CN1844207A - Method for preparation of ordered porous conductive polymer by suction filtration / immersion method - Google Patents
Method for preparation of ordered porous conductive polymer by suction filtration / immersion method Download PDFInfo
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- CN1844207A CN1844207A CN 200610018387 CN200610018387A CN1844207A CN 1844207 A CN1844207 A CN 1844207A CN 200610018387 CN200610018387 CN 200610018387 CN 200610018387 A CN200610018387 A CN 200610018387A CN 1844207 A CN1844207 A CN 1844207A
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Abstract
The invention relates to a method for preparation of an order and porous conducting polymer with the method of suctioning /dipping. The method includes: simultaneously immersing the monomer and initiator into the cemented crystal mold to polymerize by suctioning, then removing the mold to obtain the three-dimensional order and porous conducting polymer. The method is characterized in that it is of simple craft, the requirement for reaction unit is not high, and the prepared porous conducting polymer has a higher regular degree at a larger range of area.
Description
Technical field
The present invention relates to ordered porous material field, particularly a kind of method with preparation of ordered porous conductive polymer by suction filtration/immersion method.
Background technology
Large pore material (being of a size of 50~hundreds of nanometer) be used widely at aspects such as support of the catalyst, chromosorb and parting materials, but the large pore material pore size distribution that traditional preparation process technology makes is wide, and irregular, and its application has been subjected to certain restriction.At the end of the nineties in last century, Vevel usefulness colloidal crystal template methods such as (Nature, 1997,389:447~448) has successfully prepared three-dimensional ordered macroporous (3DOM) material, makes the research of large pore material enter a new stage.This 3DOM material, the wide aperture that not only has general large pore material, and pore size distribution is narrow, the duct is neat and orderly, hole wall is made up of nanoparticle, being the novel macroporous catalyst of a class, sorbent material, chromatographic material and microbe carrier, and because the space lattice arrangement architecture of high-sequential, is a kind of photonic crystal of having optimized.
And the end of the seventies in last century, Shiraknwa H (J.Chemsoc., Chem.Commun., 1977:578) grade is to the discovery of conduction polyacetylene (PA), broken polymer and only be the traditional concept of isolator, subsequently people again in succession the exploitation a series of conductive polymerss (for example: polyaniline, polypyrrole, Polythiophene etc.).Because these conductive polymerss have caused the extensive attention of academia in the property of aspects such as electricity, magnetic, light, develop very rapid.
Bartlett (J.Mater.Chem., 2001,11:849~853) etc. adopt the electrochemically oxidative polymerization method, at first polystyrene microsphere is deposited on the Au electrode, form colloidal crystal template, then be inserted in the presoma (monomer) of certain density conductive polymers, and anodised electrochemical reaction takes place on the Au electrode, make monomer in the hole of colloidal crystal, polymerization take place, then the template with polystyrene etches away, thereby form the three-dimensional ordered polyporous material of conductive polymers, they have prepared polyaniline by this method, polypyrrole, the three-dimensional ordered polyporous material of Polythiophene.But the required colloidal crystal template of this method must be deposited on earlier on the electrode, and mode of deposition is required to be difficult to realize the preparation of the continuous poriferous conductive polymers of big area than higher.
F Caruso (Adv.Mater., 2001,13:350~353) etc. adopt centrifugal/pickling process, at first polystyrene moulding is put into special centrifuge tube, then be taken up in order of priority with the hydrochloric acid soln of the hydrochloric acid soln of aniline monomer and ammonium persulfate centrifugal/dipping three times, make aniline monomer in the centrifugal process, enter in the hole of polystyrene moulding and initiated polymerization, then remove polystyrene moulding and obtain the porous, electrically conductive polyaniline by the suction filtration of organic solvent.But this method need be carried out under centrifugal condition, and the requirement of equipment and template all than higher, is difficult to realize the preparation of big area porous conductive polymer.
