CN105013331B - Method for preparing PDMS/PVDF blend pervaporation membrane by using membrane casting solution - Google Patents
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Abstract
The invention discloses a method for preparing a PDMS/PVDF blend pervaporation membrane using a membrane casting solution, and relates to the technical field of membrane preparation. The membrane casting solution comprises polyvinylidene fluoride, N,N-dimethylacetamide, polydimethylsiloxane and tetrahydrofuran. According to the invention, polyvinylidene fluoride (PVDF) is adopted as a pore-forming membrane material, and polydimethylsiloxane (PDMS) is introduced for blending, such that the asymmetric PDMS/PVDF blend pervaporation membrane is prepared. According to the invention, the problems of low flux and poor strength of existing PDMS homogeneous symmetric membranes used in pervaporation are solved from the fundamental aspect, i.e., the membrane materials. The two hydrophobic membrane materials PVDF and PDMS are used for preparing the novel asymmetric PDMS/PVDF blend pervaporation membrane, such that the above properties of the PDMS pervaporation membrane can be improved.
Description
Technical field
The present invention relates to the preparing technical field of film, and in particular to a kind of to ooze using casting solution preparation PDMS/PVDF blendings
The method for vaporizing thoroughly film.
Background technology
Membrane separation technique possesses following plurality of advantages, such as：Relative to conventional separation techniques, the low, cost that consumes energy is few, efficient,
Environmental protection, can reclaim that content in feed liquid is low, costly material simultaneously, also can simultaneously with distillation, crystallization, extraction, absorb etc. and to separate
PROCESS COUPLING.In recent years, it has been widely used in commercial production and daily life, people are for the research of membrane separation technique
Increasingly pay attention to.
Polydimethylsiloxane (PDMS) is a kind of chemically stable the macromolecule organic silicon compound, and it has heat-resisting cold-resistant
Property, strong-hydrophobicity energy, good mobility and vibratility, solvent resistance energy, high-low temperature resistant, resistance to ozone, hydrophobic etc. are many excellent
Performance.Meanwhile, the low cost of PDMS is nontoxic, not volatile, therefore PDMS is widely used in preparing the homogenizing of preferential Organic substance thoroughly
Symmetrical infiltrating and vaporizing membrane.
But PDMS membrane fluxs are not big enough, and intensity is poor.Not enough for these of PDMS films, people are generally to be changed by film
Property improving the performance of film, the method such as such as, surface is modified, blending, post processing is being modified to film.
Polyvinylidene fluoride (PVDF) is a kind of novel fluoro-carbon thermoplastic, as membrane material because of its excellent performance
It is of considerable interest, there is high mechanical strength relative to other business-like polymeric materials, heat stability, chemical resistance,
The features such as high with hydrophobicity.Therefore, PVDF is widely used in membrance separation field.Asymmetric oozing can be prepared using immersion precipitation
Vaporize thoroughly film.
The content of the invention
(1) technical problem for solving
For the deficiencies in the prior art, the present invention provides a kind of using casting solution preparation PDMS/PVDF blending infiltration evaporations
The method of film, the present invention are, with polyvinylidene fluoride (PVDF) as pore membrane material, to introduce polydimethylsiloxane (PDMS) and enter
Row blending, prepares asymmetric PDMS/PVDF and infiltrating and vaporizing membrane is blended, not big enough to improve PDMS membrane fluxs, the problems such as intensity difference.
(2) technical scheme
To realize object above, the present invention is achieved by the following technical programs：
The method that PDMS/PVDF is blended infiltrating and vaporizing membrane is prepared using casting solution, is comprised the following steps：
S1, the casting solution of mix homogeneously is stood into 24 hours fully to deviate from bubble in system first, using ultrasonic deaeration
Or vacuum defoamation 1～2 hour, the casting solution is made up of the raw material of following weight portion：Polyvinylidene fluoride 10～18, N, N- bis-
The mass ratio of methylacetamide 50～60, polydimethylsiloxane and tetrahydrofuran is 1:10；
S2, by the casting solution for preparing with scraper uniformly blade coating on clean smooth glass plate, in air evaporation,
Evaporation time be 10～70min, then glass plate is put in coagulation bath, film solidification depart from glass plate after, taking-up be placed in from
Soak 72 hours in sub- water, residual solvent in completely out film, finally take out to be placed in dust free room and dry.
Preferably, air evaporation time described in step S2 is respectively 10,30,50,70min.
