface
Having the pore structure of prosperity, and surface pore size adjustable, fibre diameter reaches submicron order, has high-specific surface area and table
Face energy of adsorption, may be used for the fine dust in the Organic substance in absorption effluent, absorption air and toxic gas.
Technical scheme is as follows:
A kind of regulatable polysulfones of pore-size/polylactic acid nano porous superfine fibre, described nanoporous ultrafine fiber
Surface has intensive pore structure, and the average pore size of described pore structure is 39-102nm.The shape of described pore structure is near
Like cellular.
The average diameter of described nanoporous ultrafine fiber is 530nm～1.36 μm.
The inside of described nanoporous ultrafine fiber has intensive pore structure.
The regulatable polysulfones of described pore-size/polylactic acid nano porous superfine fibre is by regulation and control polysulfones and polylactic acid
Blended part by weight regulates and controls the size of described pore structure, specifically, becomes big by controlling the weight content of polysulfones, can make
The size of described pore structure diminishes.
Described polysulfones/polylactic acid nano porous superfine fibre is prepared by the following method:
By polysulfones and polylactic acid according to the ratio of setting the most miscible in dichloromethane/dimethyl acetylamide or dichloromethane/
In dimethylformamide or dichloromethane/acetone mixed solvent, prepare electrostatic spinning solution；Wherein polysulfones and polylactic acid
The percent concentration of quality sum be the blending ratio of 6%-12%, polysulfones and polylactic acid be arbitrary proportion, described mixed solvent
The mass ratio of middle dichloromethane and dimethyl acetylamide or dichloromethane and dimethylformamide or dichloromethane and acetone
For 4.5:1～18:1.The setting ratio of described polysulfones and polylactic acid is entered according to the size of the average pore size of required pore structure
Row sets；
Electrostatic spinning solution obtained above is carried out electrostatic spinning, prepares polysulfones/polylactic acid nano porous superfine fibre.
Specifically, the step of electrostatic spinning can be: the described electrostatic spinning solution implantation glass injection that first will configure
In device, the head end of glass syringe connects No. 9 rustless steel syringe needles of internal diameter 0.6mm, then glass syringe is positioned over trace note
Penetrating pump, and place drum-type receiving screen in glass syringe front end, the distance between receiving screen and stainless pin head's end is 10
～15cm, rustless steel syringe needle connects high-voltage power cathode, and receiving screen connects high voltage power supply negative pole in succession；Regulation spinning liquid flow is
0.5～1.5ml/h, spinning voltage is 12kV～18kV, and receiving screen rotating speed is 5m/min～10m/min, and spinning environment temperature is
10～25 DEG C, relative humidity is 30%～60%.Additionally, the syringe needle that electrostatic spinning uses can also is that No. 8 or No. 12.
Compared with prior art, beneficial effects of the present invention is as follows:
First, polysulfones and polylactic acid blend, by selecting suitable dicyandiamide solution, are dissolved in dichloromethane/diformazan by the present invention
Base Methanamide, or dichloromethane/dimethyl acetylamide, or the binary mixed solvent such as dichloromethane/acetone, and select the most poly-
Compound concentration, prepares electrostatic spinning solution, then uses electrospinning device to carry out electrostatic spinning, and a step prepares surface tool
There is the porous superfine fibre of nanometer micropore；
Second, the present invention can be prepared had different aperture size by regulation and control polysulfones and the blending ratio of polylactic acid
Nanoporous ultrafine fiber；
3rd, the shape approximation of the surface void of the polysulfones of the present invention/polylactic acid nano porous superfine fibre is cellular, greatly
Improve greatly the porosity of fiber surface；
4th, the surface of the polysulfones of the present invention/polylactic acid nano porous superfine fibre has the pore structure of prosperity, and table
Face gap size adjustable, fibre diameter reaches submicron order, has high-specific surface area and surface adsorption energy, may be used for absorption dirt
Organic substance in water, the fine dust in absorption air and toxic gas；
5th, the surface of the polysulfones of the present invention/polylactic acid nano porous superfine fibre and the internal hole being respectively provided with prosperity,
Substantially increase the specific surface area of fiber, thus add its absorption to nano-particle, organic pollution and toxic gas
Performance.
