CN106633132A - SPEEK (sulfonated polyether ether ketone)-PVDF (polyvinylidene fluoride) gas regulating composite membrane, and preparation and application thereof - Google Patents
SPEEK (sulfonated polyether ether ketone)-PVDF (polyvinylidene fluoride) gas regulating composite membrane, and preparation and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- 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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
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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
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/16—Homopolymers or copolymers or vinylidene fluoride
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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
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/16—Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
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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
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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Abstract
The invention belongs to the technical field of membrane materials, and discloses an SPEEK (sulfonated polyether ether ketone)-PVDF (polyvinylidene fluoride) gas regulating composite membrane, and preparation and application thereof. A preparation method is characterized in that PEEK (polyether ether ketone) is added into a container; then, concentrated H2SO4 is added; heating and stirring are performed until the PEEK is completely dissolved; a claybank solution is obtained; the claybank solution is dripped into an ice and water mixture to form a white solid; the solid is washed and dried to obtain SPEEK; the SPEEK and PVDF are together dissolved into DMP (dimethyl phthalate) to obtain a casting membrane solution; then, the casting membrane solution is subjected to curtain coating on a flat plate to form a membrane; drying and membrane uncovering are performed to obtain the SPEEK-PVDF gas regulating composite membrane. The preparation method is simple; the membrane forming conditions are easy to control; the obtained SPEEK-PVDF gas regulating composite membrane has an obvious inhibiting effect on fruit and vegetable breathing, and can be applied to fruit and vegetable gas regulation fresh keeping.
Description
Technical field
The invention belongs to technology field of membrane materials, and in particular to a kind of SPEEK-PVDF gas regulations composite membrane and prepare with
Using.
Background technology
Fresh fruit of vegetables preservation and freshness is an important topic in field of food.Fresh fruit of vegetables is must in people's life
Few food, but its tissue water content is high, and easily putrid and deteriorated, normal temperature storage life is short, there is very strong seasonality in production, variable
Property, the shortcomings of regional.It is increasing with regard to the research of postharvest technology of fruits and vegetables both at home and abroad, and research direction gradually to materialogy,
The numerous areas such as Food Chemistry, organic chemistry, biology, mechanical engineering develop.Preservation technique main at this stage has fresh-keeping
Film, refrigeration, sterilization, irradiation etc., air-conditioning preservative film is practical because simple to operate, low cost and of good preservation effect, becomes fruits and vegetables storage
Hide fresh-keeping prefered method.
Fruit and vegetable air-conditioning preservation technology is referred under uniform temperature and damp condition, by the gas composition for controlling storage environment
To reach the method for keeping fruit-vegetable quality, extending the storage fruit and vegetable phase.Packaging membrane material is the basis of controlled atmosphere fresh-keeping packing, is protected
Fresh film leaves some apertures according to molecular diameter size during making on film, controls different size of gas molecule and leads to
Cross, Main Function is that the gas for being unfavorable for preserving fruit and vegetable utilizing inside preservative film is discharged into outside, and some are conducive to into fresh-keeping gas
Remain in preservative film, control the oxygen and carbon dioxide inside preservative film, so as to reduce fruits and vegetables respiration, reduce nutrition and disappear
Consumption, reaches fresh-keeping effect.Controlled atmospheric packing has higher requirement to the performance and kind of packing membrane material, does not also obtain extensively in China
General application.
The key of membrane technology is membrane material, and conventional membrane material has polyether-ether-ketone (PEEK), Kynoar (PVDF), vinegar
Acid cellulose (CA), polysulfones (PS), polyether sulfone (PES) etc..Polyether-ether-ketone (PEEK) is aromatic series crystalline thermoplastic polymer,
It is a kind of high-performance engineering special plastic, it has high-fire resistance, radiation hardness, chemical-resistant resistance, excellent in cushion effect, wearability
The features such as, excellent electrical property good, fire-retardant with fatigue durability.Additionally, another material Kynoar (PVDF) is also a kind of
The engineering plastics of high comprehensive performance, it has excellent heat endurance and chemical stability, corrosion resistance be strong, resistance to ag(e)ing
By force, the features such as low-friction coefficient, high mechanical strength and easy film forming.PEEK and PVDF is because with excellent performance, curing
The fields such as treatment, the energy, aviation and food become requisite important materials, but due to stable in properties, the indissoluble of PEEK
In nearly all solvent, and its fusing point is high, it is difficult to process film forming, therefore, single PEEK as membrane material, its application be subject to compared with
Big restriction.
