CN105544096A - Method improving water stability of polyglutamic acid-Pullulan nanometer fiber film - Google Patents
Method improving water stability of polyglutamic acid-Pullulan nanometer fiber film Download PDFInfo
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- CN105544096A CN105544096A CN201510886796.XA CN201510886796A CN105544096A CN 105544096 A CN105544096 A CN 105544096A CN 201510886796 A CN201510886796 A CN 201510886796A CN 105544096 A CN105544096 A CN 105544096A
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- polyglutamic acid
- pulullan polysaccharide
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- fibrous membrane
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/12—Aldehydes; Ketones
- D06M13/123—Polyaldehydes; Polyketones
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to a method improving water stability of a polyglutamic acid-Pullulan nanometer fiber film; the method comprises the following steps: selecting polyglutamic acid with 400,000 molecular weight and 85% and Pullulan with 200,000 molecular weight and 94% purity as raw materials so as to respectively prepare solutions; mixing the solutions in proportion; using static spinning to prepare nanometer fiber film; crosslinking the nanometer fiber film so as to obtain the polyglutamic acid-Pullulan nanometer fiber film with good biology compatibility, thus improving the stability of the polyglutamic acid-Pullulan nanometer fiber film in the water environment, and providing latent application values in the material field; the method is simple in operation process, mild in technical conditions, and easy in raw material availability.
Description
Technical field
The present invention relates to the technical field of nanofiber film preparation, is a kind of method improving polyglutamic acid-pulullan polysaccharide nano fibrous membrane water stability specifically.
Background technology
Static Spinning (electrostaticspinning) refers to and utilizes electrostatic field force to make charged polymer solution or melt jet drawing-off in electrostatic field, forms the novel spinning method of micro-or nano size fiber.Electrostatic spinning technique has a series of advantage: first, the fiber diameter range obtained with electrostatic spinning technique is generally between nanometer to micron, much smaller than with the obtained fibre diameter of conventional method, and gained fiber has that porosity is high, specific area large, fiber fine degree and uniformity advantages of higher.These good characteristics that cannot obtain by conventional spinning method, impart electrostatic spinning fiber application prospect widely.Secondly, simply, fast, efficiently, equipment is easy to operation to electrostatic spinning process, can be used for preparation complexity, exempts to sew up support, and is easy to chemical constituent and the physical property of control fiber.
Gamma-polyglutamic acid-(γ-PGA) is the homopolymers of glutamic acid, can be produced by fermentable.γ-PGA is connected to form by one of glutamic acid amido link between amino and carboxyl, and its molecular weight (Mw) is 2 × 10
5-1 × 10
6da.γ-PGA does not have cumulative bad, Side effect.Due to the biocompatibility that it is good, biological degradability, avirulence and pollution-free, γ-PGA, as a kind of desirable biomaterial, has very large purposes at medical domain.Pulullan polysaccharide is the high molecular polymer combined by maltotriose by α-1,6 glycosidic bond, and its molecular weight (Mw) distribution is extensive, usually 4.8 × 10
4to 2.2 × 10
6da, pulullan polysaccharide possesses the nontoxic and characteristic of bio-safety because of it, is widely used in the fields such as medicine, food, cosmetics.Because gamma-polyglutamic acid-(γ-PGA) has good water-soluble, containing a large amount of hydrophilic radicals on pulullan polysaccharide strand, both are as bio-compatible, eco-friendly material, it is instant that the nano fibrous membrane prepared by electrostatic spinning technique meets water, therefore be necessary to be cross-linked it, to improve the stability in water.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method improving polyglutamic acid-pulullan polysaccharide nano fibrous membrane water stability.
