CN106977796A - A kind of honeycomb structure micropore waterproof breathable membrane and preparation method thereof - Google Patents
A kind of honeycomb structure micropore waterproof breathable membrane and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/05—Elimination by evaporation or heat degradation of a liquid phase
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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- C08L2203/14—Applications used for foams
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention belongs to technical field of function materials, and in particular to a kind of honeycomb structure micropore waterproof breathable membrane, and further disclose its preparation method.Micropore waterproof breathable membrane of the present invention, using specially designed modified poly ethylene as base-material, is aided with the modifying function of ionic liquid, the obtained waterproof breathable membrane with honeycomb structure, and it has more preferable advantage in waterproof and permeability.And obtained film is modified then better than with general ion liquid modified obtained film with amino acid ion liquid.
Description
Technical field
The invention belongs to technical field of function materials, and in particular to a kind of honeycomb structure micropore waterproof breathable membrane, go forward side by side
One step discloses its preparation method.
Background technology
Waterproof ventilated membrane is a kind of new high polymer waterproof material, is that one kind can allow gas permeation, but can obstruct
The film that liquid such as water is passed through.From manufacture craft, the technical requirements of waterproof ventilated membrane are higher than general waterproof material
It is many；Simultaneously from quality, waterproof ventilated membrane also has the functional characteristics not available for other waterproof materials.
In order to reach ventilative purpose, it is thin that waterproof breathable membrane is designed and manufactured into unique plastics with multi-cellular structure
Film, in terms of the transverse section of film, is then dispersed with the microscopic pinholes that many diameters only have 1-2 microns.So, as air and/or water
Gas molecule as steam is easy to through these apertures from damp and hot environment to exosmosis, and the fresh air of outside is not
It is disconnected to pass through these aperture endosmosises, so as to reach the purpose of displacement so that film has the function of breathing；And on the other hand,
Fluid molecule as to aqueous water is then because the effect of surface tension is difficult to permeate and is obstructed, so that this ventilative thin
Film possesses ventilated and waterproof feature.
At present, in the market has had a variety of waterproof breathable membranes to occur, such as：1) TPU Waterproof ＆ Moisture Permeable Films, are a kind of equal
The non-porous film of matter, uses the polyurethane elastomer with hydrophilic radical for main material, is added using salivation or blow molding process
Work, but this film melting points are low (120 DEG C or so), dampness is anti-big, cryogenic property and it is compound after water-sprinkling processability it is bad etc.；2)
The many ester films of copolyether, the film is also a kind of homogeneous nonporous film, is based on PEO and terephthalic acid (TPA) fourth two
The fusing extrusion copolymerization film of ester, but its production prices is high, and due to non-porous, the dampness of film resist it is bigger than normal, it is airtight；3)
PTFE films are polytetrafluoroethylene (PTFE) through function film that micro-pore diameter formed by stretch processes is 0.14 μm or so.
But above-mentioned conventional waterproof breathable membrane is on the one hand because the arrangement of micropore is disordering so that existing film
Permeability is poor, while being limited to prepare the performance limitation of material, its ductility is also poor.
The content of the invention
Therefore, the technical problems to be solved by the invention are to provide a kind of honeycomb structure micropore waterproof breathable membrane, with
The problem of solving waterproof breathable membrane gas permeability in the prior art and poor ductility.
In order to solve the above technical problems, a kind of film liquid composition for preparing the saturating film of waterproof of the present invention, including matter
Amount is than being 10-20：2-5：40-60 modified poly ethylene, ionic liquid and film forming solvent.
It is preferred that, the mass ratio of the modified poly ethylene, ionic liquid and film forming solvent is 15：3：50.
More excellent, the modified poly ethylene is made by the component modification of following parts by weight：
The parts by weight are g/mL in the proportionate relationship of parts by volume.
