CN102091533A - Method for preparing poly(N-2-carboxyethyl pyrrole)-anodic aluminum oxide composite membrane - Google Patents
Method for preparing poly(N-2-carboxyethyl pyrrole)-anodic aluminum oxide composite membrane Download PDFInfo
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Abstract
The invention discloses a method for preparing a poly(N-2-carboxyethyl pyrrole)-anodic aluminum oxide composite membrane, relates to a composite membrane preparation technique and provides a method for preparing a poly(N-2-carboxyethyl pyrrole)-anodic aluminum oxide composite membrane with high hydrophily and high biocompatibility. The method comprises the following steps: placing a pretreated anodic aluminum oxide membrane and a N-2-carboxyethyl pyrrole monomer in a vapor phase deposition polymerization device, vacuumizing the vapor phase deposition polymerization device and performing a vapor phase deposition polymerization reaction; and after the reaction is accomplished, cooling, and removing impurities to obtain the poly(N-2-carboxyethyl pyrrole)-anodic aluminum oxide composite membrane. The prepared poly(N-2-carboxyethyl pyrrole)-anodic aluminum oxide composite membrane covers the oxide layer on the anodic aluminum oxide membrane, and lowers the non-specific absorption of the anodic aluminum oxide membrane. The preparation method is simple, and can be widely used in affinity separation.
Description
Technical field
The present invention relates to the composite membrane technology of preparing, particularly a kind of preparation method of poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film.
Background technology
Traditional separation method can make product purity improve as precipitation, crystallization, chromatography etc., but exist problems such as technology is loaded down with trivial details, activity recovery is lower.The affinity film chromatography technology has the technical advantage that high selectivity, high yield and a step obtain high purity product, has become one of otherwise effective technique of protein purification.Affine membrane separation efficiency depends primarily on the performance of membrane material, and affinity membrane material commonly used mainly is an organic film material.Natural macromolecular material such as cellulose, polysaccharide has excellent biological compatibility and hydrophily, and contains a large amount of active groups, but often is difficult to film forming, and its application is restricted.Artificial synthesized polymer material such as polysulfones, polyamide, polyethylene have good filming performance, but more hydrophobic grouping is contained on its surface, and the especially easy and irreversible non-selective absorption of its generation of protein of biomolecule pollutes film.Compare with organic film material, inorganic material film has good chemistry, machinery and heat endurance, has represented wide application prospect at affine separation field.
Affinity membrane isolation technics requirement membrane matrix aperture and porosity distribution are even, and available chemical group is many, and non-specific adsorption is few.Anodic alumina films not only has the membrane pore structure of super homogeneous as a kind of commodity inoranic membrane, and has excellent mechanical intensity, but because layer of oxide layer is contained on its surface, there is stronger non-specific adsorption in most protein.In addition, hydroxy radical content is few on the anodic alumina films, and activity is not high, is difficult for immobilized aglucon, must make its satisfied requirement as affine diffusion barrier to its modification.Chinese patent 200710009962.3 discloses a kind of gelatin-amino silane-anodised aluminum compound film of compatibility, Chinese patent 200710009960.4 discloses a kind of gelatin-epoxy radicals silicone hydride-anodised aluminum compound film of compatibility, Chinese patent 200810071236.9 discloses a kind of chitose-aminosilane-anodised aluminum compound film of compatibility, and they all have excellent biological compatibility and abundant active group.But the composite membrane of these three kinds of compatibilities all adopts natural polymer antianode pellumina to carry out modification, adopts artificial synthetic macromolecular material to carry out the method that the antianode pellumina carries out modification and does not appear in the newspapers as yet.
Summary of the invention
Purpose of the present invention aims to provide a kind of preparation method with poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film of good hydrophilic performance and good biocompatibility.
The preparation method of described poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film may further comprise the steps:
1) will place in the vapor deposition polymerization device through pretreated anodic alumina films and N-2-carboxyethyl pyrrole monomer, and described vapor deposition polymerization device will be vacuumized laggard promoting the circulation of qi phase deposition polymerization reaction;
2) reaction finishes the back cooling, removes impurity and promptly gets and gather N-2-carboxyethyl pyrroles-anodised aluminum compound film.