The technical scheme that the present invention takes for the technical problem existed in solution known technology is:
The method improving polyglutamic acid-pulullan polysaccharide nano fibrous membrane water stability of the present invention, comprises the following steps:
(1) respectively configuration quality concentration be 40% polyglutamic acid solution and mass concentration be 20% pulullan polysaccharide solution, by above-mentioned two solution by polyglutamic acid: the volume ratio of pulullan polysaccharide=1:12 mixes, at spinning voltage 14kv, carry out electrostatic spinning under the condition of spinning distance 15cm, prepare nano fibrous membrane;
(2) glutaraldehyde and absolute ethyl alcohol are mixed with solution according to the volume ratio of 1:90 ~ 1:80, the concentration adding 0.1mL-0.2mL be again 98% the concentrated sulfuric acid stir after, nano fibrous membrane in step (1) is immersed in crosslinked 18-22h in mixed solution, reaction end is placed on dry 2h in drier, namely obtains the polyglutamic acid-pulullan polysaccharide nano fibrous membrane with water stability.
The present invention can also adopt following technical measures:
In step (1), polyglutamic acid molecular weight is 400,000, and purity is 85%; Pulullan polysaccharide molecular weight is 200,000, and purity is 94%.
The advantage that the present invention has and good effect are:
Of the present inventionly improve in the method for polyglutamic acid-pulullan polysaccharide nano fibrous membrane water stability, molecular weight is selected to be 400,000, purity be 85% polyglutamic acid and molecular weight be 200,000, purity be 94% pulullan polysaccharide be raw material, to be configured to after solution Homogeneous phase mixing in proportion respectively, by electrospun nanofibers film, again nano fibrous membrane is cross-linked, the polyglutamic acid obtained-pulullan polysaccharide nanometer fiber membrane biological compatibility is good, improve the polyglutamic acid-stability of pulullan polysaccharide nano fibrous membrane in water environment, at Material Field, there is potential using value, process operation is easy, process conditions are gentle, raw material are easy to get.
Detailed description of the invention
Below by way of specific embodiment, the technical scheme in the present invention is described in detail:
Embodiment 1:
The method improving polyglutamic acid-pulullan polysaccharide nano fibrous membrane water stability of the present invention, comprises the following steps:
(1) respectively configuration quality concentration be 40% polyglutamic acid solution and mass concentration be 20% pulullan polysaccharide solution, by above-mentioned two solution by polyglutamic acid: the volume ratio of pulullan polysaccharide=1:12 mixes, at spinning voltage 14kv, carry out electrostatic spinning under the condition of spinning distance 15cm, prepare nano fibrous membrane;
(2) by glutaraldehyde and the absolute ethyl alcohol volume ratio according to 1:88, i.e. glutaraldehyde 1mL, ethanol 88mL, be mixed with solution, the concentration adding 0.1mL be again 98% the concentrated sulfuric acid stir after, nano fibrous membrane is immersed in crosslinked 22h in mixed solution, reaction end is placed on dry 2h in drier, namely obtains the polyglutamic acid-pulullan polysaccharide nano fibrous membrane with water stability.
In raw material, polyglutamic acid molecular weight is 400,000, and purity is 85%; Pulullan polysaccharide molecular weight is 200,000, and purity is 94%.
Measured and contact angle determination discovery by SEM, fibre diameter, uncrosslinked polyglutamic acid-pulullan polysaccharide nanofiber surface is smooth without beading, be cross-linked and closely form network structure, diameter is less is 144nm, after crosslinked, average fibre diameter is all large than uncrosslinked fiber, is 189nm, but even have fiber adhesion to occur, the result of contact angle determination is 36 ° and becomes 65 °.
Embodiment 2:
The method improving polyglutamic acid-pulullan polysaccharide nano fibrous membrane water stability of the present invention, comprises the following steps:
(1) respectively configuration quality concentration be 40% polyglutamic acid solution and mass concentration be 20% pulullan polysaccharide solution, by above-mentioned two solution by polyglutamic acid: the volume ratio of pulullan polysaccharide=1:12 mixes, at spinning voltage 14kv, carry out electrostatic spinning under the condition of spinning distance 15cm, prepare nano fibrous membrane;
(2) by glutaraldehyde and the absolute ethyl alcohol volume ratio according to 1:80, i.e. glutaraldehyde 1mL, ethanol 80mL, be mixed with solution, the concentration adding 0.15mL be again 98% the concentrated sulfuric acid stir after, nano fibrous membrane is immersed in crosslinked 20h in mixed solution, reaction end is placed on dry 2h in drier, namely obtains the polyglutamic acid-pulullan polysaccharide nano fibrous membrane with water stability.