More excellent, the modified poly ethylene is made by the component modification of following parts by weight：
Particularly, the modified poly ethylene is prepared by the following method：
(1) under normal temperature, a selected amount of polyethylene is taken to be dissolved in ethanol solution, and add 1,2- phthalic acids list [2- [(1- oxygen
Generation -2- acrylic) oxygen] ethyl] ester, polyethylene terephthalate and carbonyl dimidazoles mixing；
(2) 40-50 DEG C is warming up to, chitosan is added to by gained mixture, is sufficiently stirred for mixing, and Temperature fall；
(3) a selected amount of cellulase is added into the mixture after cooling to mix；
(4) add a selected amount of cyclohexanone to mix, discharge, produce after vacuum drying.
The ionic liquid is amino acid ion liquid or glyoxaline ion liquid：The amino acid ion liquid is selected from L-
Proline ionic liquid and/or L-phenylalanine ionic liquid；The glyoxaline ion liquid is selected from 1- butyl -3- methylimidazoles
Tetrafluoro boric acid and/or 1- butyl -3- methylimidazole chlorine.
The film forming solvent includes carbon disulfide, chloroform, dichloromethane or toluene.
The material of the substrate is one kind in glass, silicon chip, polyester film.
The invention also discloses a kind of honeycomb structure micropore waterproof breathable membrane, it is made by the film liquid composition film forming,
It is in orderly honeycomb arrangement between the micropore of the film.
The film formation step is water droplet template or water assisted self assembling method.
The invention also discloses a kind of method for preparing described honeycomb structure micropore waterproof breathable membrane, including following step
Suddenly：
(a) take the modified poly ethylene to be dissolved in the film forming solvent, and add the ionic liquid and mix, polymerize
Thing solution；
(b) resulting polymers solution is coated in the substrate surface of cleaning, it is the normal of 60%-90% to be positioned over relative humidity
In warm atmospheric environment, 1-4min is stood, the waterproof breathable membrane with honeycomb structure is made after solvent volatilizees completely；Or
Person,
(b) substrate surface in cleaning is added dropwise in resulting polymers solution, the ultrasonic wave using frequency of oscillation 1.7MHz adds
Wet device ultrasonic atomizatio microlayer model, by microlayer model air-flow guides to surface, flow is 20mL/ using the rubber tube that internal diameter is 2cm
S, and sprayed by jet hole, jet hole is placed in vertically downward above substrate center at 5cm；Jet hole sprays in superjacent
Time is 20s, and jet hole is removed afterwards, until solvent and microlayer model volatilize completely, it is formable go out cellular microporous membrane.
Micropore waterproof breathable membrane of the present invention, using specially designed modified poly ethylene as base-material, is aided with ionic liquid
Modifying function, the obtained waterproof breathable membrane with honeycomb structure, its in waterproof and permeability have preferably it is excellent
Gesture.And obtained film is modified then better than with general ion liquid modified obtained film with amino acid ion liquid.
Film of the present invention is using the obtained film with honeycomb of method known in the art, and it is anti-
Compared to general random microporous membrane on water, permeability, its performance has certain advantage.
Brief description of the drawings
In order that present disclosure is more likely to be clearly understood, specific embodiment and combination below according to the present invention
Accompanying drawing, the present invention is further detailed explanation, wherein,
Fig. 1 is the simulation drawing of microcellular structure shown in the Electronic Speculum of embodiment 1.
Embodiment
The preparation of the modified poly ethylene of embodiment 1
Modified poly ethylene described in the present embodiment is made by the component modification of following parts by weight：
Modified poly ethylene is prepared by the following method described in the present embodiment：
(1) under normal temperature, a selected amount of polyethylene is taken to be dissolved in ethanol solution, and add 1,2- phthalic acids list [2- [(1- oxygen
Generation -2- acrylic) oxygen] ethyl] ester, polyethylene terephthalate and carbonyl dimidazoles mixing；
(2) 40-50 DEG C is warming up to, chitosan is added to by gained mixture, is sufficiently stirred for mixing, and Temperature fall；
(3) a selected amount of cellulase is added into the mixture after cooling to mix；
(4) add a selected amount of cyclohexanone to mix, discharge, produce after vacuum drying.