In step 1), described pretreated method can be: anodic alumina films is immersed liquor ferri trichloridi 0.5～3h, carry out vacuum drying after the taking-up; The concentration of described liquor ferri trichloridi can be 0.1～0.5mol/L; Described vacuum drying temperature can be 50～100 ℃, and the time can be 10～24h; The aperture of described anodic alumina films can be 0.1～0.8 μ m, and thickness can be 50～200 μ m, and porosity can be 40%～85%; The mass ratio of described anodic alumina films and N-2-carboxyethyl pyrrole monomer can be 1: (0.17～0.67); Described anodic alumina films preferably places vapor deposition polymerization device middle part, and described N-2-carboxyethyl pyrrole monomer preferably places the bottom of vapor deposition polymerization device; The described vacuum that vacuumizes back vapor deposition polymerization device is 0.01～0.1Pa; The condition of described vapor deposition polymerization reaction is: 110～180 ℃ of reaction temperatures, reaction time 4～10h.
In step 2) in, the described impurity available water of removing is washed the anodic alumina films surface repeatedly and it is carried out drying.
The present invention is basement membrane with the anodic alumina films, by the vapor deposition polymerization method, manually synthetic polyphosphazene polymer N-2-carboxyethyl pyrroles is coated in anodic alumina films surface and the hole wall, prepares poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film.
Prepared poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film has been covered the oxide layer on the anodic alumina films, has reduced its non-specific adsorption.Poly-N-2-carboxyethyl pyrroles has good electrical conductivity and biocompatibility, and itself has active function groups-COOH, make and to contain available in a large number-COOH on poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film and the fenestra, and need not additionally to introduce complex operating steps such as active group.The poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film of the present invention's preparation gets up the advantages of anodic alumina films and poly-this two classes material of N-2-carboxyethyl pyrroles, the preparation method is easy, can prepare the organic-inorganic compoiste affinity membrane base material of excellent performance by step of vapor deposition polymerization reaction, can be used for affine separation field behind the immobilized last aglucon, in affine separation, have widely and use.
Description of drawings
Fig. 1 is the stereoscan photograph of the prepared poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film of the embodiment of the invention 1.In Fig. 1, scale is 500nm.
The specific embodiment
The invention will be further described below by specific embodiment.
Embodiment 1
1) preliminary treatment of anodic oxidation aluminum-based film
Getting an aperture is that 0.2 μ m, thickness are that 60 μ m, porosity are 85% anodic alumina films, be dipped in the ferric chloride aqueous solutions 30min of 0.2mol/L, the film that will soak places the slow suction filtration ferric chloride aqueous solutions of filter 5 times then, then, film is placed 50 ℃ the dry 12h of vacuum drying chamber.
2) vapor deposition polymerization
The 0.12g anodic oxidation aluminum-based film that step 1) is handled well is fixed in the middle of the vapor phase growing apparatus, gets N-2-carboxyethyl pyrrole monomer 0.06g and places bottom of device, device is vacuumized after vacuum reaches 0.06Pa, in 150 ℃ of reaction 6h.
3) cleaning of film, preservation
Reaction finishes the back cool to room temperature, takes out the anodic oxidation aluminum-based film, with a large amount of deionized waters flushing membrane surface impurity repeatedly, after the drying at room temperature, promptly gets and gathers N-2-carboxyethyl pyrroles-anodised aluminum compound film.
Embodiment 2
1) preliminary treatment of anodic alumina films
Getting an aperture is that 0.8 μ m, thickness are that 200 μ m, porosity are 40% anodic alumina films, carries out preliminary treatment according to the preprocess method antianode pellumina of anodic alumina films among the embodiment 1.
2) vapor deposition polymerization
The 0.12g anodic alumina films that step 1) is handled well is fixed in the middle of the vapor phase growing apparatus, gets N-2-carboxyethyl pyrrole monomer 0.02g and places bottom of device, device is vacuumized after vacuum reaches 0.1Pa, in 180 ℃ of reaction 10h.