Certainly, the arbitrary product implementing the present invention it is not absolutely required to reach all the above advantage simultaneously.
Accompanying drawing explanation
Fig. 1 be the polysulfones of the embodiment of the present invention 1 with polylactic acid blend than the porous fibre surface SEM photograph for 1:9；
Fig. 2 be the polysulfones of the embodiment of the present invention 2 with polylactic acid blend than the porous fibre surface SEM photograph for 5:5；
Fig. 3 be the polysulfones of the embodiment of the present invention 3 with polylactic acid blend than the porous fibre surface SEM photograph for 1:9.
Detailed description of the invention
The present invention provides a kind of regulatable polysulfones of pore-size/polylactic acid nano porous superfine fibre, described ultra-fine fibre
Dimension combines polysulfones and the advantage of polylactic acid matrix, and surface has the pore structure of prosperity, and inside also has pore structure, and table
Face gap size adjustable, has high-specific surface area and surface adsorption energy, may be used for the Organic substance in absorption effluent, absorption sky
Fine dust in gas and toxic gas.
In this article, " numerical value is to another numerical value " scope represented, is that one is avoided enumerating in the description
The summary representation of all numerical value in this scope.Therefore, the record of a certain special value scope, contain this numerical range
Interior any number and the relatively fractional value scope defined by any number in this numerical range, as the brightest
It is the same compared with fractional value scope with this that literary composition writes out this any number.
Below in conjunction with specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate this
Bright, rather than limit protection scope of the present invention.Those skilled in the art are according to changing that the present invention makes in actual applications
Enter and adjust, still falling within protection scope of the present invention.
Embodiment 1
A kind of polysulfones/polylactic acid nano porous superfine fibre that the present embodiment provides, is prepared by the following method:
The mass ratio that polysulfones mixes with polylactic acid is 1:9, and both are dissolved in the dichloromethane that mass ratio is 10:1 jointly
With the binary mixed solvent of dimethyl acetylamide, after magnetic agitation is uniform, form the spinning that mass percent is 10% molten
Liquid.Carrying out electrostatic spinning afterwards, spinning flow is 1.0ml/h, and spinning voltage is 13kV, and receiving screen rotating speed is 8m/min, spinning
Ambient temperature is 20 DEG C, and relative humidity is 40% ± 5.Fig. 1 is polysulfones/ultra-fine fibre of polylactic acid nano porous prepared by the present embodiment
The SEM photograph of dimension.It can be seen from figure 1 that the surface of polysulfones/polylactic acid blend fiber prepared of the present embodiment and inside have close
Collection, flourishing pore structure, the average pore size being computed pore structure is 102nm, and the average diameter of superfine fibre is 1.36nm.
Embodiment 2
A kind of polysulfones/polylactic acid nano porous superfine fibre that the present embodiment provides, is prepared by the following method:
The mass ratio that polysulfones mixes with polylactic acid is 5:5, and both are dissolved in the dichloromethane that mass ratio is 10:1 jointly
With the binary mixed solvent of dimethyl acetylamide, after magnetic agitation is uniform, form the spinning that mass percent is 8% molten
Liquid.Carrying out electrostatic spinning afterwards, spinning flow is 1.0ml/h, and spinning voltage is 13kV, and receiving screen rotating speed is 8m/min, spinning
Ambient temperature is 20 DEG C, and relative humidity is 40% ± 5.Fig. 2 is polysulfones/ultra-fine fibre of polylactic acid nano porous prepared by the present embodiment
The SEM photograph of dimension.It can be seen in fig. 2 that the surface of polysulfones/polylactic acid blend fiber prepared of the present embodiment and inside have close
Collection, flourishing pore structure, and average pore size is 53nm, average diameter is 656nm.