Vacuum filtration is widely used in product separation, filters basic fields such as pure as the easy laboratory facilities of a kind of routine.Utilize the vacuum filtration technology can in than the big area scope, prepare the colloidal crystal template of higher regularity, utilize this technology can make polymer precursor (monomer) and initiator fully flood the colloidal crystal template polymerization reaction take place equally.Prepare the larger area porous polymer material after removing template.
Summary of the invention
The objective of the invention is at the prepared porous conductive polymer area of prior art little, the equipment requirements height, deficiencies such as complex process are utilized the advantage of vacuum filtration/dipping technique, and a kind of method with vacuum filtration/immersion process for preparing ordered porous conductive polymer that provides.The characteristics of this method are: 1. the preparation method of template is simple and area is bigger; 2. conversion unit less demanding (the micropore filter paper of common G4 sand core funnel and 0.22 μ); 3. Zhi Bei porous conductive polymer has higher regularity in than the big area scope.
The objective of the invention is to adopt following technological line to realize:
At first, the emulsion droplets that will contain particle size range and be 300nm~2 μ mono-dispersion microballoons is added in the G4 sand core funnel of the millipore filtration that is lined with aperture 0.22 μ, by vacuum filtration the liquid in the emulsion is taken out, made microballoon on millipore filtration, form wetting colloidal crystal.
Secondly, with the monomer of conductive polymers and initiator by mass ratio 1~5: 0.5 mixes rapidly, is added drop-wise on the wetting colloid crystal film, makes initiated polymerization behind the hole of mixing solutions immersion colloidal crystal of monomer and initiator by vacuum filtration simultaneously.The baking oven of subsequently complex body of conductive polymers and colloidal crystal template being put into temperature and be 60 ℃ dries by the fire 24h.
At last, the template of colloidal crystal is removed, promptly get ordered porous conductive polymer with removing the mould agent.
With mono-dispersion microballoon described in the method for preparation of ordered porous conductive polymer by suction filtration/immersion method is polystyrene microsphere (PS), poly (methyl methacrylate) micro-sphere (PMMA), poly-(vinylbenzene-methyl methacrylate) copolymer microballoon (PS/PMMA); Monomer is aniline, pyrroles, thiophene; Initiator is ammonium persulfate, Potassium Persulphate; Removing the mould agent is toluene, dimethylbenzene, trichloromethane.
The present invention has following advantage: the preparation method of (1) template is simple and in than the big area scope regular (as Fig. 2) in order; (2) conversion unit less demanding (the micropore filter paper of common G4 sand core funnel and 0.22 μ), reaction need not be carried out under electrochemical conditions or centrifugal condition; (3) Zhi Bei porous conductive polymer has higher regularity (as Fig. 3) in than the big area scope.
Description of drawings
Accompanying drawing 1 is a technological line of the present invention.A. mono-dispersion microballoon among the figure; B. the mixing solutions of conductive polymers monomer and initiator; C. remove the mould agent; 1. the preparation of colloidal crystal template; 2. extracting/dipping polymerization; 3. template removes.
Fig. 2 is the structure iron of template.
Fig. 3 is the structure iron of porous conductive polymer.
Embodiment
Embodiment 1
PS mono-dispersion microballoon (particle diameter the is 300nm) emulsion droplets of 1g 1w.t% is added in the G4 sand core funnel of the millipore filtration that is lined with aperture 0.22 μ, by vacuum filtration the liquid in the emulsion is taken out, made the PS microballoon on millipore filtration, form wetting PS colloidal crystal.Then aniline and ammonium persulfate are rapidly mixed by mass ratio at 1: 0.5, be added drop-wise on the wetting PS colloid crystal film, make the mixing solutions of aniline and ammonium persulfate immerse the hole of colloidal crystal by vacuum filtration simultaneously, initiated polymerization generates polyaniline.The baking oven of subsequently complex body of polyaniline and PS colloidal crystal template being put into temperature and be 60 ℃ dries by the fire 24h.At last, the PS colloidal crystal template is removed, promptly got the porous polyaniline with toluene.
