CN112844070A - Method for preparing polyvinylidene fluoride hollow film by microfluidics - Google Patents
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Abstract
A method for preparing a polyvinylidene fluoride hollow membrane by microfluidics is characterized by comprising the following steps: the method comprises the following steps: firstly, preparing raw materials for preparing the PVDF hollow membrane, and then preparing the PVDF hollow membrane by adopting a microfluidic system to obtain a final target product. According to the method for preparing the film by the micro-fluidic method, the micro-channels with different sizes or the flow velocity of each channel can be adjusted to control the mixing and distribution of each medium in the channel, so that the method has the advantages of accurately controlling the thickness and the components of the film, enabling the thickness of the film to be more uniform, and meanwhile, due to the natural advantages of the micro-size, the method has the advantages of material saving, high synthesis efficiency and the like.
Description
Technical Field
The application relates to the technical field of thin film preparation, in particular to a method for preparing a polyvinylidene fluoride hollow film through microfluidics.
Background
The PVDF (polyvinylidene fluoride) hollow film is a semi-crystalline polymer with good toughness and high strength, has the characteristics of corrosion resistance, heat resistance, radiation resistance and the like, and is an ideal industrial separation film material. The prior art preparation methods comprise a solution spinning method, a melt spinning stretching method, a thermally induced phase separation method and the like. However, the above method may have a problem that solid-liquid phase separation occurs due to crystallization during the production process.
In recent years, Microfluidics (Microfluidics) refers to science and technology involved in systems that use microchannels (tens to hundreds of microns in size) to process or manipulate tiny fluids (nanoliters to attoliters), and is an emerging interdiscipline that involves chemistry, fluid physics, microelectronics, new materials, biology, and biomedical engineering. Because of their miniaturization, integration, etc., microfluidic devices are commonly referred to as microfluidic chips, also known as Lab-on-a-chips (Lab-on-a-chips) and micro-Total Analytical systems (micro-Total Analytical systems). The early concept of microfluidics can be traced back to gas chromatographs fabricated on silicon wafers by photolithography in the 70 s of the 19 th century, and then developed into microfluidic capillary electrophoresis instruments, microreactors and the like. One of the important features of microfluidics is the unique fluid properties in microscale environments, such as laminar flow and droplets. With these unique fluidic phenomena, microfluidics can achieve a range of microfabrication and micromanipulation that are difficult to accomplish with conventional methods. Microfluidics is currently considered to have great development potential and broad application prospects in biomedical research.
However, no report is available on how to prepare PVDF hollow membranes by a microfluidic method.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for preparing a polyvinylidene fluoride hollow membrane by microfluidics without solid-liquid phase separation caused by crystallization.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for preparing a PVDF hollow membrane by a microfluidic method comprises the following steps: firstly, preparing raw materials for preparing the PVDF hollow membrane, and then preparing the PVDF hollow membrane by adopting a microfluidic system to obtain a final target product.
Preferably, the preparation of the raw material: 5 wt% polyethylene water solution as external phase, fluorine Polyethylene (PVDF)/dimethyl formamide (DMF) solution as intermediate phase, 25.0g PVDF dissolved in 70 deg.C 75.0g DMF, continuous stirring for 6 h; internal phase 50g of molten paraffin (melting point 27 ℃ C.);
preferably, the preparation of the PVDF hollow membrane specifically comprises:
the method comprises the following steps of (1) introducing a material into a channel of a micro-fluidic system by using an injection pump, wherein the micro-fluidic system comprises a first micro-channel, a second micro-channel and a third micro-channel which are positioned on a micro-fluidic mainboard, the first micro-channel is positioned in the middle of the micro-fluidic mainboard and extends along the length direction, one end of the first micro-channel is a medium feeding end, and the other end of the first micro-channel is a medium output end; the second microchannel and the third microchannel are distributed on the side surface of the first microchannel and are vertically connected with the first microchannel, the second microchannel is positioned at the upstream of the medium circulation, and the third microchannel is positioned at the downstream of the medium circulation; the media in the second microchannel and the third microchannel are gathered in the first microchannel and output from the media output end;
then inputting the internal phase into a first microchannel of a microfluidic system through a medium feeding end, inputting the intermediate phase into a second microchannel, and inputting the external phase into a third microchannel;
and then collecting the gel membrane which is subjected to the micro-fluidic system and is gelated in a container containing deionized water, heating the gel membrane to 60-70 ℃ or soaking the gel membrane in an n-octane solution for 20-30 hours, removing paraffin to form a hollow membrane, and then washing and drying the hollow membrane by using the deionized water to obtain the PVDF hollow membrane.