The preparation of the modified poly ethylene of embodiment 2
Modified poly ethylene described in the present embodiment is made by the component modification of following parts by weight：
The preparation method be the same as Example 1 of modified poly ethylene described in the present embodiment.
The preparation of the modified poly ethylene of embodiment 3
Modified poly ethylene described in the present embodiment is made by the component modification of following parts by weight：
The preparation method be the same as Example 1 of modified poly ethylene described in the present embodiment.
The preparation of the honeycomb structure micropore waterproof breathable membrane of embodiment 4
The film liquid composition of the saturating film of preparation waterproof described in the present embodiment, including modified poly ethylene prepared by embodiment 1
10kg, L-PROLINE ionic liquid 5kg, carbon disulfide 40kg.
The method that the present embodiment prepares described honeycomb structure micropore waterproof breathable membrane, according to water droplet mould in the prior art
Plate method is carried out, and be can refer to method disclosed in Chinese patent CN103937017A and is carried out, specifically includes following steps：
(a) take the modified poly ethylene to be dissolved in the film forming solvent, and add the ionic liquid and mix, polymerize
Thing solution；
(b) resulting polymers solution is coated in the mylar substrate surface of cleaning, relative humidity is positioned over for 60%-
In 90% normal temperature atmospheric environment, 1-4min is stood, the waterproof and breathable with honeycomb structure is made after solvent volatilizees completely
Film.
Detected through Electronic Speculum, in honeycomb arrangement, (Fig. 1 gives the microcellular structure of the waterproof breathable membrane made from the present embodiment
The simulation drawing of microcellular structure shown in the present embodiment Electronic Speculum is gone out).
The preparation of the honeycomb structure micropore waterproof breathable membrane of embodiment 5
The film liquid composition of the saturating film of preparation waterproof described in the present embodiment, including modified poly ethylene prepared by embodiment 2
20kg, L-phenylalanine ionic liquid 2kg, dichloromethane 60kg.
The method that the present embodiment prepares described honeycomb structure micropore waterproof breathable membrane, is aided according to prior art reclaimed water
Self-assembly method is carried out, and be can refer to the method disclosed in Chinese patent CN104211981A and is carried out, that is, comprises the following steps：
(a) take the modified poly ethylene to be dissolved in the film forming solvent, and add the ionic liquid and mix, polymerize
Thing solution；
Take glass substrate to be cleaned using cleanser, then rinsed well with deionized water, is put into glass container, held to glass
200ml-1000ml deionized water is added in device, then glass container is placed in supersonic cleaning machine, in power 700W-
The first pretreated substrate is obtained after being cleaned by ultrasonic 10min-20min under conditions of 1000W, working frequency 25KHz-40KHz；
First pretreated substrate is put into another glass container, adding 200ml-1000ml mass percent concentrations is
Glass container, is then placed in supersonic cleaning machine by 95% absolute ethyl alcohol, in power 700W-1000W, working frequency
The second pretreated substrate is obtained after being cleaned by ultrasonic 10min-20min under conditions of 25KHz-40KHz；
Second pretreated substrate is dried in 80 DEG C of -120 DEG C of environment of temperature and taken out after 10-30min, base must be both cleaned
Plate；
(b) substrate surface in cleaning is added dropwise in resulting polymers solution, the ultrasonic wave using frequency of oscillation 1.7MHz adds
Wet device ultrasonic atomizatio microlayer model, by microlayer model air-flow guides to surface, flow is 20mL/ using the rubber tube that internal diameter is 2cm
S, and sprayed by jet hole, jet hole is placed in vertically downward above substrate center at 5cm；Jet hole sprays in superjacent
Time is 20s, and jet hole is removed afterwards, until solvent and microlayer model volatilize completely, it is formable go out cellular microporous membrane.
Detected through Electronic Speculum, the microcellular structure of the waterproof breathable membrane made from the present embodiment is in honeycomb arrangement.
The preparation of the honeycomb structure micropore waterproof breathable membrane of embodiment 6
The film liquid composition of the saturating film of preparation waterproof described in the present embodiment, including modified poly ethylene prepared by embodiment 3
15kg, L-phenylalanine ionic liquid 3kg, carbon disulfide 50kg.