Preferably, the preparation method of the casting solution is comprised the following steps, and is comprised the following steps：
S1, by polyvinylidene fluoride and N,N-dimethylacetamide in 80 DEG C of water-baths, it is under conditions of mechanical agitation, fully molten
Solution, takes out the casting solution, seals, is placed in ripening 20-30 hours in 80 DEG C of baking oven；
S2, polydimethylsiloxane is dissolved in tetrahydrofuran, is stirred 1～2 hour at 25 DEG C, mix the two equal
It is even；
S3, step S1 solution is taken out from baking oven, be cooled to room temperature, add step S2 solution, under room temperature, stir 3-5
Hour, each component mix homogeneously is made, casting solution is obtained final product.
Preferably, the curing time described in step S1 is 24 hours.
Preferably, it is characterised in that mixing time described in step S3 is 4 hours.
(3) beneficial effect
The invention provides a kind of application casting solution prepare PDMS/PVDF be blended infiltrating and vaporizing membrane method, the present invention with
Polyvinylidene fluoride (PVDF) is pore membrane material, introduces polydimethylsiloxane (PDMS) and is blended, prepares asymmetric
PDMS/PVDF is blended infiltrating and vaporizing membrane, and not big enough for the existing PDMS membrane fluxs for infiltration evaporation, intensity difference etc. is asked
Topic, from membrane material, this is fundamentally started with, and using two kinds of hydrophobic membrane materials of PVDF, PDMS, prepares a kind of new asymmetric
PDMS/PVDF is blended infiltrating and vaporizing membrane, to improve the performances such as PDMS infiltration evaporation homogenizing symmetric membrane mechanical strengths, flux.
Specific embodiment
To make purpose, technical scheme and the advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, rather than the embodiment of whole.Based on the embodiment in the present invention, those of ordinary skill in the art are not making
The every other embodiment obtained under the premise of creative work, belongs to the scope of protection of the invention.
Casting solution of the present invention is made up of the raw material of following weight portion：
Polyvinylidene fluoride 10～18
DMAC N,N' dimethyl acetamide 50～60
The mass ratio of polydimethylsiloxane and tetrahydrofuran is 1:10
PDMS/PVDF of the present invention is blended the preparation process of infiltrating and vaporizing membrane casting solution：
S1, by polyvinylidene fluoride and N,N-dimethylacetamide in 80 DEG C of water-baths, it is under conditions of mechanical agitation, fully molten
Solution, takes out the casting solution, seals, is placed in ripening 24 hours in 80 DEG C of baking oven；
S2, polydimethylsiloxane is dissolved in tetrahydrofuran, is stirred 1～2 hour at 25 DEG C, mix the two equal
It is even；
S3, step S1 solution is taken out from baking oven, be cooled to room temperature, add step S2 solution, under room temperature, stirring 4 is little
When, each component mix homogeneously is made, casting solution is obtained final product.
The casting solution of above-mentioned acquisition is prepared into the method that PDMS/PVDF is blended infiltrating and vaporizing membrane, first by mix homogeneously
Casting solution stands 24 hours fully to deviate from bubble in system, using ultrasonic deaeration or vacuum defoamation 1～2 hour；To prepare
Casting solution uniformly scratched on clean, smooth glass plate with scraper, in air evaporation, then glass plate is put into solidifying
In glue bath, after film solidification departs from glass plate, taking-up is placed in deionized water soaks 72 hours, residual solvent in completely out film,
Finally take out to be placed in dust free room and dry.
Embodiment 1：
1st, 10.00g PVDF are weighed, in 80 DEG C of water-baths, under conditions of mechanical agitation, 50.00g DMAc solvents is dissolved in
In.80 DEG C of water-baths and mechanical agitation are kept, until polymer is completely dissolved, the casting solution is taken out, is sealed, is placed in 80 DEG C of baking oven
Middle ripening 24 hours.
Weigh 2.00PDMS to be dissolved in 20.00g THF, magnetic agitation 1 hour at 25 DEG C makes the two mix homogeneously.
The PVDF casting solutions of ripening are taken out from baking oven, room temperature is cooled to, 22.00g PDMS/THF solution, room is added
Under temperature, mechanical agitation 4 hours makes each component mix homogeneously.
2nd, the casting solution of mix homogeneously is stood into 24 hours with the bubble in fully abjection system, it may be necessary to using super
Sound deaeration or vacuum defoamation.
