CN104693475A - Preparation method of polymer porous material - Google Patents
Preparation method of polymer porous material Download PDFInfo
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- CN104693475A CN104693475A CN201310673727.1A CN201310673727A CN104693475A CN 104693475 A CN104693475 A CN 104693475A CN 201310673727 A CN201310673727 A CN 201310673727A CN 104693475 A CN104693475 A CN 104693475A
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Abstract
The invention discloses a preparation method of a polymer porous material, and belongs to the technical field of function materials. The preparation method comprises the following steps: 1, soaking the polymer material in a mixed solution of good solvent and bad solvent in a certain proportion for a certain time; 2, rapidly taking out the polymer material, placing in a glass container filled with liquid nitrogen, freezing for a certain time; 3, taking out a polymer sample, slowly releasing at a certain temperature to coagulate the good solvent in the polymer, inducing the formation of micro-nano-level porous on the polymer surface. The method disclosed by the invention has the advantages of being simple in process, low in energy consumption and high in efficiency.
Description
Technical field
The present invention relates to a kind of preparation method of high-molecular porous material, belong to technical field of function materials.
Background technology
The nineties in 20th century, highly ordered porous materials rose rapidly as novel nano structure material, just obtained the great attention of international physics, chemistry and each educational circles of material immediately, and became one of study hotspot interdisciplinary.Nano ordered porous material due to its have that pore passage structure size is adjustable, the queueing discipline in hole and the feature such as porous specific surface area is larger, make it in separation, absorption, catalysis, biology, medical science etc., have great application potential.In addition, porous material is also used as efficient air liquid phase column material, sensor sensitive material, special cells material, the protective layer material even in enzyme or albumen transport process.Meanwhile, multiple dimensioned ordered porous membrane material can be used as support of the catalyst, dye-sensitized solar cell anode, membrane reactor etc.Therefore porous-film and corresponding membrane separation technique such as micro-filtration, ultrafiltration, electrodialysis, reverse osmosis etc. have been widely used in the fields such as food, medical and health, biotechnology, chemical industry, the energy, environment at present, and play more and more important effect.
Through the research of highly ordered porous materials for many years and the effort of scientific worker, this field has achieved appreciable progress.But because the research of each side such as preparation, character, function of highly ordered porous materials needs comprehensive chemistry and physical knowledge, thus still there is the problem that some need to solve.Porous material preparation method is a lot, and conventional has phase inversion method, phase separation method, sol-gel method, macromole rigging method, solvent pore and solvent-nonsolvent effect etc.And the formation of micron and nanostructure has indentation method, solvent and non-solvent effect, phase separation method, emulsion polymerization, masterplate method, etching method, self-assembly method etc. usually.These methods often operating process more complicated, consume energy high, the used time is of a specified duration.For seeking method more simple to operation to prepare porous membrane, we study and find to carry out direct supersound process to film, used time is short effective, effectively can be controlled vesicular structure and the hole density distribution of film by the ratio and ultrasonic time controlling solvent and non-solvent, obtain orderly porous-film.
Summary of the invention
The object of this invention is to provide a kind of preparation method of high-molecular porous material, the method step is as follows:
(1) preparation of mixed solution
The solvent of macromolecule member material and another two kinds of non-solvents mixing can be dissolved by a kind of.
(2) macromolecule membrane preparation
To be placed in macromolecular material at mixed solution, after certain hour, PS sheet is swelling, and volume increases;
(3) preparation of high-molecular porous material
(1) swelling PS sheet is placed in liquid nitrogen freezing, it is inner that solvent toluene envelope is enclosed in PS sheet;
(2) slowly heat up, toluene is evaporated gradually from PS sheet.In volatilization process, bring out PS sheet surface form orderly micron or nanometer porous structure.
Adopt cold method to prepare high-molecular porous material, described macromolecular material thing is selected from polyethylene, polypropylene, polyvinyl chloride, polyvinylidene difluoride (PVDF), polystyrene, polyethylene terephthalate, rhodia, Mierocrystalline cellulose, polyvinyl alcohol, nylon, polymethacrylate, polycarbonate, polyphenylene oxide, polyoxymethylene, polyimide, polyacrylonitrile, polyvinylacetate, resol.
