CN1189236C - Preparation method of nylon-shell glycan compound film for affinity microfilter - Google Patents
Preparation method of nylon-shell glycan compound film for affinity microfilter Download PDFInfo
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- CN1189236C CN1189236C CNB021309264A CN02130926A CN1189236C CN 1189236 C CN1189236 C CN 1189236C CN B021309264 A CNB021309264 A CN B021309264A CN 02130926 A CN02130926 A CN 02130926A CN 1189236 C CN1189236 C CN 1189236C
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Abstract
The present invention discloses a preparation method of a nylon-chitosan compound film for an affinity microfilter. In the method, a nylon film with the hole diameter of 0.4 to 3 mu m is used as a basal film activated through a formaldehyde solution, a double-epoxy alkane solution, a carbonyldiimidazole solution, a glutaraldehyde solution and an epoxy chloropropane solution which are activating agents, the activation temperature is from 20 DEG C to 90 DEG C, active groups are generated, is further coupled with chitosan and then is cleaned, and then a nylon-chitosan compound film is formed. The present invention is characterized in that the activated film and 1% to 3% of chitosan acidic solution with the pH of 2 to 5 generate reaction to couple with the chitosan, and then the nylon-chitosan compound film is formed. The compound film prepared by the present invention has the advantages of favorable mechanical property and chemical stability, good hydrophilicity, low nonspecific adsorption and good biocompatibility, and can be widely used for the affinity microfiltration and separation of biological matter, and the quantity of the active groups is from 8 to 10 times higher than that of the original nylon film.
Description
Technical field
The present invention relates to a kind of preparation method who is used for the nylon-chitosan complex film of affine micro-filtration, belong to the technology of preparing of micro-filtration composite membrane.
Background technology
Affine micro-filtration mainly is based on the biologic specificity of desiring separate substance and being bonded between the affine dentate on the film and interacts, and realizes the separation to object.The employed filter membrane of affine micro-filtration should have good chemical stability, excellent in chemical reactivity worth and not influence activity of biological substance etc.The modification of nylon film is to be applied to the comparatively desirable filter membrane of affine micro-filtration at present.Beeskow etc. with the hydroxyethylcellulose covalent bonding on the surface and hole wall of nylon membrane, introduced active-OH base on the made composite membrane, the high 3-5 of active group quantity times of [Beeskow TC than original nylon membrane, Kusharyoto W, Anspach FB, et al.Surfacemodification of microporous polyamide membranes with hydroxyethylcellulose and their application as affinity membranes.Journal ofChromatography A, 1995,715:49-65].The nylon of inventions such as Castilho-agarose composite membrane and nylon-composite membrane of polyvinyl alcohol have improved the hydrophilicity of film significantly and have effectively reduced by the caused non-specific adsorption of ion-exchange sites [Castilho LR, Deckwer W-D and Anspach FB.Influence of matrix activation and polymer coating on purification ofhuman IgG with protein A affinity membranes.Journal of Membrane Science, 2000,172:269-277].The hydrophilicity of above-mentioned composite membrane is good, and non-specific adsorption is low, but active group quantity awaits further raising on the film.
Summary of the invention
The object of the present invention is to provide a kind of preparation method who is used for the nylon-chitosan complex film of affine micro-filtration.The prepared composite membrane of Using such method has-NH
2Base and-2 kinds of active groups of OH base, than the high 8-10 of active group quantity of original nylon membrane doubly, and have good hydrophilicity energy and good biocompatibility and blood compatibility.This composite membrane can be widely used in the separation and the purifying of biological substance.
The present invention is realized by following technical proposals: the nylon membrane that with the aperture is 0.4-3 μ m is a basement membrane, through formaldehyde, bis-epoxy alkane, carbonyl dimidazoles, glutaraldehyde or epoxychloropropane solution is the activator activation, activation temperature 20-90 ℃, produce active group, and then coupled chitosan, again through cleaning post processing, form nylon-chitosan complex film, it is characterized in that: film after the activation and the pH 1-3% shitosan acid solution between 2-5 forms nylon-chitosan complex film at 20-50 ℃ of reaction-coupling shitosan.
Above-mentioned shitosan acid solution is the hydrochloric acid solution of shitosan, the acetic acid solution of shitosan or the phosphoric acid solution of shitosan.
Above-mentioned shitosan acid solution pH value is 2-3.
Film after the above-mentioned activation and shitosan acid solution reaction temperature are 30-40 ℃.
Prepared nylon-the chitosan complex film of the present invention has favorable mechanical performance and chemical stability, and hydrophilicity is good, and non-specific adsorption is low, and biocompatibility and blood compatibility are good, and active group quantity than the high 8-10 of original nylon membrane doubly and has-NH
2With-two kinds of active groups of OH, for the further immobilized dentate of this film is provided convenience.This composite membrane can be widely used in affine micro-filtration separating bio material.
The specific embodiment
Embodiment one:
1. the activation of nylon membrane
Get in the NaOH solution that 5 milliliters of epoxychloropropane join 10 milliliters of 1M.With 3 nylon membranes, the aperture is 0.45 μ m, and diameter is 47mm, puts into this solution, under 70 ℃, and oscillating reactions 20 hours, and under room temperature, cleaned 30 minutes with distilled water.