Embodiment 2
PMMA mono-dispersion microballoon (particle diameter the is 500nm) emulsion droplets of 1.3g 0.8w.t% is added in the G4 sand core funnel of the millipore filtration that is lined with aperture 0.22 μ, by vacuum filtration the liquid in the emulsion is taken out, made the PMMA microballoon on millipore filtration, form wetting PMMA colloidal crystal.Then aniline and Potassium Persulphate are rapidly mixed by mass ratio at 2: 0.5, be added drop-wise on the wetting PMMA colloid crystal film, make the mixing solutions of aniline and Potassium Persulphate immerse the hole of colloidal crystal by vacuum filtration simultaneously, initiated polymerization generates polyaniline.The baking oven of subsequently complex body of polyaniline and PMMA colloidal crystal template being put into temperature and be 60 ℃ dries by the fire 24h.At last, the PMMA colloidal crystal template is removed, promptly got the porous polyaniline with dimethylbenzene.
Embodiment 3
PS/PMMA mono-dispersion microballoon (particle diameter the is 450nm) emulsion droplets of 1.5g 0.6w.t% is added in the G4 sand core funnel of the millipore filtration that is lined with aperture 0.22 μ, by vacuum filtration the liquid in the emulsion is taken out, made the PS/PMMA microballoon on millipore filtration, form wetting PS/PMMA colloidal crystal.Then aniline and ammonium persulfate are rapidly mixed by mass ratio at 4: 0.5, be added drop-wise on the wetting PS/PMMA colloid crystal film, make the mixing solutions of aniline and ammonium persulfate immerse the hole of colloidal crystal by vacuum filtration simultaneously, initiated polymerization generates polyaniline.The baking oven of subsequently complex body of polyaniline and PS/PMMA colloidal crystal template being put into temperature and be 60 ℃ dries by the fire 24h.At last, the PS/PMMA colloidal crystal template is removed, promptly got the porous polyaniline with dimethylbenzene.
Embodiment 4
PS mono-dispersion microballoon (particle diameter the is 600nm) emulsion droplets of 0.8g 5w.t% is added in the G4 sand core funnel of the millipore filtration that is lined with aperture 0.22 μ, by vacuum filtration the liquid in the emulsion is taken out, made the PS microballoon on millipore filtration, form wetting PS colloidal crystal.Then aniline and Potassium Persulphate are rapidly mixed by mass ratio at 3: 0.5, be added drop-wise on the wetting PS colloid crystal film, make the mixing solutions of aniline and Potassium Persulphate immerse the hole of colloidal crystal by vacuum filtration simultaneously, initiated polymerization generates polyaniline.The baking oven of subsequently complex body of polyaniline and PS colloidal crystal template being put into temperature and be 60 ℃ dries by the fire 24h.At last, the PS colloidal crystal template is removed, promptly got the porous polyaniline with trichloromethane.
Embodiment 5
PS mono-dispersion microballoon (particle diameter the is 1 μ) emulsion droplets of 2g 0.3w.t% is added in the G4 sand core funnel of the millipore filtration that is lined with aperture 0.22 μ, by vacuum filtration the liquid in the emulsion is taken out, made the PS microballoon on millipore filtration, form wetting PS colloidal crystal.Then aniline and ammonium persulfate are rapidly mixed by mass ratio at 5: 0.5, be added drop-wise on the wetting PS colloid crystal film, make the mixing solutions of aniline and ammonium persulfate immerse the hole of colloidal crystal by vacuum filtration simultaneously, initiated polymerization generates polyaniline.The baking oven of subsequently complex body of polyaniline and PS colloidal crystal template being put into temperature and be 60 ℃ dries by the fire 24h.At last, the PS colloidal crystal template is removed, promptly got the porous polyaniline with trichloromethane.
