CN110433674A - PVDF/ ionic liquid/PSU efficient low-resistance filter membrane and preparation method thereof - Google Patents
PVDF/ ionic liquid/PSU efficient low-resistance filter membrane and preparation method thereof Download PDFInfo
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- CN110433674A CN110433674A CN201910666588.7A CN201910666588A CN110433674A CN 110433674 A CN110433674 A CN 110433674A CN 201910666588 A CN201910666588 A CN 201910666588A CN 110433674 A CN110433674 A CN 110433674A
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- pvdf
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- ionic liquid
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- filter membrane
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/39—Electrospinning
Abstract
The present invention provides a kind of PVDF/ ionic liquid/PSU efficient low-resistance filter membranes and preparation method thereof, preparation method is the following steps are included: step S1, PVDF solution and PSU solution is respectively configured, and ionic liquid AmimCl mixing is added in PVDF solution, obtains PVDF blend spinning liquid；Step S2 places one layer of filter cloth as backing material on receiver board, PVDF blend spinning liquid and PSU solution is injected separately into electrostatic spinning syringe needle and carry out separately or concurrently spinning, obtains PVDF/ ionic liquid/PSU efficient low-resistance filter membrane.Using technical solution of the present invention, obtained filter membrane has both electret filtering and intercepts the multi-filterings effects such as filtering, and because PSU fibre diameter is thicker, PVDF fibre diameter is thin, reduces the resistance of filtering, while also increasing filter efficiency.
Description
Technical field
The invention belongs to field of material technology more particularly to a kind of PVDF/ ionic liquid/PSU efficient low-resistance filter membrane and
Preparation method.
Background technique
In recent years, air pollution constantly aggravates the harm of human health, develops efficient low-resistance and effect is durable
Air filting material is necessary.Simultaneously with the continuous improvement of people's awareness of environment protection and health, the inhibition of microbiosis opportunistic pathogen
It is particularly important with killing.Existing high-efficiency air filtering technology mainly includes electrostatic precipitation formula filtering technique, electric field intensity
Fibrous filtration technology, stretching membrane filtration technique, fibrous filtration technology etc., wherein fibrous filtration technology is because it is with strainability
Well, the advantages that environmental suitability is strong, becomes current primary air filtering technique.Fiber-like air filting material mainly has commonly
Non-woven fibre, melt-blown electret fiber, ultra-fine fibre glass, wherein common nonwoven material diameter is thick, aperture is big, to thin
The filtering accuracy of microparticle object is difficult to ensure；It is meltblown electret fibrous material and electrostatic adsorption is generated to particle by Coulomb force,
Can promote filter efficiency while not increasing material pressure drag, but its there are electret effects easily to decay, filter efficiency stability is poor
Critical defect；The advantages of ultra-fine fibre glass material diameter is thin, compact structure, thus can bring filtration efficiency, but it is caused
Close packed structures also cause air drag larger simultaneously.
In recent years, the nano-fiber material that scientific research personnel's discovery is prepared using electrostatic spinning technique thin, aperture with diameter
Structure feature small, porosity is high, it is abundant so as to be provided while guaranteeing to fine particulates high efficiency filter for air-flow
Channel is expected to become a kind of ideal efficient low-resistance air filting material.It is deposited inside it during military service due to material
Contaminant particle can be continuously increased, and the particle meeting screening filtering material electrostatic adsorption of fiber surface cladding leads to its performance
It is greatly reduced.
So although current electrostatic spinning nano fiber membrane material can achieve higher filter efficiency, but resistance pressure
It drops still higher, it is difficult to meet currently the needs of to efficient low-resistance air filting material, it is how efficient simultaneously in holding, it is real
Existing resistance pressure drop further decreases, and is that Electrospun nano-fibers are applied to the to be solved of entire air filting material field
Problem.In addition, although the filtering to particulate matter may be implemented in electrostatic spinning nano fiber, piezoelectric property how is obtained preferably and hole
The high fiber of uniformity has a significant impact for improving strainability.