Described macromolecular material obtains by physics or chemical process.
Described mixed solution will be selected a kind ofly can dissolve the solvent of macromolecule member material and other two kinds of non-solvents.And solvent and non-solvent can not dissolve each other.
Volume fraction shared by described solvent is 10%-20%.
Described macromolecular material needs at mixed solution kind swelling treatment 1h
Described macromolecular material needs liquid nitrogen freezing process 2h.Afterwards, clean with distilled water flushing immediately, then dry.
The invention has the beneficial effects as follows:
(1) can prepare multiple high-molecular porous material, applied range, which greatly simplifies technological process.
(2) have multiple due to a kind of high molecular solvent can be dissolved, so the selectable solvent of preparation process and non-solvent scope are extensively, can effectively select more suitable solvent.
(3) because freezing treatment is simple to operate and the time used is short, energy consumption and time is greatly reduced.
(4) amount of solvent and non-solvent and swelling, freezing treatment time can be controlled, effectively control pore size and hole density distribution, so the scope of application is wider, the porous material of a series of different pore size distribution can be prepared.
Accompanying drawing explanation
Fig. 1 is polystyrene porous material SEM picture prepared by embodiment 1.
Embodiment
Adopting cold method, is that high-molecular porous material prepared by raw material with macromolecular material.
Below in conjunction with embodiment, the invention will be further described, can better understand the present invention and can be implemented, but illustrated embodiment is not as a limitation of the invention to make those skilled in the art.
Embodiment 1
A preparation method for organic porous material, the method step is as follows:
(1) preparation of mixed solution
A certain amount of toluene is scattered in the mixed solution that mixed solvent that ethanol (or methyl alcohol) and the ratio of water are 7:3 makes into 18%.
(2) preparation of high-molecular porous film
By polystyrene (PS, Mw=200kDa, Goodfellow Co.Ltd., Britain) plate is placed in the mixed solution of toluene, second alcohol and water, swelling treatment 1h, liquid nitrogen freezing process 2h, rapid taking-up PS plate, makes it heat up and makes the solvent evaporates time be that about 100min discharges toluene, use distilled water wash afterwards, drying, obtains PS porous material.
Fig. 1 is the SEM figure of the PS porous material of preparation, and as seen from the figure, obtained porous-film pore size distribution is narrower, and basic controlling is at 300nm-1 μm, and hole density is comparatively large, has good application potential.
As seen from the above-described embodiment, prepared PS porous-film has narrower pore size distribution, and basic controlling is at 300nm-1 μm, and hole density is larger.And pore size can be controlled by the concentration of toluene and water mixed liquid and swelling and freezing time, both can obtain the less pore structure in aperture, can prepare again the larger porous-film in aperture, have larger practical value.And simple to operate, to reducing costs, there is great help.
Claims (10)
1. a preparation method for high-molecular porous material, is characterized in that,
In the both side surface of polystyrene board, be uniformly distributed this hemispheric cavity structure, described polystyrene plate thickness is 1mm, and the chemical composition in polystyrene board is pure polystyrene.The controlled diameter scope in the hole in described polystyrene is between about 40nm-10 μm.
2. a kind of cold method as claimed in claim 1 prepares polystyrene porous material, it is characterized in that described polystyrene molecular weight is 100kDa-300kDa.
3. a kind of cold method as claimed in claim 1 prepares polystyrene porous material, it is characterized in that described method is cold method.
4. a kind of cold method as claimed in claim 1 prepares polystyrene porous material, it is characterized in that described comprising the following steps,
1) preparation of mixed solution: choose three kinds to the different good solvent of macromolecular material solubility property and poor solvent; Poor solvent is two kinds.By these two kinds of solvent liquid combination treatment in certain proportion, make it to form the homogeneous emulsion of dispersion;
2) the swelling refrigerating process of macromolecular material: mixed solution macromolecular material being placed in above-mentioned good solvent and poor solvent, after swelling certain hour, takes out macromolecule plate freezing treatment certain hour in liquid nitrogen atmosphere rapidly;
3) the vesicular structure preparation in macromolecular material: after macromolecular material is taken out from liquid nitrogen, be placed in the nearly surface that good solvent intensification is made it to be discharged in the middle of macromolecular material macromolecular material by certain temperature atmosphere, dry through distilled water wash and under room temperature, obtain high-molecular porous material.