The content of the invention
In order to solve the shortcoming and defect part of above prior art, the primary and foremost purpose of the present invention is to provide a kind of
The preparation method of SPEEK-PVDF gas regulation composite membranes.
Another object of the present invention is to provide a kind of SPEEK-PVDF gas regulations prepared by said method
Composite membrane.
It is still another object of the present invention to provide above-mentioned SPEEK-PVDF gas regulations composite membrane is in fruit and vegetable air-conditioning preservation
Application.
The object of the invention is achieved through the following technical solutions：
A kind of preparation method of SPEEK-PVDF gas regulations composite membrane, including following preparation process：
(1) in polyether-ether-ketone (PEEK) being added to into container, it is subsequently adding dense H2SO4, heating stirring to PEEK is completely molten
Solution, obtains brown yellow solution, and gained brown yellow solution is added drop-wise in mixture of ice and water, forms white solid state thing, solid Jing
Wash, be dried, obtain sulfonated polyether-ether-ketone (SPEEK).
(2) sulfonated polyether-ether-ketone (SPEEK) and Kynoar (PVDF) are dissolved in into together N,N-dimethylformamide
(DMF) in, casting solution is obtained, film is taken off in then casting film-forming, the drying on flat board by casting solution, obtains the SPEEK-PVDF
Gas regulation composite membrane.
Preferably, the washing described in step (1) refers to that it is neutrality to be washed with deionized to cleaning solution pH；Described drying
Refer to and be dried 24h at 60 DEG C.
Preferably, the mass ratio that SPEEK described in step (2) and PVDF is added is 1:1～1:3；In the casting solution
SPEEK and PVDF total mass concentration is 5%～15%.
Preferably, the casting solution described in step (2) is removing insoluble matter using front first Jing centrifugations.
Preferably, described flat board refers to glass plate, the glass plate first being cleaned with purificant using front, by
Diluted acid is rinsed, then with soaked in absolute ethyl alcohol, finally clean with ultrapure water, dry for standby.
Preferably, the drying described in step (2) refers to and 8～12h is dried at 60～80 DEG C.
Described in step (2) take off film refer to immersion deionized water in carry out taking off film.
A kind of SPEEK-PVDF gas regulations composite membrane, is prepared by said method, gained SPEEK-PVDF gases
The thickness for adjusting composite membrane is 17～24 μm.
Application of the above-mentioned SPEEK-PVDF gas regulations composite membrane in fruit and vegetable air-conditioning preservation.
The present invention principle be：By being grafted sulfo group in PEEK molecules, sulfonated polyether-ether-ketone (SPEEK) is prepared,
SPEEK not only has the good characteristic similar to PEEK, and SPEEK is soluble in the common organic solvents such as DMF, DMAc
In；Obtained SPEEK is combined PVDF, with DMF (DMF) as solvent, using solution evaporation method SPEEK- is prepared
PVDF gas regulation composite membranes.By controlling the film forming conditions such as solvent, casting solution concentration, drying temperature, masking mode, Yi Jigen
According to the stalling characteristic of controlled atmosphere film, the selective ventilated membrane for being adapted to fruit and vegetable air-conditioning preservation is obtained.