3) cleaning of film, preservation:
Method according to embodiment 1 is cleaned, is preserved, and promptly obtains poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film.
Embodiment 3
1) preliminary treatment of anodic alumina films:
Getting an aperture is that 0.3 μ m, thickness are that 150 μ m, porosity are 55% anodic alumina films, film is placed in the middle of the diffusion cell device that contains two ponds, the ferric chloride aqueous solutions that only adds the 0.5mol/L of 8mL therein in the pond, leave standstill 3h so that ferric trichloride diffuses through anodic alumina films automatically, then, film is placed 50 ℃ the dry 12h of vacuum drying chamber.
2) vapor deposition polymerization:
The 0.12g anodic alumina films that step 1) is handled well is fixed in the middle of the vapor phase growing apparatus, gets N-2-carboxyethyl pyrrole monomer 0.08g and places bottom of device, device is vacuumized after vacuum reaches 0.03Pa, in 160 ℃ of reaction 7h.
3) cleaning of film, preservation:
Method according to embodiment 1 is cleaned, is preserved, and promptly obtains poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film.
Embodiment 4
1) preliminary treatment of anodic alumina films
Getting an aperture is that 0.7 μ m, thickness are that 140 μ m, porosity are 45% anodic alumina films, carries out preliminary treatment according to the preprocess method antianode pellumina of anodic alumina films among the embodiment 3.
2) vapor deposition polymerization
The 0.12g anodic alumina films that step 1) is handled well is fixed in the middle of the vapor phase growing apparatus, gets N-2-carboxyethyl pyrrole monomer 0.10g and places bottom of device, device is vacuumized after vacuum reaches 0.01Pa, in 110 ℃ of reaction 4h.
3) cleaning of film, preservation:
Method according to embodiment 1 is cleaned, is preserved, and promptly obtains poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film.
Embodiment 5
1) preliminary treatment of anodic alumina films
Getting an aperture is that 0.55 μ m, thickness are that 120 μ m, porosity are 65% anodic alumina films, be placed in the obturator of a ferric chloride aqueous solutions that contains 0.1mol/L, decompression vacuum pumping then, places film 50 ℃ the dry 12h of vacuum drying chamber.
2) vapor deposition polymerization
Get the 0.12g anodic alumina films that step 1 handles well and be fixed in the middle of the vapor phase growing apparatus, 0.02g places bottom of device with N-2-carboxyethyl pyrrole monomer, device is vacuumized after vacuum reaches 0.08Pa, in 170 ℃ of reaction 10h.
3) cleaning of film, preservation
Method according to embodiment 1 is cleaned, is preserved, and promptly obtains poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film.
Embodiment 6
1) preliminary treatment of anodic alumina films:
Getting an aperture is that 0.1 μ m, thickness are that 50 μ m, porosity are 50% anodic alumina films, carries out preliminary treatment according to the preprocess method antianode pellumina of anodic alumina films among the embodiment 3.
2) vapor deposition polymerization:
The 0.12g anodic alumina films that step 1) is handled well is fixed in the middle of the vapor phase growing apparatus, gets N-2-carboxyethyl pyrrole monomer 0.08g and places bottom of device, device is vacuumized after vacuum reaches 0.1Pa, in 160 ℃ of reaction 5h.
3) cleaning of film, preservation:
Method according to embodiment 1 is cleaned, is preserved, and promptly obtains poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film.
Embodiment 7
1) preliminary treatment of anodic alumina films:
Getting an aperture is that 0.15 μ m, thickness are that 180 μ m, porosity are 80% anodic alumina films, carries out preliminary treatment according to the preprocess method antianode pellumina of anodic alumina films among the embodiment 5.
2) vapor deposition polymerization
Get the 0.12g anodic alumina films that step 1) handles well and be fixed in the middle of the vapor phase growing apparatus, 0.04g places bottom of device with N-2-carboxyethyl pyrrole monomer, device is vacuumized after vacuum reaches 0.05Pa, in 150 ℃ of reaction 7h.