Preferably, the inner pore size of the first microchannel is 40-300 microns, the inner pore size of the second microchannel is 400-500 microns, and the inner pore size of the third microchannel is 600-800 microns.
Preferably, the number of the second micro-channels is at least one: preferably, the number of the second microchannels is two, and the two second microchannels are vertically connected with the first microchannel and symmetrically distributed on two sides of the first microchannel.
Preferably, the number of the third micro-channels is at least one: preferably, the number of the third microchannels is two, and the two third microchannels are vertically connected with the first microchannel and symmetrically distributed on two sides of the first microchannel.
Preferably, the medium flow of the first microchannel is 50-80 μ L/min, the medium flow of the second microchannel is 30-50 μ L/min, and the medium flow of the third microchannel is 80-150 μ L/min.
The film prepared by the specific method has the following advantages and advantages:
1. according to the method for preparing the film by the micro-fluidic method, the micro-channels with different sizes or the flow velocity of each channel can be adjusted to control the mixing and distribution of each medium in the channel, so that the advantages of accurately controlling the thickness and the components of the film can be achieved, the thickness of the film is more uniform, and the method has the advantages of material saving, high synthesis efficiency and the like due to the natural advantages of the micro-size.
2. The invention adopts liquid paraffin as a medium to combine with a micro-fluidic system for the first time, brings various components into the micro-fluidic system and a collecting container, and then evaporates and removes the paraffin, thereby uniformly obtaining a plurality of small holes on the obtained film and providing support for the application of the film in the field of filtration or purification. The paraffin is used as a molten state, and is set as an internal phase of the microfluidic system to be used, so that the uniform distribution effect of the holes of the film can be well realized; the paraffin and other components can be fully mixed and dispersed, the control is easier, other components are driven to operate more stably and more uniformly, and the air holes of the obtained target product are more uniformly generated.
3. The PVDF film is prepared by a microfluidic method, and the film prepared by the method has the following advantages: the cost is low, and the method has the potential of industrial production; the components are controllable, for example, films with different thicknesses can be obtained by adjusting the flow rate of the medium in each micro-channel; meanwhile, the material has the advantages of high temperature resistance, corrosion resistance, good mechanical properties and the like.
4. Adopt bilateral symmetry to set up the microchannel simultaneously among this application preferred scheme and come the feeding, can realize controlling feeding simultaneously, guarantee the stability of medium in the passageway, guarantee the symmetry of film structure and generate. Three phases are divided into three microfluidic channels to enter the system, so that the flow speed and reaction conditions of each phase can be flexibly controlled, and the film forming conditions can be accurately controlled, so that the finally obtained material has more uniform thickness and more excellent performance. In addition, the internal diameter of each passageway and the medium velocity of flow that corresponds all have reasonable control parameter in this application micro-fluidic, also make or final product do not exist because of the crystallization takes place the phenomenon of solid-liquid phase separation, also make final product have thickness even, the equipartition aperture above, can adapt to the operation requirement in filtration or purification field.
5. The micro-fluidic system can generate two or more hollow membranes simultaneously by one set of micro-fluidic system through controlling the length of the pipeline and the initial flow velocity, and greatly improves the production efficiency.
Drawings
FIG. 1 is a schematic diagram of a pipeline distribution structure of a microfluidic system for preparing a PVDF hollow membrane.
FIG. 2 is a schematic diagram of a flow structure of a method for preparing a polyvinylidene fluoride hollow membrane by microfluidics.
FIG. 3 is a simulation diagram of a polyvinylidene fluoride hollow membrane prepared by microfluidics according to the present application.
As shown in the attached drawings: 1. first microchannel (for medium inflow of the internal phase and outflow after mixing of the three phases), 2. second microchannel (for medium inflow of the intermediate phase), 3. third microchannel (for medium inflow of the external phase).
Detailed Description
The present invention will be described in further detail below with reference to specific examples, but the present invention is not limited to only the following examples.