The preparation method and resulting product of the present invention has the advantage that and beneficial effect：
(1) present invention gained SPEEK-PVDF gas regulations composite film thickness is 17～24 μm, compound with SPEEK-PVDF
Film preserves fruits and vegetables, the CO of its final state2Concentration level be dropped by nearly half, the breathing to fruits and vegetables has obvious inhibitory action, can answer
With with fruit and vegetable air-conditioning preservation；
(2) present invention forms size uneven using DMF (DMF) as solvent by solvent evaporation method
One aperture, makes composite membrane have good asymmetric gas regulatory function, and its preparation method is simple, and membrance casting condition is easy to control
System, with good industrial applications prospect.
Description of the drawings
Fig. 1 and Fig. 2 are respectively the whole of Example 1 and Example 2 of the present invention gained SPEEK-PVDF gas regulation composite membranes
Body shape appearance figure；
Fig. 3 and Fig. 4 are respectively the surface electron-microscope scanning of the gained SPEEK-PVDF gas regulation composite membranes of the embodiment of the present invention 2
Figure and section electron-microscope scanning figure；
Fig. 5 is that respiratory intensity of the fresh Brassica rapa L under SPEEK-PVDF gas regulations composite membrane parcel obtained by the present invention is surveyed
Determine result figure.
Specific embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited
In this.
Embodiment 1
(1) 10g polyether-ether-ketones (PEEK) brown cylindrical particles are accurately weighed to be put in flask, 200mL 98% is poured slowly into
Dense H2SO4, it is placed in the heating of thermostat water bath mechanical agitation.Stir 7h to PEEK under the conditions of 60 DEG C, 300r/min to be completely dissolved,
Obtain brown yellow solution.Above-mentioned brown yellow solution is slowly dropped in a large amount of mixture of ice and water, white solid state thing is formed, then is used
Deionized water is repeatedly washed, until cleaning solution pH close 7.The polymer of washing is dried into 24h at 60 DEG C of baking oven, product is obtained
Sulfonated polyether-ether-ketone (SPEEK).
(2) 2g sulfonated polyether-ether-ketones (SPEEK) and 2g Kynoar (PVDF) solid are accurately weighed, is put into ready
In 100ml beakers, 50mL DMFs (DMF) are poured slowly into, are placed in constant temperature blender with magnetic force stirring, be maintained at
60 DEG C, stir under the conditions of 500r/min, obtain dissolving thick liquid.The thick liquid of upper step is sub-packed in centrifuge tube, in 5000r/
The step of 5min, repeated centrifugation are centrifuged under min rotating speeds 2～3 times, takes supernatant and is casting solution.Flat glass first uses detergent
Cleaning, the rinsing of rear diluted acid, then with soaked in absolute ethyl alcohol a few hours after, finally rinsed well with pure water.By appropriate casting solution
It is poured on glass pane surface and is cast into film liquid in uniform thickness, be steadily put into decompression drying in baking oven, 12h is dried at 60 DEG C, takes out,
Immerse in deionized water after natural cooling, take off film, dry at room temperature, preserve, obtain the SPEEK-PVDF gas regulations
Composite membrane.
The overall shape appearance figure of the present embodiment gained SPEEK-PVDF gas regulation composite membranes is as shown in Figure 1.Gained SPEEK-
The thickness of PVDF gas regulation composite membranes is 21 μm.
Embodiment 2
(1) 10g polyether-ether-ketones (PEEK) brown cylindrical particles are accurately weighed to be put in flask, 200mL 98% is poured slowly into
Dense H2SO4, it is placed in the heating of thermostat water bath mechanical agitation.Stir 7h to PEEK under the conditions of 60 DEG C, 300r/min to be completely dissolved,
Obtain brown yellow solution.Above-mentioned brown yellow solution is slowly dropped in a large amount of mixture of ice and water, white solid state thing is formed, then is used
Deionized water is repeatedly washed, until cleaning solution pH close 7.The polymer of washing is dried into 24h at 60 DEG C of baking oven, product is obtained
Sulfonated polyether-ether-ketone (SPEEK).