2. coupling shitosan
Get 1 of the activation film of step 1 preparation, place 2% shitosan acetic acid solution, the concentration of acetic acid solution is 10% (volume).Under 40 ℃, oscillating reactions 5 hours.Take out this film and place on the decompress filter device, the solution on film surface is blotted, in 100 ℃ baking oven dry 1 hour.
3. the cleaning of film and preservation
Get the composite membrane of step 2 preparation, successively use the acetic acid solution cleaning 1 hour and the distilled water of 1% (volume) to clean 24 hours.Film is taken out in 80 ℃ of oven dryings 30 minutes, and air drying is preserved, and promptly gets nylon-chitosan complex film.
Embodiment two:
1. the activation of nylon membrane
Get 1 of nylon membrane, the aperture is 2 μ m, and diameter is 47mm, places the acetone soln of 10 milliliter 1.5% carbonyl dimidazoles, and under room temperature, oscillating reactions 1 hour is cleaned 3 times with acetone, and places 60 ℃ of baking ovens dry 30 minutes.
2. coupling shitosan
The activation film of step 1 preparation is placed shitosan acetate-sodium acetate solution of 2%, and the pH value of acetate-sodium acetate buffer is 5.4.Under room temperature, oscillating reactions 5 hours.Take out this film and place on the decompress filter device, the solution on film surface is blotted, in 60 ℃ of baking ovens dry 45 minutes.
Method according to embodiment one is cleaned, is preserved, and promptly gets nylon-chitosan complex film.
Embodiment three:
1. the activation of nylon membrane
Get 3 of nylon membranes, the aperture is 1 μ m, and diameter is that 47mm places 10 milliliter 36.5% formalin, drips 0.1 milliliter 85% phosphoric acid, and under 60 ℃, oscillating reactions 7 hours was cleaned 45 minutes down at 50 ℃ with distilled water.
2. coupling shitosan
The activation film of step 1 preparation is placed 2% the shitosan acetic acid solution of pH2, and acetic acid solution concentration is 1% (volume), under 30 ℃, and oscillating reactions 30 minutes.Take out this film and place on the decompress filter device, the solution on film surface is blotted, in 80 ℃ of baking ovens dry 30 minutes.
Method according to embodiment one is cleaned, is preserved, and promptly gets nylon-chitosan complex film.
Claims (4)
1. preparation method who is used for the nylon-chitosan complex film of affine micro-filtration, this method is that the nylon membrane of 0.4-3 μ m is a basement membrane with the aperture, through formaldehyde, bis-epoxy alkane, carbonyl dimidazoles, glutaraldehyde or epoxychloropropane solution is the activator activation, activation temperature 20-90 ℃, produce active group, and then coupled chitosan, again through cleaning post processing, form nylon-chitosan complex film, it is characterized in that: film after the activation and the pH 1-3% shitosan acid solution between 2-5 forms nylon-chitosan complex film at 20-50 ℃ of reaction-coupling shitosan.
2. by the described preparation method who is used for the nylon-chitosan complex film of affine micro-filtration of claim 1, it is characterized in that: the shitosan acid solution is the hydrochloric acid solution of shitosan, the acetic acid solution of shitosan or the phosphoric acid solution of shitosan.
3. by the described preparation method who is used for the nylon-chitosan complex film of affine micro-filtration of claim 1, it is characterized in that: the pH value of shitosan acid solution is 2-3.
4. by the described preparation method who is used for the nylon-chitosan complex film of affine micro-filtration of claim 1, it is characterized in that: film after the activation and shitosan acid solution reaction temperature are 30-40 ℃.
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CNB021309264A CN1189236C (en) | 2002-09-17 | 2002-09-17 | Preparation method of nylon-shell glycan compound film for affinity microfilter |
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CNB021309264A CN1189236C (en) | 2002-09-17 | 2002-09-17 | Preparation method of nylon-shell glycan compound film for affinity microfilter |
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CN1189236C true CN1189236C (en) | 2005-02-16 |
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Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100348302C (en) * | 2004-05-14 | 2007-11-14 | 华南理工大学 | Method for preparing water-soluble affinity ultrafiltration carrier |
CN100531872C (en) * | 2007-08-03 | 2009-08-26 | 厦门大学 | Method for preparing polypyrole-polycarbonate composite membrane of fixed load cibacron blue |
CN101125934B (en) * | 2007-09-30 | 2010-05-19 | 四川大学 | Method for preparing chitosan/nylon composite antibacterial film containing silver ion |
CN101249990B (en) * | 2008-03-11 | 2010-06-09 | 东华大学 | Method for rapidly removing metal copper ion from waste water |
CN101880403A (en) * | 2010-07-02 | 2010-11-10 | 深圳市科聚新材料有限公司 | Method for preparing nylon surface grafting chitosan hydrophilic antibiotic material |
CN102773028A (en) * | 2012-05-09 | 2012-11-14 | 江苏维赛科技生物发展有限公司 | Method for preparing hybond-N plus surface cross-linking chitosan modified membrane material |
CN102652904A (en) * | 2012-05-09 | 2012-09-05 | 江苏维赛科技生物发展有限公司 | Preparation method of PVDF (polyvinylidene fluoride) membrane surface crosslinked chitosan hydrophilic membrane |
CN108160056B (en) * | 2017-12-28 | 2020-12-18 | 大连海洋大学 | Preparation method of nylon membrane for adsorbing heavy metals |
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