The micro-fluidic system adopts the structure shown in the attached figures 1-2, and comprises a first micro-channel 1, a second micro-channel 2 and a third micro-channel 3 which are positioned on a micro-fluidic main board, wherein the first micro-channel is positioned in the middle of the micro-fluidic main board and extends along the length direction, one end of the first micro-channel is a medium feeding end, and the other end of the first micro-channel is a medium output end; the second microchannel and the third microchannel are distributed on the side surface of the first microchannel and are vertically connected with the first microchannel, the second microchannel is positioned at the upstream of the medium circulation, and the third microchannel is positioned at the downstream of the medium circulation; the media in the second microchannel and the third microchannel are gathered in the first microchannel and output from the media output end; in the embodiment of the application, two second microchannels and two third microchannels are respectively arranged, are respectively symmetrically arranged on two sides of the first microchannel and are vertical to the first microchannel; the curved pipe in fig. 2 is a pipe for feeding, which facilitates feeding.
As shown in fig. 3, a simulated preparation diagram of a ZrO2 ceramic film prepared by the microfluidic method of the present application is shown, wherein the specific color change of Phase3 represents the change of the percentage of different phases, wherein red is a paraffin Phase (the color of the top of Phase 3), blue is an aqueous Phase (the color of the bottom of Phase 3), and green is an oil Phase (the color of the middle of Phase 3); y represents the length of the micro-channel (unit is m), Z represents the specific position of the micro-channel, and the accompanying drawings (black and white figures, based on the drawings published by the application) can see that the hollow film is formed by the application along with the change of the proportion of each phase and the mutual reaction and fusion of the phase and the phase.
Example 1
(1) Material preparation
The external phase is a 5 wt% polyethylene aqueous solution,
the intermediate phase is a solution of polyvinyl fluoride (PVDF)/Dimethylformamide (DMF), namely 25.0g of PVDF is dissolved in 75.0g of DMF at 70 ℃, and the mixture is continuously stirred for 6 hours to obtain the intermediate phase;
internal phase 50g of molten paraffin (melting point 27 ℃ C.);
(2) preparation of PVDF hollow membrane
A material is introduced into a channel of the microfluidic system shown in the attached figures 1-2 by using a syringe pump, the microfluidic system comprises a first microchannel 1, a second microchannel 2 and a third microchannel 3 which are positioned on a microfluidic main board, the first microchannel is positioned in the middle of the microfluidic main board and extends along the length direction, one end of the first microchannel is a medium feeding end, and the other end of the first microchannel is a medium output end; the second microchannel and the third microchannel are distributed on the side surface of the first microchannel and are vertically connected with the first microchannel, the second microchannel is positioned at the upstream of the medium circulation, and the third microchannel is positioned at the downstream of the medium circulation; the media in the second microchannel and the third microchannel are gathered in the first microchannel and output from the media output end; in the embodiment of the application, two second microchannels and two third microchannels are respectively arranged, are respectively symmetrically arranged on two sides of the first microchannel and are vertical to the first microchannel;
then inputting the internal phase into a first microchannel of a microfluidic system through a medium feeding end, inputting the intermediate phase into a second microchannel, and inputting the external phase into a third microchannel; collecting each medium after passing through the microfluidic system;
collecting the PVDF membrane in deionized water to obtain a gel membrane, heating the gel membrane to 68 ℃ (or soaking the gel membrane in n-octane solution for 24 hours), removing paraffin to form a hollow membrane, and then washing and drying the hollow membrane by using the deionized water;
the flow rate control of the medium in each micro-channel is as follows: the medium flow of the first micro-channel is 5 muL/min, the medium flow of the second micro-channel is 32 muL/min, and the medium flow of the third micro-channel is 82 muL/min;
the inner pore diameter of the first microchannel is 50 micrometers, the inner pore diameter of the second microchannel is 420 micrometers, and the inner pore diameter of the third microchannel is 630 micrometers.
