CN108380065A - A kind of dimethyl silicone polymer perforated membrane and its preparation method and application - Google Patents
A kind of dimethyl silicone polymer perforated membrane and its preparation method and application Download PDFInfo
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- CN108380065A CN108380065A CN201810245088.1A CN201810245088A CN108380065A CN 108380065 A CN108380065 A CN 108380065A CN 201810245088 A CN201810245088 A CN 201810245088A CN 108380065 A CN108380065 A CN 108380065A
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- silicone polymer
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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
- B01D71/70—Polymers having silicon in the main chain, with or without sulfur, nitrogen, oxygen or carbon only
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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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Abstract
The present invention relates to a kind of dimethyl silicone polymer perforated membranes and its preparation method and application.The preparation method of the dimethyl silicone polymer perforated membrane based on pore-foaming agent includes：Dimethyl silicone polymer is stirred with curing agent, obtains dimethyl silicone polymer filler；Sugar is dissolved in solvent and is configured to saturation sugar juice, filtering obtains pore-foaming agent saturation sugar juice, or directly grinds sugar and pore-foaming agent powder is obtained by filtration with sieves；Dimethyl silicone polymer filler is mixed with pore-foaming agent saturation sugar juice/pore-foaming agent powder, stirs, obtains the dimethyl silicone polymer filler containing pore-foaming agent；Dimethyl silicone polymer filler containing pore-foaming agent is subjected to even film, baking obtains dimethyl silicone polymer perforated membrane.Gained dimethyl silicone polymer perforated membrane has many advantages, such as that at low cost, stability is good, permeability is good, micropore size is evenly distributed, thickness is easy to control；It cannot be only used for environmental monitoring, filtering, the production of battery etc., it may also be used in microflow control technique.
Description
Technical field
It is especially a kind of based on porous dose of dimethyl silicone polymer perforated membrane the present invention relates to microfluidic art
Preparation method.
Background technology
Currently, there are mainly four types of the method for making of organic polymer perforated membrane, including phase separation method (immersion precipitation), heat
Cause phase separation method (TIPS), alternating deposit technology and water-assisted growth.
Wherein, phase separation method is to mix polymer solution and non-solvent coagulator, makes in polymer solution solvent and non-
Solvent forms directional diffusion and is ultimately generated with the different polyalcohol stephanoporate of morphosis to cause thermodynamics Liquid liquid Separation
Film.Though the method can be used for the making of porous membrane, need the parameter of control more in manufacturing process.
Thermal inactive rule is that will have thermoplasticity and crystalline high polymer and some high boiling small molecule chemical combination
Object (diluent) forms homogeneous phase solution in higher temperatures, then brings it about liquid liquid or separation of solid and liquid by cooling, finally removes
Diluent obtains high polymer microcellular material.Although TIPS methods reduce the complexity of state modulator, but application range is confined to have
There are thermoplasticity and crystalline high polymer.
Alternating deposit technology is deposited repeatedly in the colloidal solution for invade electrically charged substrate oppositely charged, in turn
Multilayer polymer film is obtained, then it is handled using acid or aqueous slkali, makes a part of particles from getting loose and another part
Particle self assembly in substrate, to obtain porous membrane.This method is with filmogen is abundant, easy to operate, stability is good, can
For composite material the advantages that being made, but the complexity of state modulator is higher.
Water-assisted growth is then at high temperature, to make masterplate using condensed water, and cellular film is produced on solid substrate.This
Though method can be used for producing uniform pore diameter, porous membrane of the same size, the pattern of the polymer porous membrane generated often by
The influence of the factors such as solution concentration, operation temperature, humidity, the type of substrate, the type of organic solvent.
There are some defects in above-mentioned several method, be based on this, it is necessary to propose a kind of new organic polymer perforated membrane
Method for making.
