CN106633132B - A kind of SPEEK-PVDF gas regulation composite membrane and preparation and application - Google Patents
A kind of SPEEK-PVDF gas regulation composite membrane and preparation and application Download PDFInfo
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- CN106633132B CN106633132B CN201611095285.7A CN201611095285A CN106633132B CN 106633132 B CN106633132 B CN 106633132B CN 201611095285 A CN201611095285 A CN 201611095285A CN 106633132 B CN106633132 B CN 106633132B
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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
-
- 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
Abstract
The invention belongs to technology field of membrane materials, a kind of SPEEK-PVDF gas regulation composite membrane and preparation and application are disclosed.The preparation method is that: PEEK is added in container, dense H is then added2SO4, heating stirring to PEEK is completely dissolved, obtains brown yellow solution, gained brown yellow solution is added drop-wise in mixture of ice and water, forms white solid state object, and solid is washed, dry, obtains SPEEK；SPEEK and PVDF are dissolved in DMF together, obtain casting solution, then casting film-forming, drying take off film, obtain the SPEEK-PVDF gas regulation composite membrane on plate by casting solution.Preparation method of the invention is simple, and membrance casting condition is easily controllable, and gained SPEEK-PVDF gas regulation composite membrane has apparent inhibiting effect to the breathing of fruits and vegetables, can apply and fruit and vegetable air-conditioning preservation.
Description
Technical field
The invention belongs to technology field of membrane materials, and in particular to a kind of SPEEK-PVDF gas regulation composite membrane and preparation with
Using.
Background technique
Fresh fruit of vegetables preservation and freshness is an important topic in field of food.Fresh fruit of vegetables is must can not in people's life
Few food, but its tissue water content is high, easily putrid and deteriorated, it is short to be stored at room temperature the phase, there is very strong seasonality in production, variable
Property, it is regional the disadvantages of.It is increasing about the research of postharvest technology of fruits and vegetables both at home and abroad, and research direction gradually to materialogy,
The development of the numerous areas such as Food Chemistry, organic chemistry, biology, mechanical engineering.Main preservation technology has fresh-keeping at this stage
Film, refrigeration, sterilization, irradiation etc., air-conditioning preservative film is practical because easy to operate, at low cost and of good preservation effect, becomes fruits and vegetables storage
Hide fresh-keeping prefered method.
Fruit and vegetable air-conditioning preservation technology refers under certain 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
According to molecular diameter size, there are some apertures on film during production for fresh film, and it is logical to control different size of gas molecule
It crosses, main function is the gas discharge outside that will be unfavorable for preserving fruit and vegetable utilizing inside preservative film, is conducive to fresh-keeping gas for some
It remains in preservative film, controls the oxygen and carbon dioxide inside preservative film, 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 packaging membrane material, does not obtain also extensively in China
General application.
The key of membrane technology is membrane material, and common 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
With the features such as fatigue durability is good, fire-retardant, excellent electrical property.In addition, another material Kynoar (PVDF) is also one kind
The engineering plastics of high comprehensive performance, it has, and excellent thermal stability 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 being cured because having excellent performance
The fields such as treatment, the energy, aviation and food become essential important materials, but since the property of PEEK is stablized, indissoluble
In nearly all solvent, and its fusing point is high, it is difficult to processing film forming, therefore, single PEEK is used as membrane material, apply by compared with
Big limitation.
Summary of the invention
In order to solve the disadvantage that the above prior art and shortcoming, the primary purpose of the present invention is that providing one kind
The preparation method of SPEEK-PVDF gas regulation composite membrane.
Another object of the present invention is to provide a kind of SPEEK-PVDF gas regulations being prepared by the above method
Composite membrane.
A further object of the present invention is to provide above-mentioned SPEEK-PVDF gas regulation composite membranes 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 regulation composite membrane, including following preparation step:
(1) polyether-ether-ketone (PEEK) is added in container, dense H is then added2SO4, heating stirring is completely molten to PEEK
Solution, obtains brown yellow solution, gained brown yellow solution is added drop-wise in mixture of ice and water, forms white solid state object, solid warp
Washing, drying, obtain sulfonated polyether-ether-ketone (SPEEK).