Example 2
(1) Material preparation
External phase 5 wt% aqueous polyethylene solution
The intermediate phase is a solution of polyvinyl fluoride (PVDF)/Dimethylformamide (DMF), 28.0g of PVDF is dissolved in 72.0g of DMF at 70 ℃, and the mixture is continuously stirred for 5.5 hours;
internal phase 48g of molten paraffin (melting point 27 ℃ C.);
(2) preparation of PVDF hollow membrane
A material is introduced into a channel of the microfluidic system shown in the attached figures 1-2 by using a syringe pump, the microfluidic system comprises a first microchannel 1, a second microchannel 2 and a third microchannel 3 which are positioned on a microfluidic main board, the first microchannel is positioned in the middle of the microfluidic main board and extends along the length direction, one end of the first microchannel is a medium feeding end, and the other end of the first microchannel is a medium output end; the second microchannel and the third microchannel are distributed on the side surface of the first microchannel and are vertically connected with the first microchannel, the second microchannel is positioned at the upstream of the medium circulation, and the third microchannel is positioned at the downstream of the medium circulation; the media in the second microchannel and the third microchannel are gathered in the first microchannel and output from the media output end;
then inputting the internal phase into a first microchannel of a microfluidic system through a medium feeding end, inputting the intermediate phase into a second microchannel, and inputting the external phase into a third microchannel;
collecting PVDF membrane in deionized water, heating gel membrane to 70 deg.C (or soaking in n-octane solution for 24 hr), removing paraffin to form hollow membrane, and washing with deionized water;
the flow rate control of the medium in each micro-channel is as follows: the medium flow of the first micro-channel is 55 mu L/min, the medium flow of the second micro-channel is 35 mu L/min, and the medium flow of the third micro-channel is 86 mu L/min;
the inner pore diameter of the first microchannel is 70 micrometers, the inner pore diameter of the second microchannel is 450 micrometers, and the inner pore diameter of the third microchannel is 660 micrometers.
Example 3
(1) Material preparation
External phase 5 wt% aqueous polyethylene solution
The intermediate phase is a solution of polyvinyl fluoride (PVDF)/Dimethylformamide (DMF), 30.0g of PVDF is dissolved in 70.0g of DMF at 70 ℃, and the mixture is continuously stirred for 6.5 hours;
internal phase 50g of molten paraffin (melting point 27 ℃ C.);
(2) preparation of PVDF hollow membrane
A material is introduced into a channel of the microfluidic system shown in the attached figures 1-2 by using a syringe pump, the microfluidic system comprises a first microchannel 1, a second microchannel 2 and a third microchannel 3 which are positioned on a microfluidic main board, the first microchannel is positioned in the middle of the microfluidic main board and extends along the length direction, one end of the first microchannel is a medium feeding end, and the other end of the first microchannel is a medium output end; the second microchannel and the third microchannel are distributed on the side surface of the first microchannel and are vertically connected with the first microchannel, the second microchannel is positioned at the upstream of the medium circulation, and the third microchannel is positioned at the downstream of the medium circulation; the media in the second microchannel and the third microchannel are gathered in the first microchannel and output from the media output end;
then inputting the internal phase into a first microchannel of a microfluidic system through a medium feeding end, inputting the intermediate phase into a second microchannel, and inputting the external phase into a third microchannel;
collecting PVDF membrane in deionized water, heating gel membrane to 70 deg.C (or soaking in n-octane solution for 24 hr), removing paraffin to form hollow membrane, and washing with deionized water;
the flow rate control of the medium in each micro-channel is as follows: the medium flow of the first micro-channel is 60 mu L/min, the medium flow of the second micro-channel is 40 mu L/min, and the medium flow of the third micro-channel is 95 mu L/min;
the inner pore diameter of the first microchannel is 100 micrometers, the inner pore diameter of the second microchannel is 480 micrometers, and the inner pore diameter of the third microchannel is 720 micrometers.
Example 4
(1) Material preparation
External phase 5 wt% aqueous polyethylene solution
The intermediate phase is a solution of polyvinyl fluoride (PVDF)/Dimethylformamide (DMF), 32.0g of PVDF is dissolved in 68.0g of DMF at 70 ℃, and the mixture is continuously stirred for 6 hours;
internal phase 52g of molten paraffin (melting point 27 ℃ C.);
(2) preparation of PVDF hollow membrane
A material is introduced into a channel of the microfluidic system shown in the attached figures 1-2 by using a syringe pump, the microfluidic system comprises a first microchannel 1, a second microchannel 2 and a third microchannel 3 which are positioned on a microfluidic main board, the first microchannel is positioned in the middle of the microfluidic main board and extends along the length direction, one end of the first microchannel is a medium feeding end, and the other end of the first microchannel is a medium output end; the second microchannel and the third microchannel are distributed on the side surface of the first microchannel and are vertically connected with the first microchannel, the second microchannel is positioned at the upstream of the medium circulation, and the third microchannel is positioned at the downstream of the medium circulation; the media in the second microchannel and the third microchannel are gathered in the first microchannel and output from the media output end;
then inputting the internal phase into a first microchannel of a microfluidic system through a medium feeding end, inputting the intermediate phase into a second microchannel, and inputting the external phase into a third microchannel;
collecting PVDF membrane in deionized water, heating gel membrane to 72 deg.C (or soaking in n-octane solution for 24 hr), removing paraffin to form hollow membrane, and washing with deionized water;
the flow rate control of the medium in each micro-channel is as follows: the medium flow of the first micro-channel is 75 muL/min, the medium flow of the second micro-channel is 43 muL/min, and the medium flow of the third micro-channel is 110 muL/min;
the inner pore size of the first microchannel is 220 micrometers, the inner pore size of the second microchannel is 490 micrometers, and the inner pore size of the third microchannel is 760 micrometers.