The present embodiment prepares the method be the same as Example 4 of described honeycomb structure micropore waterproof breathable membrane.
The preparation of the honeycomb structure micropore waterproof breathable membrane of embodiment 7
The film liquid composition of the saturating film of preparation waterproof described in the present embodiment, including modified poly ethylene prepared by embodiment 3
15kg, 1- butyl -3- methylimidazole tetrafluoro boric acid ionic liquids 3kg, dichloromethane 50kg.
The present embodiment prepares the method be the same as Example 5 of described honeycomb structure micropore waterproof breathable membrane.
The preparation of the honeycomb structure micropore waterproof breathable membrane of embodiment 8
The film liquid composition of the saturating film of preparation waterproof described in the present embodiment, including modified poly ethylene prepared by embodiment 3
15kg, 1- butyl -3- methylimidazole chloride ion liquids 3kg, carbon disulfide 50kg.
The present embodiment prepares the method be the same as Example 4 of described honeycomb structure micropore waterproof breathable membrane.
Comparative example 1
Honeycomb structure micropore waterproof breathable membrane described in this comparative example, its film liquid composition is same as Example 6, its area
It is not only that, the modified poly ethylene is polyethylene.
Comparative example 2
Honeycomb structure micropore waterproof breathable membrane described in this comparative example, its film liquid composition is same as Example 6, its area
It is not only that, does not contain the ionic liquid.
Comparative example 3
Honeycomb structure micropore waterproof breathable membrane described in this comparative example, its film liquid composition is identical with comparative example 1, its area
It is not only that, does not contain the ionic liquid.
Comparative example 4
Micropore waterproof breathable membrane described in this comparative example, its film liquid composition is same as Example 6, and it is differed only in
It is to use and general irregular microporous membrane made from general extension drawing process.
Experimental example
Above-described embodiment 4-8 and comparative example are detected according to national standard GB/T 5453-1997, GB/T 4757-1997 Plays
The performance of obtained film in 1-3, including Air permenbility (cm3/cm2 ﹒ s), vapor transfer rate (g/m2 ﹒ d) water pressure resistance (static state/m water columns),
Tensile strength (MPa), is recorded in table 1 below.
Table 1
| Numbering | Air permenbility | Vapor transfer rate | Water pressure resistance | Tensile strength |
| Embodiment 4 | 0.81 | 6539 | 7.6 | 8.1 |
| Embodiment 5 | 0.82 | 6552 | 7.6 | 8.2 |
| Embodiment 6 | 0.85 | 6670 | 7.7 | 8.5 |
| Embodiment 7 | 0.73 | 6324 | 7.3 | 7.6 |
| Embodiment 8 | 0.75 | 6312 | 7.3 | 7.4 |
| Comparative example 1 | 0.62 | 5552 | 7.0 | 6.0 |
| Comparative example 2 | 0.67 | 5580 | 6.9 | 6.3 |
| Comparative example 3 | 0.61 | 5547 | 6.8 | 5.8 |
| Comparative example 4 | 0.69 | 5500 | 6.8 | 6.2 |
It was found from upper table data, micropore waterproof breathable membrane of the present invention, using specially designed modified poly ethylene as base
Material, is aided with the modifying function of ionic liquid, the obtained waterproof breathable membrane with honeycomb structure, and it is in waterproof and permeability
It is upper that there is more preferable advantage.
It was found from above-described embodiment 5-8 and comparative example 1-3 data, the film-forming composition of film of the present invention, individually
Add ion liquid modified using modified poly ethylene as raw material or individually, the performance improvement to gained film is not obvious, only two
Under person's synergy so that the waterproof and breathable performance of film of the present invention is substantially improved.
It was found from the data of above-described embodiment 4-8 and comparative example 4, film of the present invention utilizes side known in the art
The obtained film with honeycomb of method, it is in waterproof, permeability compared to general random microporous membrane, its property
There can be certain advantage.