Embodiment 6
PS mono-dispersion microballoon (particle diameter the is 1.5 μ) emulsion droplets of 1g 1w.t% is added in the G4 sand core funnel of the millipore filtration that is lined with aperture 0.22 μ, by vacuum filtration the liquid in the emulsion is taken out, made the PS microballoon on millipore filtration, form wetting PS colloidal crystal.Then aniline and ammonium persulfate are rapidly mixed by mass ratio at 2: 0.5, be added drop-wise on the wetting PS colloid crystal film, make the mixing solutions of aniline and ammonium persulfate immerse the hole of colloidal crystal by vacuum filtration simultaneously, initiated polymerization generates polyaniline.The baking oven of subsequently complex body of polyaniline and PS colloidal crystal template being put into temperature and be 60 ℃ dries by the fire 24h.At last, the PS colloidal crystal template is removed, promptly got the porous polyaniline with dimethylbenzene.
Embodiment 7
PS mono-dispersion microballoon (particle diameter the is 2 μ) emulsion droplets of 0.5g 2w.t% is added in the G4 sand core funnel of the millipore filtration that is lined with aperture 0.22 μ, by vacuum filtration the liquid in the emulsion is taken out, made the PS microballoon on millipore filtration, form wetting PS colloidal crystal.Then aniline and ammonium persulfate are rapidly mixed by mass ratio at 3: 0.5, be added drop-wise on the wetting PS colloid crystal film, make the mixing solutions of aniline and ammonium persulfate immerse the hole of colloidal crystal by vacuum filtration simultaneously, initiated polymerization generates polyaniline.The baking oven of subsequently complex body of polyaniline and PS colloidal crystal template being put into temperature and be 60 ℃ dries by the fire 24h.At last, the PS colloidal crystal template is removed, promptly got the porous polyaniline with toluene.
Embodiment 8
PS/PMMA mono-dispersion microballoon (particle diameter the is 1.3 μ) emulsion droplets of 0.6g 3w.t% is added in the G4 sand core funnel of the millipore filtration that is lined with aperture 0.22 μ, by vacuum filtration the liquid in the emulsion is taken out, made the PS/PMMA microballoon on millipore filtration, form wetting PS/PMMA colloidal crystal.Then aniline and ammonium persulfate are rapidly mixed by mass ratio at 3: 0.5, be added drop-wise on the wetting PS/PMMA colloid crystal film, make the mixing solutions of aniline and ammonium persulfate immerse the hole of colloidal crystal by vacuum filtration simultaneously, initiated polymerization generates polyaniline.The baking oven of subsequently complex body of polyaniline and PS/PMMA colloidal crystal template being put into temperature and be 60 ℃ dries by the fire 24h.At last, the PS/PMMA colloidal crystal template is removed, promptly got the porous polyaniline with toluene.
Embodiment 9
PMMA mono-dispersion microballoon (particle diameter the is 750nm) emulsion droplets of 0.4g 7w.t% is added in the G4 sand core funnel of the millipore filtration that is lined with aperture 0.22 μ, by vacuum filtration the liquid in the emulsion is taken out, made the PMMA microballoon on millipore filtration, form wetting PMMA colloidal crystal.Then aniline and Potassium Persulphate are rapidly mixed by mass ratio at 3: 0.5, be added drop-wise on the wetting PMMA colloid crystal film, make the mixing solutions of aniline and Potassium Persulphate immerse the hole of colloidal crystal by vacuum filtration simultaneously, initiated polymerization generates polyaniline.The baking oven of subsequently complex body of polyaniline and PMMA colloidal crystal template being put into temperature and be 60 ℃ dries by the fire 24h.At last, the PMMA colloidal crystal template is removed, promptly got the porous polyaniline with dimethylbenzene.
Embodiment 10
PS mono-dispersion microballoon (particle diameter the is 1 μ) emulsion droplets of 0.9g 1.6w.t% is added in the G4 sand core funnel of the millipore filtration that is lined with aperture 0.22 μ, by vacuum filtration the liquid in the emulsion is taken out, made the PS microballoon on millipore filtration, form wetting PS colloidal crystal.Then pyrroles and ammonium persulfate are rapidly mixed by mass ratio at 5: 0.5, be added drop-wise on the wetting PS colloid crystal film, make the mixing solutions of pyrroles and ammonium persulfate immerse the hole of colloidal crystal by vacuum filtration simultaneously, initiated polymerization generates polypyrrole.The baking oven of subsequently complex body of polypyrrole and PS colloidal crystal template being put into temperature and be 60 ℃ dries by the fire 24h.At last, the PS colloidal crystal template is removed, promptly got the porous polypyrrole with dimethylbenzene.