3) cleaning of film, preservation:
Method according to embodiment 1 is cleaned, is preserved, and promptly obtains poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film.
Claims (9)
1. gather the preparation method of N-2-carboxyethyl pyrroles-anodised aluminum compound film, it is characterized in that comprising may further comprise the steps:
1) will place in the vapor deposition polymerization device through pretreated anodic alumina films and N-2-carboxyethyl pyrrole monomer, and described vapor deposition polymerization device will be vacuumized laggard promoting the circulation of qi phase deposition polymerization reaction;
2) reaction finishes the back cooling, removes impurity and promptly gets and gather N-2-carboxyethyl pyrroles-anodised aluminum compound film.
2. the preparation method of poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film as claimed in claim 1, it is characterized in that in step 1), described pretreated method is: anodic alumina films is immersed liquor ferri trichloridi 0.5～3h, carry out vacuum drying after the taking-up.
3. the preparation method of poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film as claimed in claim 2, the concentration that it is characterized in that described liquor ferri trichloridi is 0.1～0.5mol/L; Described vacuum drying temperature is 50～100 ℃, and the time is 10～24h.
4. the preparation method of poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film as claimed in claim 1, the aperture that it is characterized in that described anodic alumina films is 0.1～0.8 μ m, and thickness is 50～200 μ m, and porosity is 40%～85%.
5. the preparation method of poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film as claimed in claim 1 is characterized in that the mass ratio of described anodic alumina films and N-2-carboxyethyl pyrrole monomer is 1: 0.17～0.67.
6. the preparation method of poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film as claimed in claim 1, it is characterized in that described anodic alumina films places vapor deposition polymerization device middle part, described N-2-carboxyethyl pyrrole monomer places the bottom of vapor deposition polymerization device.
7. the preparation method of poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film as claimed in claim 1 is characterized in that the described vacuum that vacuumizes back vapor deposition polymerization device is 0.01～0.1Pa.
8. the preparation method of poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film as claimed in claim 1 is characterized in that the condition of described vapor deposition polymerization reaction is: 110～180 ℃ of reaction temperatures, reaction time 4～10h.
9. the preparation method of poly-N-2-carboxyethyl pyrroles-anodised aluminum compound film as claimed in claim 1 is characterized in that in step 2) described in to remove impurity be that water washes anodic alumina films surface repeatedly and it is carried out drying.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105688686A (en) * | 2016-03-10 | 2016-06-22 | 长春工业大学 | Preparation method of difunctional catalytic pervaporation composite membrane |
| CN107829330A (en) * | 2017-11-17 | 2018-03-23 | 哈尔滨工业大学 | A kind of preparation method of photo-thermal distillation film and the high-efficiency solar desalter containing photo-thermal distillation film |
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| CN101254415A (en) * | 2007-12-07 | 2008-09-03 | 厦门大学 | Preparation of gelatine-epoxy radicals silicone hydride-anodised aluminium compound film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101254415A (en) * | 2007-12-07 | 2008-09-03 | 厦门大学 | Preparation of gelatine-epoxy radicals silicone hydride-anodised aluminium compound film |
Non-Patent Citations (1)
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| 《中国优秀硕士学位论文全文数据库医药卫生科技辑》 20100115 曹慧慧 基于导电聚合物构建的亲和基础及其性能研究 , 第1期 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105688686A (en) * | 2016-03-10 | 2016-06-22 | 长春工业大学 | Preparation method of difunctional catalytic pervaporation composite membrane |
| CN105688686B (en) * | 2016-03-10 | 2018-07-06 | 长春工业大学 | The preparation method of double-function catalyzing osmosis vaporizing compound membrane |
| CN107829330A (en) * | 2017-11-17 | 2018-03-23 | 哈尔滨工业大学 | A kind of preparation method of photo-thermal distillation film and the high-efficiency solar desalter containing photo-thermal distillation film |
| CN107829330B (en) * | 2017-11-17 | 2020-05-05 | 哈尔滨工业大学 | Preparation method of photo-thermal distillation membrane and efficient solar desalination device containing photo-thermal distillation membrane |
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Application publication date: 20110615 |