(2) sulfonated polyether-ether-ketone (SPEEK) and Kynoar (PVDF) are dissolved in N,N-dimethylformamide together
(DMF) in, casting solution is obtained, then casting film-forming, drying take off film, obtain the SPEEK-PVDF on plate by casting solution
Gas regulation composite membrane.
Preferably, washing described in step (1) refers to that being washed with deionized to cleaning solution pH is neutrality；The drying
Refer to that drying is for 24 hours 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, casting solution described in step (2) is first removing insoluble matter through centrifugation using preceding.
Preferably, the plate refers to that glass plate, the glass plate are first cleaned with purificant using preceding, by
Diluted acid rinsing, then with soaked in absolute ethyl alcohol, it is finally clean with ultrapure water, it is dried for standby.
Preferably, drying described in step (2) refers to dry 8~12h at 60~80 DEG C.
Taken off described in step (2) film refer to immerse deionized water in carry out taking off film.
A kind of SPEEK-PVDF gas regulation composite membrane, is prepared by the above method, gained SPEEK-PVDF gas
Adjust composite membrane with a thickness of 17~24 μm.
Application of the above-mentioned SPEEK-PVDF gas regulation composite membrane in fruit and vegetable air-conditioning preservation.
The principle of the present invention are as follows: by being grafted sulfo group in PEEK molecule, sulfonated polyether-ether-ketone (SPEEK) is prepared,
SPEEK not only has the good characteristic similar to PEEK, but also SPEEK is soluble in the common organic solvents such as DMF, DMAc
In；The compound PVDF of SPEEK obtained prepares SPEEK- using solution evaporation method with n,N-Dimethylformamide (DMF) for solvent
PVDF gas regulation composite membrane.Pass through the film forming conditions such as control solvent, casting solution concentration, drying temperature, film mode, Yi Jigen
According to the stalling characteristic of controlled atmosphere film, the selective ventilated membrane for being suitble to fruit and vegetable air-conditioning preservation is obtained.
Preparation method of the invention and obtained product have the following advantages that and the utility model has the advantages that
(1) present invention gained SPEEK-PVDF gas regulation composite film thickness is 17~24 μm, compound with SPEEK-PVDF
Film saves fruits and vegetables, the CO of final state2Concentration level be dropped by nearly half, have apparent inhibiting effect to the breathing of fruits and vegetables, can answer
With with fruit and vegetable air-conditioning preservation；
(2) present invention is used as solvent using n,N-Dimethylformamide (DMF), and it is uneven to form size by solvent evaporation method
One aperture makes composite membrane have good asymmetric gas regulatory function, and preparation method is simple, and membrance casting condition is easy to control
System has good industrial applications prospect.
Detailed description of the invention
Fig. 1 and Fig. 2 is respectively the whole of SPEEK-PVDF gas regulation composite membrane obtained by Example 1 and Example 2 of the present invention
Body shape appearance figure；
Fig. 3 and Fig. 4 is respectively the surface electron-microscope scanning of 2 gained SPEEK-PVDF gas regulation composite membrane of the embodiment of the present invention
Figure and section electron-microscope scanning figure；
Fig. 5 is that the respiratory intensity under fresh Brassica rapa L SPEEK-PVDF gas regulation composite membrane obtained by present invention package is surveyed
Determine result figure.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) 10g polyether-ether-ketone (PEEK) brown cylindrical particles are accurately weighed to be put into flask, are poured slowly into 200mL 98%
Dense H2SO4, it is placed in the heating of thermostat water bath mechanical stirring.7h to PEEK is stirred 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, forms white solid state object, then use
Deionized water is repeatedly washed, until cleaning solution pH is close to 7.By the polymer of washing, drying for 24 hours, obtains product at 60 DEG C of baking oven
Sulfonated polyether-ether-ketone (SPEEK).