3rd, the casting solution for preparing uniformly is scratched on bright and clean smooth glass plate with scraper, is steamed in air respectively
10 are sent out, after 30,50,70min, glass plate is put in coagulation bath, the coagulation bath is dual coagulation bath, first in 30%DMAc, 5%
15min is soaked in THF and 65% deionized water solution, then 30min is soaked in deionized water, after film solidification departs from glass plate, take
Go out to be placed in deionized water and soak 72 hours, with the solvent that remains in completely out film and additive, period every 24 hours more
Change a water.Afterwards, take the film out be placed in dust free room dry it is standby.
Method of testing used in following embodiments is mainly：
First, the ethanol infiltration flux test of film, before test, film is put in test device and is fixed, then at 60 DEG C
After circulating 1 hour in the ethanol water of 15wt%, per-meate side keeps vacuum 90KPa, starts test, and parallel assay 3 times takes
Meansigma methodss.
2nd, the measuring mechanical property of film：The mechanical strength of film is surveyed with material tensile tester (3365, Instron, the U.S.)
Examination.Loading speed is 20mm/min.
Contrast test：
Take the film that thickness of the present invention is 130 microns to be contrasted with existing PDMS films.
The present embodiment adopts coagulation bath for 30%DMAc, 5%THF and 65% deionized water, according to not under the coagulation bath
The asymmetric PDMS/PVDF blending infiltration evaporation film properties obtained with the air evaporation time and PDMS homogeneity permeation vaporisation film performances
It is listed in Table 1 below.
1 different air evaporation times of table asymmetric PDMS/PVDF blend film and PDMS homogeneous membrane performance comparisons
The second that infiltrating and vaporizing membrane is blended by PDMS/PVDF prepared by the present embodiment method is can be seen that by the data in table 1
Alcohol permeation flux, mechanical strength increasing than PDMS homogeneity permeation vaporisation film, especially in terms of ethanol infiltration flux
On improvement it is the most obvious.As can be seen from Table 1, under the conditions of coagulation bath is 30%DMAc, 5%THF, 65% deionized water
Evaporation time is that the structure of film prepared by 50min and 70min is more uniform, and finger-like pore structure is more and uniform, effectively can increase
Plus ethanol infiltration flux, mechanical strength enhancing.
Embodiment 2：
1st, 10.00g PVDF are weighed, in 80 DEG C of water-baths, under conditions of mechanical agitation, 50.00g DMAc solvents is dissolved in
In.80 DEG C of water-baths and mechanical agitation are kept, until polymer is completely dissolved, the casting solution is taken out, is sealed, is placed in 80 DEG C of baking oven
Middle ripening 24 hours.
Weigh 2.00PDMS to be dissolved in 20.00g THF, magnetic agitation 1 hour at 25 DEG C makes the two mix homogeneously.
The PVDF casting solutions of ripening are taken out from baking oven, room temperature is cooled to, 22.00g PDMS/THF solution, room is added
Under temperature, mechanical agitation 4 hours makes each component mix homogeneously.
2nd, the casting solution of mix homogeneously is stood into 24 hours with the bubble in fully abjection system, it may be necessary to using super
Sound deaeration or vacuum defoamation.
3rd, the casting solution for preparing uniformly is scratched on bright and clean smooth glass plate, in air evaporation with scraper
After 10,30,50,70min, glass plate is put in coagulation bath, the coagulation bath is dual coagulation bath, first in 35%DMAc and 65%
Soak 15min in deionized water solution, then soak 30min in deionized water, after film solidification departs from glass plate, taking-up be placed in from
Soak 72 hours in sub- water, with the solvent that remains in completely out film and additive, period changed a water every 24 hours.It
Afterwards, take the film out be placed in dust free room dry it is standby.
The present embodiment adopts coagulation bath for 35%DMAc, 65% deionized water, is steamed according to different air under the coagulation bath
The asymmetric PDMS/PVDF blending infiltration evaporation film properties and PDMS homogeneity permeation vaporisation film performances that the time of sending out obtains are listed in table 2
In.
2 different air evaporation times of table asymmetric PDMS/PVDF blend film and PDMS homogeneous membrane performance comparisons
The second that infiltrating and vaporizing membrane is blended by PDMS/PVDF prepared by the present embodiment method is can be seen that by the data in table 2
Alcohol permeation flux, mechanical strength increasing than PDMS homogeneity permeation vaporisation film, wherein ethanol infiltration flux have very big
Improve.Found out by table 2, be 35%DMAc in coagulation bath, the second of film prepared by evaporation time 70min under the conditions of 65% deionized water
It is larger that alcohol flux compares other.