Embodiment 11
PS/PMMA mono-dispersion microballoon (particle diameter the is 800nm) emulsion droplets of 0.5g 8w.t% is added in the G4 sand core funnel of the millipore filtration that is lined with aperture 0.22 μ, by vacuum filtration the liquid in the emulsion is taken out, made the PS/PMMA microballoon on millipore filtration, form wetting PS/PMMA colloidal crystal.Then pyrroles and ammonium persulfate are rapidly mixed by mass ratio at 4: 0.5, be added drop-wise on the wetting PS/PMMA colloid crystal film, make the mixing solutions of pyrroles and ammonium persulfate immerse the hole of colloidal crystal by vacuum filtration simultaneously, initiated polymerization generates polypyrrole.The baking oven of subsequently complex body of polypyrrole and PS/PMMA colloidal crystal template being put into temperature and be 60 ℃ dries by the fire 24h.At last, the PS/PMMA colloidal crystal template is removed, promptly got the porous polypyrrole with dimethylbenzene.
Embodiment 12
PMMA mono-dispersion microballoon (particle diameter the is 900nm) emulsion droplets of 1g 0.7w.t% is added in the G4 sand core funnel of the millipore filtration that is lined with aperture 0.22 μ, by vacuum filtration the liquid in the emulsion is taken out, made the PMMA microballoon on millipore filtration, form wetting PMMA colloidal crystal.Then thiophene and Potassium Persulphate are rapidly mixed by mass ratio at 2: 0.5, be added drop-wise on the wetting PMMA colloid crystal film, make the mixing solutions of thiophene and Potassium Persulphate immerse the hole of colloidal crystal by vacuum filtration simultaneously, initiated polymerization generates Polythiophene.The baking oven of subsequently complex body of Polythiophene and PMMA colloidal crystal template being put into temperature and be 60 ℃ dries by the fire 24h.At last, the PMMA colloidal crystal template is removed, promptly got the porous Polythiophene with dimethylbenzene.
Embodiment 13
PS mono-dispersion microballoon (particle diameter the is 500nm) emulsion droplets of 2g 0.9w.t% is added in the G4 sand core funnel of the millipore filtration that is lined with aperture 0.22 μ, by vacuum filtration the liquid in the emulsion is taken out, made the PS microballoon on millipore filtration, form wetting PS colloidal crystal.Then thiophene and Potassium Persulphate are rapidly mixed by mass ratio at 3: 0.5, be added drop-wise on the wetting PS colloid crystal film, make the mixing solutions of thiophene and Potassium Persulphate immerse the hole of colloidal crystal by vacuum filtration simultaneously, initiated polymerization generates Polythiophene.The baking oven of subsequently complex body of Polythiophene and PS colloidal crystal template being put into temperature and be 60 ℃ dries by the fire 24h.At last, the PS colloidal crystal template is removed, promptly got the porous Polythiophene with toluene.
Embodiment 14
PS/PMMA mono-dispersion microballoon (particle diameter the is 800nm) emulsion droplets of 0.5g 8w.t% is added in the G4 sand core funnel of the millipore filtration that is lined with aperture 0.22 μ, by vacuum filtration the liquid in the emulsion is taken out, made the PS/PMMA microballoon on millipore filtration, form wetting PS/PMMA colloidal crystal.Then thiophene and ammonium persulfate are rapidly mixed by mass ratio at 4: 0.5, be added drop-wise on the wetting PS/PMMA colloid crystal film, make the mixing solutions of thiophene and ammonium persulfate immerse the hole of colloidal crystal by vacuum filtration simultaneously, initiated polymerization generates Polythiophene.The baking oven of subsequently complex body of Polythiophene and PS/PMMA colloidal crystal template being put into temperature and be 60 ℃ dries by the fire 24h.At last, the PS/PMMA colloidal crystal template is removed, promptly got the porous Polythiophene with trichloromethane.