Invention content
Insufficient present in technical background in order to overcome, the present invention provides a kind of dimethyl silicone polymer based on pore-foaming agent
The preparation method of perforated membrane.This method can overcome the complexity of state modulator present in phase separation method and alternating deposit method high
The shortcomings that, and the deficiency that TIPS methods are of limited application can be solved, moreover it is possible to make up in water-assisted growth porous membrane by solution concentration,
The defect that many factors such as temperature, humidity, substrate type and organic solvent influence.
A kind of preparation method of the dimethyl silicone polymer perforated membrane based on pore-foaming agent, including：
(1) dimethyl silicone polymer ontology is stirred with its curing agent to fine and closely woven bubble is generated, and is vacuumized, is obtained poly- diformazan
Radical siloxane filler；
(2) sugar is dissolved in solvent and is configured to saturation sugar juice, filtering obtains pore-foaming agent saturation sugar juice, or directly
Sugar is ground and pore-foaming agent powder is obtained by filtration with sieves；
(3) dimethyl silicone polymer filler made from step (1) and pore-foaming agent saturation sugar made from step (2) is molten
Then liquid/pore-foaming agent powder mixing, stirring are vacuumized, are taken out after bubble collapse to blistering, filter, obtain containing pore-foaming agent
Dimethyl silicone polymer filler, it is spare；
(4) step (3) the dimethyl silicone polymer filler obtained containing pore-foaming agent is subjected to even film, baking is naturally cold
But it rinses afterwards, obtains dimethyl silicone polymer perforated membrane.
In step (1), the pumpdown time is 40-120min.
In step (1), what the optional those skilled in the art of the curing agent were grasped makes dimethyl silicone polymer sheet
The cured auxiliary agent of body.The mass ratio of the dimethyl silicone polymer and curing agent is 10:1.
In step (2), the solvent is selected from organic solvent and/or water；The organic solvent is selected from acetone, absolute ethyl alcohol
Deng.
In step (2), the aperture of the filtering is 0.22 μm；The sieves is the mesh of 500 mesh/1000.
In step (3), the mass ratio of the pore-foaming agent and dimethyl silicone polymer filler can be according to required perforated membrane
The density in hole be adjusted, such as：1:1、1:2、1:3 etc..
In step (3), the pumpdown time is 40-120min.
In step (4), the even film is that the dimethyl silicone polymer filler for containing pore-foaming agent is placed on slide glass, is adjusted even
The parameter of glue machine carries out even film；Wherein, the Parameter Conditions of the even film are：Sol evenning machine is in dripping glue state, rotating speed 500-550
Revolutions per second, run time is 60 seconds；, in spin coating state, rotating speed can be adjusted according to the thickness of film for it, 500-6000 turn/
Change in the range of second, run time is 120 seconds.The slide glass is selected from silicon chip, sheet glass, PMMA pieces, potsherd etc..
In step (4), the baking temperature is 65-80 DEG C, preferably 75 DEG C；Baking time is 30-40min, preferably
35min。
In step (4), the solution of the flushing is the ethanol water of mass concentration 20%；When flushing, first use ultrasound clear
The cleaning that instrument carries out sample 5 minutes is washed, is then directly rinsed again, the flushing temperature is 50-90 DEG C, preferably 60 DEG C.
The present invention also provides the dimethyl silicone polymer perforated membranes made from the above method.The dimethyl silicone polymer is more
The film thickness of pore membrane is 5-100 microns, and aperture changes in the range of hundreds of nanometers to tens microns.
The present invention also provides above-mentioned dimethyl silicone polymer perforated membranes in environmental monitoring, filtering, battery production, micro-fluidic skill
The application of art etc..
The preparation method of dimethyl silicone polymer perforated membrane of the present invention has at low cost, easy to operate, parameter and thin
The features such as film thickness is easy to control.Gained perforated membrane has many advantages, such as that stability is good, permeability is good, micropore size is evenly distributed.