Summary of the invention
Against the above technical problems, the invention discloses a kind of PVDF/ ionic liquid/PSU efficient low-resistance filter membrane and its
Preparation method improves strainability.
In this regard, the technical solution adopted by the present invention are as follows:
A kind of preparation method of PVDF/ ionic liquid/PSU efficient low-resistance filter membrane comprising following steps:
PVDF solution and PSU solution is respectively configured in step S1, and ionic liquid AmimCl is added in PVDF solution and is mixed
It closes, obtains PVDF blend spinning liquid；
Step S2 places one layer of filter cloth as backing material on receiver board, PVDF blend spinning liquid and PSU solution is infused respectively
Enter electrostatic spinning syringe needle and carry out separately or concurrently spinning, obtains PVDF/ ionic liquid/PSU efficient low-resistance filter membrane.
PVDF itself has piezoelectric property, interception absorption can be carried out to molecule by electrostatic effect, unobvious
Filtration of material efficiency is effectively improved under the premise of increasing filtration resistance；Electrostatic spinning nano fiber non-woven material has fine pore special
Sign, and have many advantages, such as specific surface area height, fiber homogeneity is good, and the sieving effect of itself can just be such that filter efficiency reaches
90% or more.
It adopting this technical solution, the fiber thickness being prepared using electrostatic spinning process is uniform, hole even compact, than
Surface area is high；And PVDF material itself has piezoelectric property, can carry out charging electret to every fiber during the spinning process, makes
A large amount of space charges are trapped in fiber surface；Obtained filter membrane has both electret filtering and intercepts the multi-filterings such as filtering effect
Fruit.Ionic liquid is introduced to realize to the modification of PVDF fiber regularity；PSU is introduced, because the diameter of PVDF fiber and PSU fiber is not
Together, thus increased efficiency, and reduce pressure drag.
As a further improvement of the present invention, in step S2, the volume ratio of PVDF blend spinning liquid and PSU solution is 1:2
~6。
As a further improvement of the present invention, the volume ratio of PVDF blend spinning liquid and PSU solution is 1:4.
As a further improvement of the present invention, in step S2,1 syringe is drawn into PVDF blend spinning liquid, in addition takes 4
Branch syringe draws PSU solution, separately or concurrently carries out electrostatic spinning.
As a further improvement of the present invention, in step S1, in PVDF solution, the mass percent of PVDF is 10 ~ 20%.
Further, the mass percent of the PVDF is 15%.
As a further improvement of the present invention, it in step S1, prepares in PVDF blend spinning liquid, the volume point of ionic liquid
Number is the 5 ~ 15% of PVDF liquor capacity.Further, the volume of ionic liquid is the 10% of PVDF liquor capacity.
Further, in step S1, in PVDF blend spinning liquid, ionic liquid AmimCl accounts for the quality of PVDF blend spinning
Percentage is 2%.
As a further improvement of the present invention, in step S1, in PSU solution, the mass percent of PSU is 20 ~ 30%；Into
One step, the mass percent of PSU is 25%.
As a further improvement of the present invention, in step S1, the configuration method of PVDF solution are as follows: PVDF is dissolved in DMF/
It is obtained in acetone mixed solvent；DMF in DMF/ acetone mixed solvent, acetone volume ratio be 6 ~ 8:2 ~ 4；Further, DMF/
DMF in acetone mixed solvent, acetone volume ratio be 7:3.
As a further improvement of the present invention, the configuration method of PVDF blend spinning liquid are as follows:, will in 75 ~ 85 DEG C of oil baths
Ionic liquid is added in PVDF solution and is stirred, and carries out sonic oscillation, obtains uniformly mixed spinning solution.
As a further improvement of the present invention, the process conditions of electrostatic spinning are as follows: injection speed is 0.2-1.0 ml/h, electricity
Pressure is 6 ~ 12kv, 12 ~ 18cm of spinning distance.