Claims (7)
1. A method for preparing a polyvinylidene fluoride hollow membrane by microfluidics is characterized by comprising the following steps: the method comprises the following steps: firstly, preparing raw materials for preparing the PVDF hollow membrane, and then preparing the PVDF hollow membrane by adopting a microfluidic system to obtain a final target product.
2. The method for preparing the polyvinylidene fluoride hollow membrane in a microfluidic mode according to claim 1, wherein the method comprises the following steps: the preparation of the raw material comprises the following steps: 5 wt% polyethylene water solution as external phase, fluorine polyethylene/dimethyl formamide solution as intermediate phase, 25.0g PVDF dissolved in 70 deg.C 75.0g DMF, continuous stirring for 6 h; internal phase 50g of molten paraffin.
3. The method for preparing the polyvinylidene fluoride hollow membrane in a microfluidic mode according to claim 1, wherein the method comprises the following steps: the preparation method of the PVDF hollow membrane specifically comprises the following steps:
the method comprises the following steps of (1) introducing a material into a channel of a micro-fluidic system by using an injection pump, wherein the micro-fluidic system comprises a first micro-channel, a second micro-channel and a third micro-channel which are positioned on a micro-fluidic mainboard, the first micro-channel is positioned in the middle of the micro-fluidic mainboard and extends along the length direction, one end of the first micro-channel is a medium feeding end, and the other end of the first micro-channel is a medium output end; the second microchannel and the third microchannel are distributed on the side surface of the first microchannel and are vertically connected with the first microchannel, the second microchannel is positioned at the upstream of the medium circulation, and the third microchannel is positioned at the downstream of the medium circulation; the media in the second microchannel and the third microchannel are gathered in the first microchannel and output from the media output end;
then inputting the internal phase into a first microchannel of a microfluidic system through a medium feeding end, inputting the intermediate phase into a second microchannel, and inputting the external phase into a third microchannel;
and then collecting the gel membrane which is subjected to the micro-fluidic system and is gelated in a container containing deionized water, heating the gel membrane to 60-70 ℃ or soaking the gel membrane in n-octane solution for 20-30 hours, removing paraffin to form a hollow membrane, and then cleaning and drying the hollow membrane by using the deionized water to obtain the PVDF hollow membrane.
4. The method for preparing the polyvinylidene fluoride hollow membrane in a microfluidic mode according to claim 3, wherein the method comprises the following steps: the inner pore diameter of the first micro-channel is 40-300 microns, the inner pore diameter of the second micro-channel is 400-800 microns, and the inner pore diameter of the third micro-channel is 600-800 microns.
5. The method for preparing the polyvinylidene fluoride hollow membrane in a microfluidic mode according to claim 3, wherein the method comprises the following steps: the number of the second micro-channels is at least one, and the number of the third micro-channels is at least one.
6. The method for preparing the polyvinylidene fluoride hollow membrane in a microfluidic mode according to claim 3, wherein the method comprises the following steps: the number of the second micro-channels is two, and the two second micro-channels are vertically connected with the first micro-channel and symmetrically distributed on two sides of the first micro-channel; the number of the third micro-channels is two, and the two third micro-channels are vertically connected with the first micro-channel and symmetrically distributed on two sides of the first micro-channel.
7. The method for preparing the polyvinylidene fluoride hollow membrane in a microfluidic mode according to claim 3, wherein the method comprises the following steps: the medium flow of the first micro-channel is 50-80 mu L/min, the medium flow of the second micro-channel is 30-50 mu L/min, and the medium flow of the third micro-channel is 80-150 mu L/min.
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