Specific implementation mode
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
A kind of dimethyl silicone polymer method for preparing porous film based on pore-foaming agent of embodiment 1
A kind of dimethyl silicone polymer method for preparing porous film based on pore-foaming agent, step are：
(1) preparation of dimethyl silicone polymer filler：
By dimethyl silicone polymer ontology and the stirring of dimethyl silicone polymer curing agent until generating fine and closely woven bubble, then
It is placed in vacuum drying chamber and vacuumizes and keep 40min or more, it is spare；
Wherein, the mass ratio 10 of dimethyl silicone polymer ontology and dimethyl silicone polymer curing agent:1；
(2) preparation of pore-foaming agent：
The sugar that quality is more than to its solubility is dissolved in alcohol or water, and is sufficiently stirred to accelerate to dissolve, then with filtering
Device filters the solution and obtains saturation sugar juice, or directly grinds sugar and pore-foaming agent powder is obtained by filtration with sieves；
Wherein the aperture of filter can be 0.22 micron, and sieves is the mesh of 500 mesh/1000.
(3) preparation of the dimethyl silicone polymer filler containing pore-foaming agent：
The pore-foaming agent prepared in the dimethyl silicone polymer filler and step (2) that are prepared in step (1) is mixed
To blistering, it is subsequently placed in vacuum drying chamber and vacuumizes and kept for 40 minutes or more, taken out after bubble collapse, filter paper mistake is used in combination
Filter obtains the dimethyl silicone polymer filler containing sugar, spare；
Wherein, the mass ratio 1 of pore-foaming agent and dimethyl silicone polymer filler:1、1:2、1:3 according to required perforated membrane
The density in hole is changed；
(4) preparation of dimethyl silicone polymer perforated membrane：
The dimethyl silicone polymer filler containing pore-foaming agent prepared in a small amount of step (3) is taken to be placed in silicon chip with beaker
On, and adjust the parameter of sol evenning machine to 500 revolutions per seconds of dispensing and operation 60 seconds, 6000 revolutions per seconds of dispensing and operation 120 seconds carry out even
Film.Then it is toasted about 35 minutes in the baking sheet for being placed in about 75 degrees Celsius, after its at normal temperatures natural cooling, first with super
It is about 1 that sound, which rinses instrument in the mass ratio of absolute ethyl alcohol and water,:Flushing in 5 minutes is carried out in 4 60 degrees Celsius of solution to it, then
60 degrees Celsius of solution of identical proportioning rinses about 7 times, obtains dimethyl silicone polymer perforated membrane repeatedly.
The thickness of gained dimethyl silicone polymer perforated membrane be 5 microns, micropore size be distributed in hundreds of nanometers to tens it is micro-
Variation in rice range.
A kind of dimethyl silicone polymer method for preparing porous film based on pore-foaming agent of embodiment 2
A kind of dimethyl silicone polymer method for preparing porous film based on pore-foaming agent, step are：
(1) preparation of dimethyl silicone polymer filler：
By dimethyl silicone polymer ontology and curing agent stirring until generating fine and closely woven bubble, it is subsequently placed in vacuum drying chamber
In vacuumize and keep 40 minutes or more it is spare；
Wherein, the mass ratio of dimethyl silicone polymer ontology and curing agent is 10:1；
(2) preparation of pore-foaming agent：
The sugar that quality is more than to its solubility is dissolved in alcohol or water, and is sufficiently stirred to accelerate to dissolve, then with filtering
Device filters the solution and obtains saturation sugar juice, or directly grinds sugar and pore-foaming agent powder is obtained by filtration with sieves；
Wherein, the aperture of filter can be 0.22 micron, and sieves is the mesh of 500 mesh/1000；
(3) preparation of the dimethyl silicone polymer filler containing pore-foaming agent：
The pore-foaming agent prepared in the dimethyl silicone polymer filler prepared in step (1) and step (2) is mixed and stirred