As a further improvement of the present invention, the process conditions of electrostatic spinning are as follows: injection speed 0.8ml/h, voltage are
12kv, spinning distance 15cm.
The invention also discloses a kind of PVDF/ ionic liquid/PSU efficient low-resistance filter membranes, use any one as above
The PVDF/ ionic liquid/PSU efficient low-resistance filter membrane preparation method is prepared.
Compared with prior art, the invention has the benefit that
Using technical solution of the present invention, Static Spinning PVDF nanofiber electret can spun due to material piezoelectric property
Charging electret is carried out to every fiber during silk, a large amount of space charges is made to be trapped in fiber surface.It is real to introduce ionic liquid
Now PVDF fiber regularity is modified, size is obtained and is distributed uniform tunica fibrosa, while the ionic liquid being added can be in electric field pole
Fiber further stretch under the conditions of change and obtains polarizability and the better static spinning membrane of piezoelectric property, thus has both and stays
The multi-filterings effect such as pole filtering and interception filtering.In addition, the increasing with PSU introduces, membrane filtration efficiency increases.This is
Because PVDF fibre diameter is thin, fiber membrane aperture can be reduced；PSU fibre diameter is thicker, and the accumulation that can reduce tunica fibrosa is close
Degree extends solid particulate matter residence time in film, increases the catch rate to particle, therefore filter efficiency increases.PSU simultaneously
When fiber persistently increases, the thick proportion of fibers of diameter increases, and makes aperture increases, air-flow is easier to pass through, so that pressure drag be made to reduce.
Detailed description of the invention
Fig. 1 is the apparatus structure schematic diagram of the electrostatic spinning of an embodiment of the present invention.
Specific embodiment
Preferably embodiment of the invention is described in further detail below.
A kind of PVDF/ ionic liquid/PSU efficient low-resistance filter membrane, uses following steps to be prepared:
PVDF solution and PSU solution is respectively configured in step S1, and ionic liquid AmimCl is added in PVDF solution and is mixed
It closes, obtains PVDF blend spinning liquid, specifically:
The PVDF particle of certain mass is dissolved in the in the mixed solvent that DMF/ acetone volume ratio is 7/3, wherein the quality of PVDF
Percentage is 10 ~ 20%, it is preferred that the mass fraction of PVDF is 15%, and ionic liquid is added in 80 DEG C of oil baths and after stirring 2h
[AMIM] [Cl] (mass percent 2% that ionic liquid accounts for PVDF blend spinning liquid) to mixed liquor, is placed in sonic oscillation instrument
Processing obtains initial spinning solution until forming homogeneous and transparent solution.Wherein, the volume fraction of ionic liquid is PVDF solution body
Long-pending 5 ~ 15%.
The PSU of certain mass is dissolved in DMF solvent and is configured to that uniform solution is spare, wherein the mass fraction of PSU is
25%。
Step S2, as shown in Figure 1, above-mentioned solution is carried out electrostatic spinning:
One layer of filter cloth is placed on receiver board as backing material, and PVDF blend spinning liquid and PSU solution are injected separately into electrostatic
Spinning syringe needle, adjusting injection speed to 0.8ml/h, and voltage is debugged until 12kV, it is seen that continuous-stable jet stream is sprayed from syringe needle
It falls on receiver board, carries out layering spinning.According to spinning condition, laminated ratio is regulated and controled by the distribution spinning time.PVDF
The volume ratio of blend spinning liquid and PSU solution is 1:2 ~ 6.
Preferably, 15% PVDF solution 5mL is drawn with 1 syringe, then is inhaled respectively with 4 disposable syringes
Take 25% PSU solution 5ml spare.Spinning time total 60min, wherein the spinning time scale of PVDF and PSU be
12/48min.Finally obtain PVDF/ ionic liquid/PSU efficient low-resistance filter membrane.