(2) 2g sulfonated polyether-ether-ketone (SPEEK) and 2g Kynoar (PVDF) solid are accurately weighed, is put into ready
In 100ml beaker, it is poured slowly into 50mL n,N-Dimethylformamide (DMF), constant temperature blender with magnetic force stirring is placed in, is maintained at
60 DEG C, stir evenly under the conditions of 500r/min, obtain dissolution crude liquid.Upper step crude liquid is sub-packed in centrifuge tube, in 5000r/
5min is centrifuged under min revolving speed, step 2~3 time of repeated centrifugation, taking supernatant is casting solution.Flat glass first uses detergent
Cleaning, rear diluted acid rinsing, then with after soaked in absolute ethyl alcohol a few hours, finally rinsed well with pure water.By suitable casting solution
It being poured on glass pane surface and is cast into film liquid in homogeneous thickness, be steadily put into decompression drying in baking oven, dry 12h at 60 DEG C takes out,
It is immersed in deionized water after natural cooling, takes off film, dry at room temperature, saved, obtain the SPEEK-PVDF gas regulation
Composite membrane.
The whole shape appearance figure of SPEEK-PVDF gas regulation composite membrane obtained by the present embodiment is as shown in Figure 1.Gained SPEEK-
PVDF gas regulation composite membrane with a thickness of 21 μm.
Embodiment 2
(1) 10g polyether-ether-ketone (PEEK) brown cylindrical particles are accurately weighed to be put into flask, are poured slowly into 200mL 98%
Dense H2SO4, it is placed in the heating of thermostat water bath mechanical stirring.7h to PEEK is stirred 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, forms white solid state object, then use
Deionized water is repeatedly washed, until cleaning solution pH is close to 7.By the polymer of washing, drying for 24 hours, obtains product at 60 DEG C of baking oven
Sulfonated polyether-ether-ketone (SPEEK).
(2) 1g sulfonated polyether-ether-ketone (SPEEK) and 3g Kynoar (PVDF) solid are accurately weighed, is put into ready
In 100ml beaker, it is poured slowly into 50mL n,N-Dimethylformamide (DMF), constant temperature blender with magnetic force stirring is placed in, is maintained at
60 DEG C, stir evenly under the conditions of 500r/min, obtain dissolution crude liquid.Upper step crude liquid is sub-packed in centrifuge tube, in 5000r/
5min is centrifuged under min revolving speed, step 2~3 time of repeated centrifugation, taking supernatant is casting solution.Flat glass first uses detergent
Cleaning, rear diluted acid rinsing, then with after soaked in absolute ethyl alcohol a few hours, finally rinsed well with pure water.By suitable casting solution
It being poured on glass pane surface and is cast into film liquid in homogeneous thickness, be steadily put into decompression drying in baking oven, dry 8h at 80 DEG C takes out,
It is immersed in deionized water after natural cooling, takes off film, dry at room temperature, saved, obtain the SPEEK-PVDF gas regulation
Composite membrane.
The whole shape appearance figure of SPEEK-PVDF gas regulation composite membrane obtained by the present embodiment is as shown in Figure 2.Gained SPEEK-
PVDF gas regulation composite membrane with a thickness of 20 μm.
Product structure characterization and application performance test:
(1) Electronic Speculum pretreatment is scanned to 2 gained SPEEK-PVDF gas regulation composite membrane of embodiment, sample presentation analysis is surveyed
Scanning electron microscope is done at examination center, obtains surface electron-microscope scanning figure and section electron-microscope scanning figure difference is as shown in Figure 3 and Figure 4.Pass through Fig. 3
It is observed with Fig. 4, SPEEK-PVDF composite film surface is made of loose and out-of-flatness granular molecule, and section electron microscope is presented
There are a large amount of bubbles to be evenly distributed on inside composite film material for honeycomb or spongiform structure out.It takes this as a foundation, it can be with
The surface of proof SPEEK-PVDF composite membrane and the internal hole that all there is micron level, so that different size of gas molecule
It is free to permeation composite membrane, realized with this to the effect of the controlled atmospheres of fruits and vegetables.