It mixes to blistering, is subsequently placed in vacuum drying chamber and vacuumizes and kept for 40 minutes or more, taken out after bubble collapse and use filter paper
It is spare that the dimethyl silicone polymer filler containing sugar is obtained by filtration；
Wherein, the mass ratio of pore-foaming agent and dimethyl silicone polymer filler can be according to the density in the hole of required perforated membrane
It is changed；
(4) preparation of dimethyl silicone polymer perforated membrane：
The dimethyl silicone polymer filler containing pore-foaming agent prepared in a small amount of step (3) is taken to be placed in PMMA pieces with beaker
On, and adjust the parameter of sol evenning machine to 500 revolutions per seconds of dispensing and operation 60 seconds, 1500 revolutions per seconds of dispensing and operation 120 seconds carry out even
Then film toasts it about 35 minutes in the baking sheet for being placed in about 75 degrees Celsius, after its at normal temperatures natural cooling, first with super
It is about 1 that sound, which rinses instrument in the mass ratio of absolute ethyl alcohol and water,:Flushing in 5 minutes is carried out in 4 60 degrees Celsius of solution to it, then
The solution of identical proportioning rinses about 7 times repeatedly, obtains dimethyl silicone polymer perforated membrane.
The thickness of gained dimethyl silicone polymer perforated membrane be 50 microns, micropore size be distributed in hundreds of nanometers to tens it is micro-
Variation in rice range.
A kind of dimethyl silicone polymer method for preparing porous film based on pore-foaming agent of embodiment 3
Specific embodiment three, a kind of dimethyl silicone polymer method for preparing porous film based on pore-foaming agent, step are：
(1) preparation of dimethyl silicone polymer filler：
By dimethyl silicone polymer ontology and curing agent stirring until generating fine and closely woven bubble, it is subsequently placed in vacuum drying chamber
In vacuumize and keep 40 minutes or more it is spare；
Wherein, the ratio of dimethyl silicone polymer ontology and curing agent is 10:1；
(2) preparation of pore-foaming agent：
Slight excess of sugar is dissolved in alcohol or water, and is sufficiently stirred to accelerate to dissolve, it then should with filter filtering
Solution obtains saturation sugar juice, or directly grinds sugar and pore-foaming agent powder is obtained by filtration with sieves；
Wherein, the aperture of filter can be 0.22 micron, and sieves is the mesh of 500 mesh/1000；
(3) preparation of the dimethyl silicone polymer filler containing pore-foaming agent：
The pore-foaming agent prepared in the dimethyl silicone polymer filler prepared in step (1) and step (2) is mixed and stirred
It mixes to blistering, is subsequently placed in vacuum drying chamber and vacuumizes and kept for 40 minutes or more, taken out after bubble collapse and use filter paper
It is spare that the dimethyl silicone polymer filler containing sugar is obtained by filtration；
Wherein, the mass ratio of pore-foaming agent and dimethyl silicone polymer filler can be according to the density in the hole of required perforated membrane
It is changed；
(4) preparation of dimethyl silicone polymer perforated membrane：
The dimethyl silicone polymer filler containing pore-foaming agent prepared in a small amount of step (3) is taken to be placed in potsherd with beaker
On, and adjust the parameter of sol evenning machine to 500 revolutions per seconds of dispensing and operation 60 seconds, 500 revolutions per seconds of dispensing and operation 120 seconds carry out even
Then film toasts it about 35 minutes in the baking sheet for being placed in about 75 degrees Celsius, wait for that natural cooling first uses ultrasound at normal temperatures for it
It is about 1 that instrument, which is rinsed, in the mass ratio of absolute ethyl alcohol and water:Flushing in 5 minutes is carried out to it in 4 60 degrees Celsius of solution, it is rear to use
The acetone soln of room temperature rinses about 7 times repeatedly, obtains dimethyl silicone polymer perforated membrane.