Spinning first can also be carried out with PVDF solution, the spinning time is 12 minutes, then carries out spinning with PSU solution, spins
The silk time is 48 minutes.
In step S2, in spinning technology parameter, in the case that voltage is lower than 5 kV and is higher than 15 kV, can not it be formed
Taylor cone, therefore when voltage value is the regulation of the section 5kv-15kV, and fixed injection speed is 0.8ml/h it has been observed that voltage exists
Fiber discontinuously has drop appearance when 5kV, illustrates that electric field strength is too low, is not sufficiently tensile fiber；When voltage is 15kV,
The fiber of formation is excessively thick, makes fiber rougher mainly due to the excessive formation flow-disturbing of electric field strength.Voltage is controlled in 12kV, adjustment
Flow velocity is 0.2-1.0ml/h, and when can not form solid jet when flow velocity is too low, and arrive high flow rate, fiber size is inhomogenous,
Solvent is caused to have little time to volatilize this is because injection speed is too fast.So obtaining spinning process condition to the end are as follows: injection speed
For 0.8ml/h, voltage 12kv, spinning distance 15cm.
The above-mentioned filter membrane being prepared is used to be fabricated to 1170*1170 filter, rolls over a height of 75mm, tooth pitch 10cm,
30 foldings, by test, in 2000m3Initial resistance is 60Pa, filter efficiency 99.99978% under the air quantity of/h.In addition, same
Test condition, by test when PVDF/PSU spinning solution volume ratio is 1:4, same size mistake that obtained filter paper is prepared
Filter efficiency highest, resistance is minimum, respectively 60Pa and 99.99978%.When PVDF/PSU spinning solution volume ratio is 1:3 or 1:
When 5, resistance is higher than 60Pa, and efficiency is lower than 99.99978%.
When ionic liquid volume fraction is the 1/10 of PVDF solution, it is nanometer that filter membrane surface obtained, which shows diameter,
Fibrous reticular structure, and when ionic liquid volume fraction is higher, cause by force very much to spin since ionic liquid receives electric field action power
Silk liquid cannot form the taylor cone of continuous-stable, can not spin stable fiber.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, In
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention
Protection scope.
Claims (10)
1. a kind of PVDF/ ionic liquid/PSU efficient low-resistance filter membrane preparation method, it is characterised in that: it includes following step
It is rapid:
PVDF solution and PSU solution is respectively configured in step S1, and ionic liquid AmimCl mixing is added in PVDF solution, obtains
To PVDF blend spinning liquid；
Step S2 places one layer of filter cloth as backing material on receiver board, PVDF blend spinning liquid and PSU solution is infused respectively
Enter electrostatic spinning syringe needle and carry out separately or concurrently spinning, obtains PVDF/ ionic liquid/PSU efficient low-resistance filter membrane.
2. PVDF/ ionic liquid according to claim 1/PSU efficient low-resistance filter membrane preparation method, feature exist
In: in step S2, the volume ratio of PVDF blend spinning liquid and PSU solution is 1:2 ~ 6.
3. PVDF/ ionic liquid according to claim 2/PSU efficient low-resistance filter membrane preparation method, feature exist
In: the volume ratio of PVDF blend spinning liquid and PSU solution is 1:4.
4. PVDF/ ionic liquid according to claim 3/PSU efficient low-resistance filter membrane preparation method, feature exist
In: in step S2,1 syringe is drawn into PVDF blend spinning liquid, 4 syringes is in addition taken to draw PSU solution, it is respectively or same
Shi Jinhang electrostatic spinning.
5. PVDF/ ionic liquid according to claim 1/PSU efficient low-resistance filter membrane preparation method, feature exist
In: in step S1, in PVDF solution, the mass percent of PVDF is 10 ~ 20%.
6. PVDF/ ionic liquid according to claim 1/PSU efficient low-resistance filter membrane preparation method, feature exist
In: it in step S1, prepares in PVDF blend spinning liquid, the volume fraction of ionic liquid is the 5 ~ 15% of PVDF liquor capacity.