Claims (7)
1, a kind of method with preparation of ordered porous conductive polymer by suction filtration/immersion method, it is characterized in that: 1. the emulsion droplets with mono-dispersion microballoon is added in the sand core funnel that is lined with millipore filtration, makes mono-dispersion microballoon form wetting colloidal crystal by vacuum filtration; 2. the mixing solutions of the monomer of conductive polymers and initiator is immersed initiated polymerization behind the hole of colloidal crystal by vacuum filtration, oven dry; 3. with removing the mould agent template of colloidal crystal is removed, promptly get porous conductive polymer.
2, the method for the 3-D ordered multiporous conductive polymers of preparation according to claim 1 is characterized in that mono-dispersion microballoon is polystyrene microsphere, poly (methyl methacrylate) micro-sphere, poly-(vinylbenzene-methyl methacrylate) copolymer microballoon.
3, the method for the 3-D ordered multiporous conductive polymers of preparation according to claim 1, the particle size range that it is characterized in that mono-dispersion microballoon are 300nm~2 μ.
4, the method for the 3-D ordered multiporous conductive polymers of preparation according to claim 1 is characterized in that monomer is aniline, pyrroles, thiophene.
5, the method for the 3-D ordered multiporous conductive polymers of preparation according to claim 1 is characterized in that initiator is ammonium persulfate, Potassium Persulphate.
6, the method for the 3-D ordered multiporous conductive polymers of preparation according to claim 1 is characterized in that removing the mould agent is toluene, dimethylbenzene, trichloromethane.
7, the method for the 3-D ordered multiporous conductive polymers of preparation according to claim 1, the monomer that it is characterized in that conductive polymers and initiator are by mass ratio 1~5: 0.5 mixes.
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Cited By (4)
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CN101225179B (en) * | 2008-02-05 | 2011-07-20 | 复旦大学 | Large-area ordered porous membrane material and preparation method thereof |
CN101633786B (en) * | 2008-07-23 | 2011-12-21 | 复旦大学 | Structural color film material and method for preparing same |
CN107245143A (en) * | 2017-01-15 | 2017-10-13 | 北京林业大学 | A kind of preparation method of porous polyaniline material applied to hexavalent chromium removal |
CN110304636A (en) * | 2019-06-28 | 2019-10-08 | 上海交通大学 | A kind of method that vacuum filtration prepares photo crystal thick |
Family Cites Families (4)
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CN1129641C (en) * | 2001-01-04 | 2003-12-03 | 中国科学院化学研究所 | Prepn of ordered porous material comprising ordered polymer and inorganic heterocomplex and its derivative |
DE10258491A1 (en) * | 2002-12-14 | 2004-07-01 | Merck Patent Gmbh | Sorbents with a uniform pore size |
CN1546431A (en) * | 2003-12-12 | 2004-11-17 | 上海交通大学 | Method for preparing three-dimensional ordered and pore-size adjustable porous ceramic nanotube |
CN1556067A (en) * | 2004-01-08 | 2004-12-22 | 上海交通大学 | Preparaton method of ordered macro porous inorganic oxide material |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101225179B (en) * | 2008-02-05 | 2011-07-20 | 复旦大学 | Large-area ordered porous membrane material and preparation method thereof |
CN101633786B (en) * | 2008-07-23 | 2011-12-21 | 复旦大学 | Structural color film material and method for preparing same |
CN107245143A (en) * | 2017-01-15 | 2017-10-13 | 北京林业大学 | A kind of preparation method of porous polyaniline material applied to hexavalent chromium removal |
CN110304636A (en) * | 2019-06-28 | 2019-10-08 | 上海交通大学 | A kind of method that vacuum filtration prepares photo crystal thick |
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