The thickness of gained dimethyl silicone polymer perforated membrane is 100 microns, and micropore size is distributed in hundreds of nanometers to tens
Variation in micron range.
Compliance test result
Perforated membrane obtained by embodiment 1-3 is tested, is obtained as drawn a conclusion：
(1) stability
Micropore in perforated membrane will not change because long-time is placed, and micropore size remains unchanged；Perforated membrane has
Certain elasticity and flexibility can resist the effect of pullling to a certain extent.
(2) permeability
The micropore of the perforated membrane can pass through：Water, solion, organic solvent (such as alcohol).
(3) even aperture distribution
By scanning electron microscopic observation perforated membrane, the micropore size of the perforated membrane be mainly distributed on hundreds of nanometers to tens it is micro-
In the range of rice, micropore is evenly distributed on PDMS films.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. a kind of preparation method of the dimethyl silicone polymer perforated membrane based on pore-foaming agent, which is characterized in that including：
(1) dimethyl silicone polymer is stirred with its curing agent to fine and closely woven bubble is generated, and is vacuumized, is obtained dimethyl silicone polymer and fill out
Fill agent；
(2) sugar is dissolved in solvent and is configured to saturation sugar juice, filtering obtains pore-foaming agent saturation sugar juice；Or grind sugar,
Filtering, obtains pore-foaming agent powder；
(3) pore-foaming agent made from dimethyl silicone polymer filler made from step (1) and step (2) is saturated sugar juice/cause
Agent powder in hole mixes, and then stirring is vacuumized, taken out after bubble collapse to blistering, filter, obtain the poly- diformazan containing pore-foaming agent
Radical siloxane filler, it is spare；
(4) step (3) the dimethyl silicone polymer filler obtained containing pore-foaming agent is subjected to even film, toasted, after natural cooling
It rinses, obtains dimethyl silicone polymer perforated membrane.
2. preparation method according to claim 1, which is characterized in that the pumpdown time is 40-120min.
3. preparation method according to claim 1 or 2, which is characterized in that in step (1), the dimethyl silicone polymer
Mass ratio with curing agent is 10:1.
4. according to any preparation methods of claim 1-3, which is characterized in that in step (2), the solvent is selected from organic
Solvent and/or water.
5. according to any preparation methods of claim 1-4, which is characterized in that in step (3), the pore-foaming agent and poly- two
The mass ratio of methylsiloxane filler is adjusted according to the density in the hole of required perforated membrane.
6. according to any preparation methods of claim 1-5, which is characterized in that in step (4), the parameter item of the even film
Part is：When dripping glue state, rotating speed is 500-550 revolutions per seconds；When spin coating state, rotating speed is adjusted according to the thickness of film.
7. according to any preparation methods of claim 1-6, which is characterized in that in step (4), the baking temperature is
65-80 DEG C, preferably 75 DEG C.
8. according to any preparation methods of claim 1-7, which is characterized in that in step (4), the flushing temperature is
50-90 DEG C, preferably 60 DEG C.
9. dimethyl silicone polymer perforated membrane made from any preparation methods of claim 1-8；Preferably, the poly- diformazan
The film thickness of radical siloxane perforated membrane is 5-100 microns, and aperture is in the range of hundreds of nanometers to tens microns.
10. the dimethyl silicone polymer perforated membrane described in claim 9 is in environmental monitoring, filtering, battery production, microflow control technique
The application of aspect.
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| CN111233510A (en) * | 2020-02-19 | 2020-06-05 | 南京航空航天大学 | Large-area deicing low-interface toughness porous material and preparation method thereof |
| CN112409918A (en) * | 2020-10-30 | 2021-02-26 | 北京科技大学 | Magnetic response dynamic autocrine coating and preparation method and use method thereof |
| CN116410663A (en) * | 2021-12-30 | 2023-07-11 | 中国科学院理化技术研究所 | Dynamic bionic anti-scaling coating capable of being used for long time and being efficient and energy-saving |
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