(2) 1g sulfonated polyether-ether-ketones (SPEEK) and 3g Kynoar (PVDF) solid are accurately weighed, is put into ready
In 100ml beakers, 50mL DMFs (DMF) are poured slowly into, are placed in constant temperature blender with magnetic force stirring, be maintained at
60 DEG C, stir under the conditions of 500r/min, obtain dissolving thick liquid.The thick liquid of upper step is sub-packed in centrifuge tube, in 5000r/
The step of 5min, repeated centrifugation are centrifuged under min rotating speeds 2～3 times, takes supernatant and is casting solution.Flat glass first uses detergent
Cleaning, the rinsing of rear diluted acid, then with soaked in absolute ethyl alcohol a few hours after, finally rinsed well with pure water.By appropriate casting solution
It is poured on glass pane surface and is cast into film liquid in uniform thickness, be steadily put into decompression drying in baking oven, 8h is dried at 80 DEG C, takes out,
Immerse in deionized water after natural cooling, take off film, dry at room temperature, preserve, obtain the SPEEK-PVDF gas regulations
Composite membrane.
The overall shape appearance figure of the present embodiment gained SPEEK-PVDF gas regulation composite membranes is as shown in Figure 2.Gained SPEEK-
The thickness of PVDF gas regulation composite membranes is 20 μm.
Product structure is characterized and application performance test：
(1) Electronic Speculum pretreatment is scanned to the gained SPEEK-PVDF gas regulation composite membranes of embodiment 2, sample presentation analysis is surveyed
ESEM is done at examination center, obtains surface electron-microscope scanning figure and section electron-microscope scanning figure is distinguished as shown in Figure 3 and Figure 4.By Fig. 3
Observed with Fig. 4, SPEEK-PVDF composite film surfaces are made up of loose and irregular granular molecule, section electron microscope is presented
Go out cellular or spongiform structure, be evenly distributed on inside composite film material with a large amount of bubbles.Take this as a foundation, can be with
All there is the hole of micron level in the surface and inside for proving SPEEK-PVDF composite membranes so that different size of gas molecule
Permeation composite membrane is free to, realizes that the controlled atmosphere to fruits and vegetables is acted on this.
(2) controlled atmosphere effect propety test is carried out to the gained SPEEK-PVDF gas regulations composite membrane of embodiment 1 and 2：
Unabroken fresh Brassica rapa L (about 100g) one is taken, is weighed, be placed in 3051H type fruits and vegetables respirometer respiratory chambers
In, the gained SPEEK-PVDF gas regulation composite membranes of embodiment 1 and 2 are covered respectively in respiratory chamber upper end, it is ensured that composite membrane can
Respiratory chamber upper end is covered, and whole respiratory chamber is muffled with black cloth, to prevent green vegetable from carrying out photosynthesis to experiment knot
Fruit produces impact.Setting control group：SPEEK-PVDF gas regulations composite membrane is replaced with common gas tight seal lid, other realities
Test that condition is constant, determine the CO of different time sections under the same conditions2Concentration, as a result as shown in Figure 5.As seen from Figure 5, newly
Respiration of the fresh Brassica rapa L through about 3 hours, it is left that the concentration of control group closure equilibrium carbon dioxide has reached 4600ppm
The right side, 1:The concentration of equilibrium carbon dioxide reaches 3800ppm or so in the presence of the compound air-conditioning preservative films of 1 SPEEK-PVDF,
1:The concentration of equilibrium carbon dioxide reaches 4300ppm or so in the presence of the compound air-conditioning preservative films of 3 SPEEK-PVDF, therefore
Component ratio is 1:SPEEK-PVDF composite membrane controlled atmosphere abilities when 1 are 1 than component ratio:Composite membrane when 3 is significantly stronger, tool
There is excellent controlled atmosphere effect.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention not by above-described embodiment
Limit, other any Spirit Essences and the changes, modification, replacement made under principle without departing from the present invention, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of SPEEK-PVDF gas regulations composite membrane, it is characterised in that including following preparation process：
(1) PEEK is added in container, is subsequently adding dense H2SO4, heating stirring to PEEK is completely dissolved, and obtains brown color molten
Liquid, gained brown yellow solution is added drop-wise in mixture of ice and water, forms white solid state thing, and solid is scrubbed, dry, obtains
SPEEK；
(2) SPEEK and PVDF are dissolved in together in DMF, obtain casting solution, then by casting solution on flat board casting film-forming, do
It is dry, film is taken off, obtain the SPEEK-PVDF gas regulations composite membrane.