5. a kind of cold method according to claim 1 prepares polystyrene porous MATERIALS METHODS, it is characterized in that described macromolecular material obtains by physics or chemical process.
6. a kind of cold process according to claim 1 prepares polystyrene porous MATERIALS METHODS, it is characterized in that adopted PS plate.
7. a kind of cold method according to claim 1 prepares polystyrene porous MATERIALS METHODS, it is characterized in that described mixed solution will select three kinds to the diverse good solvent of macromolecule member material solubility property and poor solvent.Wherein swelling agent and a toluene, two kinds of non-swelling agents and ethanol (or methyl alcohol) and water, the ratio of methyl alcohol and water is 7:3.
8. a kind of cold method according to claim 1 prepares polystyrene porous membrane material method, it is characterized in that the concentration of described mixed solution is 10%-20%.
9. a kind of cold method according to claim 1 prepares polystyrene porous MATERIALS METHODS, it is characterized in that preparation needs swelling treatment 1h in swelling agent of described mixed solution, the preparation of described porous material needs liquid nitrogen freezing process 2h, and the solvent evaporates time is about 100min.
10. a kind of cold method according to claim 1 prepares polystyrene porous MATERIALS METHODS, it is characterized in that described material is after freezing treatment, clean with distilled water flushing immediately, then dry under room temperature.
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| CN201310673727.1A CN104693475A (en) | 2013-12-06 | 2013-12-06 | Preparation method of polymer porous material |
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| CN201310673727.1A CN104693475A (en) | 2013-12-06 | 2013-12-06 | Preparation method of polymer porous material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104119554A (en) * | 2014-07-15 | 2014-10-29 | 天津工业大学 | Method for preparing organic porous film by adopting freezing method |
| CN105293473A (en) * | 2015-11-30 | 2016-02-03 | 天津工业大学 | Porous carbon material taking polyvinylidene fluoride as precursor and preparation method |
| CN107261866A (en) * | 2017-08-10 | 2017-10-20 | 武汉纺织大学 | A kind of preparation method of through hole membrane for water treatment |
| CN108948587A (en) * | 2018-07-24 | 2018-12-07 | 常州达奥新材料科技有限公司 | A kind of dedicated bloom modified master of transparent PVC boardy product |
| CN109621920A (en) * | 2019-01-28 | 2019-04-16 | 南京师范大学 | A kind of pipe/polyhenylethylene nano zero-valent iron composite material and its preparation method and application |
| CN112980028A (en) * | 2021-02-05 | 2021-06-18 | 浙江大学 | Polymer material with porous interface and preparation method thereof |
-
2013
- 2013-12-06 CN CN201310673727.1A patent/CN104693475A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104119554A (en) * | 2014-07-15 | 2014-10-29 | 天津工业大学 | Method for preparing organic porous film by adopting freezing method |
| CN104119554B (en) * | 2014-07-15 | 2018-01-09 | 天津工业大学 | A kind of method that organic porous films are prepared using freezing |
| CN105293473A (en) * | 2015-11-30 | 2016-02-03 | 天津工业大学 | Porous carbon material taking polyvinylidene fluoride as precursor and preparation method |
| CN107261866A (en) * | 2017-08-10 | 2017-10-20 | 武汉纺织大学 | A kind of preparation method of through hole membrane for water treatment |
| CN108948587A (en) * | 2018-07-24 | 2018-12-07 | 常州达奥新材料科技有限公司 | A kind of dedicated bloom modified master of transparent PVC boardy product |
| CN109621920A (en) * | 2019-01-28 | 2019-04-16 | 南京师范大学 | A kind of pipe/polyhenylethylene nano zero-valent iron composite material and its preparation method and application |
| CN112980028A (en) * | 2021-02-05 | 2021-06-18 | 浙江大学 | Polymer material with porous interface and preparation method thereof |
| CN112980028B (en) * | 2021-02-05 | 2022-04-29 | 浙江大学 | Polymer material with porous interface and preparation method thereof |
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Application publication date: 20150610 |