(2) test of controlled atmosphere effect propety is carried out to SPEEK-PVDF gas regulation composite membrane obtained by Examples 1 and 2:
Unabroken fresh Brassica rapa L (about 100g) one is taken, weighs, is placed in 3051H type fruits and vegetables respirometer respiratory chamber
In, SPEEK-PVDF gas regulation composite membrane obtained by Examples 1 and 2 is covered respectively in respiratory chamber upper end, it is ensured that composite membrane can
Respiratory chamber upper end is covered, and entire respiratory chamber is muffled with black cloth, experiment is tied with preventing green vegetable from carrying out photosynthesis
Fruit has an impact.Setting control group: SPEEK-PVDF gas regulation composite membrane is replaced with common gas tight seal lid, other realities
It is constant to test condition, measures CO in different time periods under the same conditions2Concentration, as a result as shown in Figure 5.As seen from Figure 5, newly
For fresh Brassica rapa L by about 3 hours respirations, it is left that the concentration of control group sealing cover equilibrium carbon dioxide has reached 4600ppm
The right side, the concentration of equilibrium carbon dioxide reaches 3800ppm or so under the action of the SPEEK-PVDF of 1:1 compound air-conditioning preservative film,
The concentration of equilibrium carbon dioxide reaches 4300ppm or so under the action of the SPEEK-PVDF of 1:3 compound air-conditioning preservative film, therefore
Composite membrane when SPEEK-PVDF composite membrane controlled atmosphere ability when component ratio is 1:1 than component ratio is 1:3 is significantly stronger, tool
There is excellent controlled atmosphere effect.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (6)
1. a kind of preparation method of SPEEK-PVDF gas regulation composite membrane, it is characterised in that including following preparation step:
(1) PEEK is added in container, dense H is then added2SO4, heating stirring to PEEK is completely dissolved, and it is molten to obtain brown color
Gained brown yellow solution is added drop-wise in mixture of ice and water by liquid, forms white solid state object, and solid is washed, dry, obtains
SPEEK；
(2) SPEEK and PVDF are dissolved in DMF together, obtain casting solution, then by casting solution on plate casting film-forming, do
It is dry, film is taken off, the SPEEK-PVDF gas regulation composite membrane is obtained；
The mass ratio that SPEEK described in step (2) and PVDF is added is 1:1~1:3；SPEEK and PVDF are total in the casting solution
Mass concentration be 5%~15%；
The drying refers to dry 8~12h at 60~80 DEG C；It is described take off film and refer to immerse in deionized water taken off
Film.
2. a kind of preparation method of SPEEK-PVDF gas regulation composite membrane according to claim 1, it is characterised in that: step
Suddenly washing described in (1) refers to that being washed with deionized to cleaning solution pH is neutrality；The drying refers to dry at 60 DEG C
24h。
3. a kind of preparation method of SPEEK-PVDF gas regulation composite membrane according to claim 1, it is characterised in that: step
Suddenly casting solution described in (2) is first removing insoluble matter through centrifugation using preceding.
4. a kind of preparation method of SPEEK-PVDF gas regulation composite membrane according to claim 1, it is characterised in that: institute
The plate stated refers to glass plate, and the glass plate is first cleaned with purificant using preceding, rinses by diluted acid, then with anhydrous
Ethyl alcohol impregnates, finally clean with ultrapure water, is dried for standby.
5. a kind of SPEEK-PVDF gas regulation composite membrane, it is characterised in that: pass through the described in any item sides of Claims 1 to 4
Method is prepared, gained SPEEK-PVDF gas regulation composite membrane with a thickness of 17~24 μm.
6. application of the SPEEK-PVDF gas regulation composite membrane in fruit and vegetable air-conditioning preservation described in claim 5.
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| 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 |
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 |
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| 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 |
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