Embodiment 3：
1st, 10.00g PVDF are weighed, in 80 DEG C of water-baths, under conditions of mechanical agitation, 50.00g DMAc solvents is dissolved in
In.80 DEG C of water-baths and mechanical agitation are kept, until polymer is completely dissolved, the casting solution is taken out, is sealed, is placed in 80 DEG C of baking oven
Middle ripening 24 hours.Weigh 2.00PDMS to be dissolved in 20.00g THF, magnetic agitation 1 hour at 25 DEG C, mix the two equal
It is even.The PVDF casting solutions of ripening are taken out from baking oven, room temperature is cooled to, 22.00g PDMS/THF solution is added, under room temperature,
Mechanical agitation 4 hours, makes each component mix homogeneously.
2nd, the casting solution of mix homogeneously is stood into 24 hours with the bubble in fully abjection system, it may be necessary to using super
Sound deaeration or vacuum defoamation.
3rd, the casting solution for preparing uniformly is scratched on bright and clean smooth glass plate, in air evaporation with scraper
After 10,30,50,70min, glass plate is put in coagulation bath, the coagulation bath is deionized water, is soaked in deionized water
30min, after film solidification departs from glass plate, taking-up is placed in deionized water soaks 72 hours, molten with what is remained in completely out film
Agent and additive, period changed a water every 24 hours.Afterwards, take the film out be placed in dust free room dry it is standby.
The present embodiment adopts coagulation bath for deionized water, according to the non-of acquisition of different air evaporation times under the coagulation bath
Symmetrical PDMS/PVDF blending infiltration evaporation film properties and PDMS homogeneity permeation vaporisation film performances are listed in Table 3 below.
The second that infiltrating and vaporizing membrane is blended by PDMS/PVDF prepared by the present embodiment method is can be seen that by the data in table 3
Alcohol permeation flux, mechanical strength increasing than pvdf membrane, wherein ethanol infiltration flux also become strong.As shown in Table 3, solidifying
It is larger that the ethanol flux of the film that glue bath is prepared for evaporation time 10min under the conditions of deionized water compares other.
3 different air evaporation times of table asymmetric PDMS/PVDF blend film and PDMS homogeneous membrane performance comparisons
Found by above-mentioned experiment, during PDMS/PVDF blending infiltrating and vaporizing membranes are prepared, the air evaporation time is
The infiltration evaporation performance relative efficacy of the asymmetric PDMS/PVDF blendings infiltrating and vaporizing membrane of 50min and 70min is preferable, Er Qie
The air evaporation time is that the structure of film prepared by 50min and 70min is more uniform, is suitable for the requirement of infiltration evaporation.
To sum up, beneficial effects of the present invention are as follows：The present invention provides one kind and oozes using casting solution preparation PDMS/PVDF blendings
The method for vaporizing thoroughly film, with polyvinylidene fluoride (PVDF) as pore membrane material, introducing polydimethylsiloxane (PDMS) is carried out
Blending, prepares asymmetric PDMS/PVDF blendings infiltrating and vaporizing membrane, inadequate for the existing PDMS membrane fluxs for infiltration evaporation
Greatly, the problems such as intensity difference, from membrane material, this is fundamentally started with, and using two kinds of hydrophobic membrane materials of PVDF, PDMS, prepares a kind of
New asymmetric PDMS/PVDF blendings infiltrating and vaporizing membrane, to improve mechanical strength, the second of the symmetrical infiltrating and vaporizing membrane of PDMS homogenizing
The performances such as alcohol permeation flux；Solvent of the present invention is DMAc, additive-free；The asymmetric PDMS/PVDF of the present invention is blended infiltration evaporation
Film compact film thickness is 2 μm -4 μm, and porosity is more than 60%；The asymmetric PDMS/PVDF of the present invention is blended infiltrating and vaporizing membrane master
It is used for preferential Organic substance infiltration evaporation (PV) thoroughly.Infiltration evaporation test result indicate that, at room temperature evaporation time be 70min,
Coagulation bath consists of 35wt%DMAc, and membrane separating property prepared by 5wt%THF and 60wt% deionized waters system is optimal.