Embodiment 3
A kind of polysulfones/polylactic acid nano porous superfine fibre that the present embodiment provides, is prepared by the following method:
The mixing quality ratio of polysulfones and polylactic acid is 9:1, both be jointly dissolved in mass ratio be 10:1 dichloromethane with
In the binary mixed solvent of acetone, after magnetic agitation is uniform, form the spinning solution that mass percent is 10%.Carry out afterwards
Electrostatic spinning, spinning flow is 1.0ml/h, and spinning voltage is 13kV, and receiving screen rotating speed is 8m/min, and spinning environment temperature is 20
DEG C, relative humidity is 40% ± 5.Fig. 3 is the SEM photograph of polysulfones/polylactic acid nano porous superfine fibre prepared by the present embodiment.
As can be seen from Fig. 3, the surface of polysulfones/polylactic acid blend fiber that prepared by the present embodiment and inside have intensive, flourishing hole
Structure, and average pore size is 39nm, average diameter is 530 μm.
Embodiment 4
The mixing quality ratio of polysulfones and polylactic acid is 9:1, both be jointly dissolved in mass ratio be 18:1 dichloromethane with
In the binary mixed solvent of dimethylformamide, after magnetic agitation is uniform, form the spinning solution that mass percent is 12%.
Carrying out electrostatic spinning afterwards, spinning flow is 1.0ml/h, and spinning voltage is 12kV, and receiving screen rotating speed is 5m/min, spinning environment
Temperature is 20 DEG C, and relative humidity is 35% ± 5.Polysulfones/polylactic acid nano porous superfine fibre through prepared by the present embodiment
SEM photographic analysis is learnt, the surface of polysulfones prepared by the present embodiment/polylactic acid blend fiber has intensive, flourishing hole knot
Structure, its average pore size is 46nm, and the average diameter of superfine fibre is 657nm.
Embodiment 5
The mixing quality ratio of polysulfones and polylactic acid is 1:9, both be jointly dissolved in mass ratio be 4.5:1 dichloromethane with
In the binary mixed solvent of dimethylformamide, after magnetic agitation is uniform, form the spinning solution that mass percent is 6%.
Carrying out electrostatic spinning afterwards, spinning flow is 1.0ml/h, and spinning voltage is 14kV, and receiving screen rotating speed is 10m/min, spinning ring
Border temperature is 18 DEG C, and relative humidity is 45% ± 5.Polysulfones/polylactic acid nano porous superfine fibre through prepared by the present embodiment
SEM photographic analysis learn, the surface of polysulfones prepared by the present embodiment/polylactic acid blend fiber has intensive, flourishing hole
Structure, its average pore size is 67nm, and the average diameter of superfine fibre is 875nm.
Under the teaching of the present invention and above-described embodiment, those skilled in the art are easy to it is envisioned that cited by the present invention
Or each raw material or its equivalent alterations, each processing method or its equivalent alterations enumerated can realize the present invention and each former
Material and the parameter bound value of processing method, interval value can realize the present invention, embodiment numerous to list herein.
Claims (6)
1. the regulatable polysulfones of pore-size/polylactic acid nano porous superfine fibre, it is characterised in that described nanoporous
Superfine fibre surface has intensive pore structure, and the average pore size of described pore structure is 39-102nm.
2. the regulatable polysulfones of pore-size/polylactic acid nano porous superfine fibre as claimed in claim 1, its feature exists
In, the average diameter of described nanoporous ultrafine fiber is 530nm～1.36 μm.
3. the regulatable polysulfones of pore-size/polylactic acid nano porous superfine fibre as claimed in claim 1, its feature exists
In, the inside of described nanoporous ultrafine fiber has intensive pore structure.