7. PVDF/ ionic liquid according to claim 1/PSU efficient low-resistance filter membrane preparation method, feature exist
In: in step S1, the configuration method of PSU solution is: PSU being dissolved in solvent DMF, the mass percent of PSU is 20 ~ 30%.
8. PVDF/ ionic liquid according to claim 1/PSU efficient low-resistance filter membrane preparation method, feature exist
In: in step S1, in PVDF solution, the mass percent of PVDF is 15%；It prepares in PVDF blend spinning liquid, ionic liquid
Volume is the 10% of PVDF liquor capacity；In PSU solution, the mass percent of PSU is 25%.
9. PVDF/ ionic liquid according to claim 1/PSU efficient low-resistance filter membrane preparation method, feature exist
In: in step S1, the configuration method of PVDF solution are as follows: PVDF is dissolved in DMF/ acetone mixed solvent and is obtained；DMF/ acetone
In the mixed solvent DMF, acetone volume ratio be 6 ~ 8:2 ~ 4；
The configuration method of PVDF blend spinning liquid are as follows: in 75 ~ 85 DEG C of oil baths, ionic liquid is added in PVDF solution and is stirred
Mixing, and sonic oscillation is carried out, obtain uniformly mixed spinning solution；
In step S2, the process conditions of electrostatic spinning are as follows: injection speed be 0.2-1.0 ml/h, voltage be 6 ~ 12kv, spinning away from
From 12 ~ 18cm.
10. a kind of PVDF/ ionic liquid/PSU efficient low-resistance filter membrane, it is characterised in that: it is used as claim 1 ~ 9 is any
PVDF/ ionic liquid described in one/PSU efficient low-resistance filter membrane preparation method is prepared.
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| CN201910666588.7A CN110433674A (en) | 2019-07-23 | 2019-07-23 | PVDF/ ionic liquid/PSU efficient low-resistance filter membrane and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112755651A (en) * | 2020-12-31 | 2021-05-07 | 东华大学 | Multi-combination functional electrostatic spinning submicron fiber air filter material and preparation thereof |
| CN113769589A (en) * | 2021-09-02 | 2021-12-10 | 重庆大学 | Preparation process of integrated synthetic filter membrane suitable for suction filtration of jatropha curcas plant insulating oil |
| CN113802266A (en) * | 2021-09-26 | 2021-12-17 | 北京石油化工学院 | Polyacrylonitrile composite nanofiber membrane, preparation method and application thereof |
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| CN103556234A (en) * | 2013-10-24 | 2014-02-05 | 杭州师范大学 | Anti-static high-beta-crystal-content polyvinylidene fluoride nanometer composite fiber film and preparation method thereof |
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2019
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103556234A (en) * | 2013-10-24 | 2014-02-05 | 杭州师范大学 | Anti-static high-beta-crystal-content polyvinylidene fluoride nanometer composite fiber film and preparation method thereof |
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| 刘学洋: "PVDF/PSU复合抗菌纳米纤维空气过滤材料的制备及其在口罩中的应用研究", 《中国优秀硕士学位论文全文数据库》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112755651A (en) * | 2020-12-31 | 2021-05-07 | 东华大学 | Multi-combination functional electrostatic spinning submicron fiber air filter material and preparation thereof |
| CN112755651B (en) * | 2020-12-31 | 2022-07-08 | 东华大学 | Multi-combination functional electrostatic spinning submicron fiber air filter material and preparation thereof |
| CN113769589A (en) * | 2021-09-02 | 2021-12-10 | 重庆大学 | Preparation process of integrated synthetic filter membrane suitable for suction filtration of jatropha curcas plant insulating oil |
| CN113802266A (en) * | 2021-09-26 | 2021-12-17 | 北京石油化工学院 | Polyacrylonitrile composite nanofiber membrane, preparation method and application thereof |
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