It should be noted that herein, such as first and second or the like relational terms are used merely to a reality
Body or operation are made a distinction with another entity or operation, and are not necessarily required or implied these entities or deposit between operating
In any this actual relation or order.And, term " including ", "comprising" or its any other variant are intended to
Nonexcludability is included, so that a series of process, method, article or equipment including key elements not only will including those
Element, but also including other key elements being not expressly set out, or also include for this process, method, article or equipment
Intrinsic key element.In the absence of more restrictions, the key element for being limited by sentence "including a ...", it is not excluded that
Also there is other identical element in process, method, article or equipment including the key element.
Above example only to illustrate technical scheme, rather than a limitation, although with reference to the foregoing embodiments
The present invention has been described in detail, it will be understood by those within the art that：Which still can be to aforementioned each enforcement
Technical scheme described in example is modified, or carries out equivalent to which part technical characteristic；And these modification or
Replace, do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (5)
1. the method that PDMS/PVDF is blended infiltrating and vaporizing membrane is prepared using casting solution, it is characterised in that comprise the following steps：
S1, the casting solution of mix homogeneously is stood into 24 hours fully to deviate from bubble in system first, using ultrasonic deaeration or true
Empty deaeration 1～2 hour, the casting solution is made up of the raw material of following weight portion：Polyvinylidene fluoride 10～18, N, N- dimethyl
The mass ratio of acetamide 50～60, polydimethylsiloxane and tetrahydrofuran is 1:10；
S2, by the casting solution for preparing with scraper uniformly blade coating on clean smooth glass plate, in air evaporation, evaporation
Time is 10～70min, and then glass plate is put in coagulation bath, and after film solidification departs from glass plate, taking-up is placed in deionized water
Middle immersion 72 hours, residual solvent in completely out film finally are taken out to be placed in dust free room and are dried.
2. application casting solution according to claim 1 prepares the method that PDMS/PVDF is blended infiltrating and vaporizing membrane, and its feature exists
In air evaporation time described in step S2 is respectively 10,30,50,70min.
3. application casting solution according to claim 1 prepares the method that PDMS/PVDF is blended infiltrating and vaporizing membrane, and its feature exists
In the preparation method of the casting solution is comprised the following steps：
S1, by polyvinylidene fluoride and N,N-dimethylacetamide in 80 DEG C of water-baths, under conditions of mechanical agitation, fully dissolve,
The casting solution is taken out, is sealed, is placed in ripening 20-30 hours in 80 DEG C of baking oven；
S2, polydimethylsiloxane is dissolved in tetrahydrofuran, stirs 1～2 hour at 25 DEG C, make the two mix homogeneously；
S3, step S1 solution is taken out from baking oven, is cooled to room temperature, add step S2 solution, under room temperature, stir 3-5 hours,
Each component mix homogeneously is made, casting solution is obtained final product.
4. application casting solution according to claim 3 prepares the method that PDMS/PVDF is blended infiltrating and vaporizing membrane, and its feature exists
In the curing time described in step S1 is 24 hours.
5. application casting solution according to claim 3 prepares the method that PDMS/PVDF is blended infiltrating and vaporizing membrane, and its feature exists
In mixing time described in step S3 is 4 hours.
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| CN114452841A (en) * | 2021-12-08 | 2022-05-10 | 中国石油大学(华东) | PVDF/PDMS @ TiO2Preparation method of self-cleaning micro-nano filter membrane |
| CN115025639A (en) * | 2022-06-09 | 2022-09-09 | 南京碳环生物质能源有限公司 | Method for preparing asymmetric composite membrane for separating VOCs (volatile organic compounds)/non-condensable gas by blending one-step method |
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| CN103464006A (en) * | 2013-09-06 | 2013-12-25 | 长春工业大学 | Preparation of PDMS/PVDF (polydimethylsiloxane/polyvinylidene fluoride) blended microporous film |
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| CN103464006A (en) * | 2013-09-06 | 2013-12-25 | 长春工业大学 | Preparation of PDMS/PVDF (polydimethylsiloxane/polyvinylidene fluoride) blended microporous film |
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| Gel polymer electrolytes based on active PVDF separator for lithium ion battery.I: Preparation and property of PVDF/poly(dimethylsiloxane) blending membrane;Hao Li et al.;《Journal of Membrane Science》;20111231;第379卷;第397-402页 * |
| 用于膜蒸馏的PDMS/PVDF共混微孔膜的制备与性能研究;亢荣敏;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20141115;第17-40页 * |
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