Obviously, above-described embodiment is only intended to clearly illustrate example, and the not restriction to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (10)
1. a kind of film liquid composition for preparing the saturating film of waterproof, it is characterised in that including mass ratio be 10-20：2-5：40-60's
Modified poly ethylene, ionic liquid and film forming solvent.
2. the film liquid composition of the saturating film of waterproof according to claim 1, it is characterised in that the modified poly ethylene, from
The mass ratio of sub- liquid and film forming solvent is 15：3：50.
3. the film liquid composition of the saturating film of waterproof according to claim 1 or 2, it is characterised in that the modified poly ethylene
It is made by the component modification of following parts by weight：
4. the film liquid composition of the saturating film of waterproof according to claim 3, it is characterised in that the modified poly ethylene is by such as
The component modification of lower parts by weight is made：
5. the film liquid composition of the saturating film of waterproof according to claim 3 or 4, it is characterised in that the modified poly ethylene
Prepare by the following method：
(1) under normal temperature, a selected amount of polyethylene is taken to be dissolved in ethanol solution, and add 1,2- phthalic acids list [2- [(1- oxos -2-
Acrylic) oxygen] ethyl] ester, polyethylene terephthalate and carbonyl dimidazoles mixing；
(2) 40-50 DEG C is warming up to, chitosan is added to by gained mixture, is sufficiently stirred for mixing, and Temperature fall；
(3) a selected amount of cellulase is added into the mixture after cooling to mix；
(4) add a selected amount of cyclohexanone to mix, discharge, produce after vacuum drying.
6. the film liquid composition of the saturating film of waterproof according to claim any one of 1-5, it is characterised in that the ionic liquid
Body is amino acid ion liquid or glyoxaline ion liquid.
7. the film liquid composition of the saturating film of waterproof according to claim any one of 1-6, it is characterised in that the film forming is molten
Agent includes carbon disulfide, chloroform, dichloromethane or toluene.
8. a kind of honeycomb structure micropore waterproof breathable membrane, it is characterised in that combined by any one of the claim 1-7 film liquids
Thing film forming is made, and is in orderly honeycomb arrangement between the micropore of the film.
9. honeycomb structure micropore waterproof breathable membrane according to claim 8, it is characterised in that the film formation step is water
Drip template or water assisted self assembling method.
10. a kind of method of the honeycomb structure micropore waterproof breathable membrane prepared described in claim 8 or 9, it is characterised in that bag
Include following steps：
(a) take the modified poly ethylene to be dissolved in the film forming solvent, and add the ionic liquid and mix, obtain polymer molten
Liquid；
(b) resulting polymers solution is coated in the substrate surface of cleaning, the normal temperature that relative humidity is 60%-90% is positioned over big
In compression ring border, 1-4min is stood, the waterproof breathable membrane with honeycomb structure is made after solvent volatilizees completely；Or,
(b) substrate surface in cleaning is added dropwise in resulting polymers solution, uses frequency of oscillation 1.7MHz ultrasonic humidifier
Ultrasonic atomizatio microlayer model, by microlayer model air-flow guides to surface, flow is 20mL/s using the rubber tube that internal diameter is 2cm, and
Sprayed, jet hole is placed in vertically downward above substrate center at 5cm by jet hole；Jet hole is in superjacent injecting time
Be 20s, jet hole removed afterwards, until solvent and microlayer model volatilize completely, it is formable go out cellular microporous membrane.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112662006A (en) * | 2020-12-07 | 2021-04-16 | 深圳技术大学 | Antibacterial waterproof breathable film and preparation method thereof |
| CN113773721A (en) * | 2021-09-18 | 2021-12-10 | 浙江润奥环保科技有限公司 | Silver ion antibacterial floor material and preparation method thereof |
-
2017
- 2017-04-26 CN CN201710280288.6A patent/CN106977796B/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112662006A (en) * | 2020-12-07 | 2021-04-16 | 深圳技术大学 | Antibacterial waterproof breathable film and preparation method thereof |
| CN113773721A (en) * | 2021-09-18 | 2021-12-10 | 浙江润奥环保科技有限公司 | Silver ion antibacterial floor material and preparation method thereof |
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