2. the preparation method of a kind of SPEEK-PVDF gas regulations composite membrane according to claim 1, it is characterised in that：Step
Suddenly the washing described in (1) refers to that it is neutrality to be washed with deionized to cleaning solution pH；Described drying is referred to and is dried at 60 DEG C
24h。
3. the preparation method of a kind of SPEEK-PVDF gas regulations composite membrane according to claim 1, it is characterised in that：Step
Suddenly the mass ratio that SPEEK described in (2) and PVDF is added is 1:1～1:3；SPEEK and PVDF total quality in the casting solution
Concentration is 5%～15%.
4. the preparation method of a kind of SPEEK-PVDF gas regulations composite membrane according to claim 1, it is characterised in that：Step
Suddenly the casting solution described in (2) is removing insoluble matter using front first Jing centrifugations.
5. the preparation method of a kind of SPEEK-PVDF gas regulations composite membrane according to claim 1, it is characterised in that：Institute
The flat board stated refers to glass plate, and the glass plate is first being cleaned using front with purificant, is rinsed by diluted acid, then with anhydrous
Ethanol soaks, finally clean with ultrapure water, dry for standby.
6. the preparation method of a kind of SPEEK-PVDF gas regulations composite membrane according to claim 1, it is characterised in that：Step
Suddenly the drying described in (2) refers to and 8～12h is dried at 60～80 DEG C.
7. the preparation method of a kind of SPEEK-PVDF gas regulations composite membrane according to claim 1, it is characterised in that：Step
Suddenly described in (2) take off film refer to immersion deionized water in carry out taking off film.
8. a kind of SPEEK-PVDF gas regulations composite membrane, it is characterised in that：By the side described in any one of claim 1～7
Method is prepared, and the thickness of gained SPEEK-PVDF gas regulation composite membranes is 17～24 μm.
9. application of the SPEEK-PVDF gas regulation composite membranes described in claim 8 in fruit and vegetable air-conditioning preservation.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112841299A (en) * | 2021-01-21 | 2021-05-28 | 华南理工大学 | Spontaneous gas dormancy preservation method for instant sweet corn |
| CN114749040A (en) * | 2022-03-03 | 2022-07-15 | 华南理工大学 | SPEEK/PEG/PVDF gas regulation composite membrane, preparation and application thereof |
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| CN101766958A (en) * | 2009-01-05 | 2010-07-07 | 厦门城市环境研究所 | Method for preparing porous membrane with intestine imitating structure |
| CN101785976A (en) * | 2009-11-13 | 2010-07-28 | 山东东岳高分子材料有限公司 | Polymer separation membrane with on-line antibiosis and self-cleaning functions and preparation method thereof |
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2016
- 2016-12-02 CN CN201611095285.7A patent/CN106633132B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101766958A (en) * | 2009-01-05 | 2010-07-07 | 厦门城市环境研究所 | Method for preparing porous membrane with intestine imitating structure |
| CN101785976A (en) * | 2009-11-13 | 2010-07-28 | 山东东岳高分子材料有限公司 | Polymer separation membrane with on-line antibiosis and self-cleaning functions and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112841299A (en) * | 2021-01-21 | 2021-05-28 | 华南理工大学 | Spontaneous gas dormancy preservation method for instant sweet corn |
| CN114749040A (en) * | 2022-03-03 | 2022-07-15 | 华南理工大学 | SPEEK/PEG/PVDF gas regulation composite membrane, preparation and application thereof |
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