4. the regulatable polysulfones of pore-size/polylactic acid nano porous superfine fibre as claimed in claim 1, its feature exists
In, described polysulfones/polylactic acid nano porous superfine fibre regulates and controls institute by the blended part by weight of regulation and control polysulfones and polylactic acid
State the size of pore structure, become big by controlling the weight content of polysulfones, it is possible to make the size of described pore structure diminish.
5. the regulatable polysulfones of pore-size/polylactic acid nano porous superfine fibre as claimed in claim 1, its feature exists
In, described polysulfones/polylactic acid nano porous superfine fibre is prepared by the following method:
Polysulfones and polylactic acid is the most miscible in dichloromethane/dimethyl acetylamide or dichloromethane/diformazan according to the ratio of setting
In base Methanamide or dichloromethane/acetone mixed solvent, prepare electrostatic spinning solution；Wherein polysulfones and the quality of polylactic acid
The percent concentration of sum be the blending ratio of 6%-12%, polysulfones and polylactic acid be arbitrary proportion, in described mixed solvent two
Chloromethanes and dimethyl acetylamide or dichloromethane and dimethylformamide or dichloromethane with the mass ratio of acetone are
4.5:1～18:1；
Electrostatic spinning solution obtained above is carried out electrostatic spinning, prepares polysulfones/polylactic acid nano porous superfine fibre.
6. the regulatable polysulfones of pore-size/polylactic acid nano porous superfine fibre as claimed in claim 5, its feature exists
In, during described electrostatic spinning, the distance between receptor and the head end of spinning head is 10～15cm, and spinning liquid flow is 0.5
～1.5ml/h, spinning voltage is 12kV～18kV, and receiving screen rotating speed is 5m/min～10m/min, spinning environment temperature be 10～
25 DEG C, relative humidity is 30%～60%；Described electrostatic spinning process uses 8 or 9 or No. 12 rustless steel syringe needles.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610647258.XA CN106087109A (en) | 2016-08-09 | 2016-08-09 | Pore-size regulatable polysulfones polylactic acid nano porous superfine fibre |
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| CN201610647258.XA CN106087109A (en) | 2016-08-09 | 2016-08-09 | Pore-size regulatable polysulfones polylactic acid nano porous superfine fibre |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107780048A (en) * | 2017-11-24 | 2018-03-09 | 吉林大学 | A kind of polylactic acid porous nano fiber electrostatic spinning preparation method of structure-controllable |
| CN114570113A (en) * | 2022-01-21 | 2022-06-03 | 中纺院（浙江）技术研究院有限公司 | Antibacterial filtering material with multi-stage gradient structure and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102517673A (en) * | 2011-11-23 | 2012-06-27 | 浙江大学 | Method for preparing polymer porous nanofiber through mixed phase separation |
| CN102747453A (en) * | 2012-07-05 | 2012-10-24 | 四川大学 | Porous superfine polymer fiber and preparation method thereof |
| CN104888629A (en) * | 2015-05-20 | 2015-09-09 | 苏州市贝克生物科技有限公司 | Polysulfone/phosphatide hemodialysis membrane and preparation method thereof |
-
2016
- 2016-08-09 CN CN201610647258.XA patent/CN106087109A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102517673A (en) * | 2011-11-23 | 2012-06-27 | 浙江大学 | Method for preparing polymer porous nanofiber through mixed phase separation |
| CN102747453A (en) * | 2012-07-05 | 2012-10-24 | 四川大学 | Porous superfine polymer fiber and preparation method thereof |
| CN104888629A (en) * | 2015-05-20 | 2015-09-09 | 苏州市贝克生物科技有限公司 | Polysulfone/phosphatide hemodialysis membrane and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107780048A (en) * | 2017-11-24 | 2018-03-09 | 吉林大学 | A kind of polylactic acid porous nano fiber electrostatic spinning preparation method of structure-controllable |
| CN114570113A (en) * | 2022-01-21 | 2022-06-03 | 中纺院（浙江）技术研究院有限公司 | Antibacterial filtering material with multi-stage gradient structure and preparation method thereof |
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Application publication date: 20161109 |