In raw material, polyglutamic acid molecular weight is 400,000, and purity is 85%; Pulullan polysaccharide molecular weight is 200,000, and purity is 94%.
Measured and contact angle determination discovery by SEM, fibre diameter, uncrosslinked polyglutamic acid-pulullan polysaccharide nanofiber surface is smooth without beading, be cross-linked and closely form network structure, diameter is less is 144nm, after crosslinked, average fibre diameter is all large than uncrosslinked fiber, is 190nm, but even have fiber adhesion to occur, the result of contact angle determination is 36 ° and becomes 68 °.
Embodiment 3:
The method improving polyglutamic acid-pulullan polysaccharide nano fibrous membrane water stability of the present invention, comprises the following steps:
(1) respectively configuration concentration to be mass concentration be 40% polyglutamic acid solution and mass concentration be 20% pulullan polysaccharide solution, by above-mentioned two solution by polyglutamic acid: the volume ratio of pulullan polysaccharide=1:12 mixes, at spinning voltage 14kv, carry out electrostatic spinning under the condition of spinning distance 15cm, prepare nano fibrous membrane;
(2) by glutaraldehyde and the absolute ethyl alcohol volume ratio according to 1:90, i.e. glutaraldehyde 1mL, ethanol 90mL, be mixed with solution, the concentration adding 0.12mL be again 98% the concentrated sulfuric acid stir after, nano fibrous membrane is immersed in crosslinked 18h in mixed solution, reaction end is placed on dry 2h in drier, namely obtains the polyglutamic acid-pulullan polysaccharide nano fibrous membrane with water stability.
In raw material, polyglutamic acid molecular weight is 400,000, and purity is 85%; Pulullan polysaccharide molecular weight is 200,000, and purity is 94%.
Measured and contact angle determination discovery by SEM, fibre diameter, uncrosslinked polyglutamic acid-pulullan polysaccharide nanofiber surface is smooth without beading, be cross-linked and closely form network structure, diameter is less is 144nm, after crosslinked, average fibre diameter is all large than uncrosslinked fiber, is 190nm, but even have fiber adhesion to occur, the result of contact angle determination is 36 ° and becomes 69 °.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, although the present invention with preferred embodiment openly as above, but, and be not used to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, certainly the technology contents of announcement can be utilized to make a little change or modification, become the Equivalent embodiments of equivalent variations, in every case be the content not departing from technical solution of the present invention, according to any simple modification that technical spirit of the present invention is done above embodiment, equivalent variations and modification, all belong in the scope of technical solution of the present invention.
Claims (2)
1. improve a method for polyglutamic acid-pulullan polysaccharide nano fibrous membrane water stability, comprise the following steps:
(1) respectively configuration quality concentration be 40% polyglutamic acid solution and mass concentration be 20% pulullan polysaccharide solution, by above-mentioned two solution by polyglutamic acid: the volume ratio of pulullan polysaccharide=1:12 mixes, at spinning voltage 14kv, carry out electrostatic spinning under the condition of spinning distance 15cm, prepare nano fibrous membrane;
(2) glutaraldehyde and absolute ethyl alcohol are mixed with solution according to the volume ratio of 1:90 ~ 1:80, the concentration adding 0.1mL-0.2mL be again 98% the concentrated sulfuric acid stir after, nano fibrous membrane in step (1) is immersed in crosslinked 18-22h in mixed solution, reaction end is placed on dry 2h in drier, namely obtains the polyglutamic acid-pulullan polysaccharide nano fibrous membrane with water stability.
2. the method improving polyglutamic acid-pulullan polysaccharide nano fibrous membrane water stability according to claim 1, it is characterized in that: in step (1), polyglutamic acid molecular weight is 400,000, and purity is 85%; Pulullan polysaccharide molecular weight is 200,000, and purity is 94%.
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| CN201510886796.XA CN105544096A (en) | 2015-12-07 | 2015-12-07 | Method improving water stability of polyglutamic acid-Pullulan nanometer fiber film |
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| CN201510886796.XA CN105544096A (en) | 2015-12-07 | 2015-12-07 | Method improving water stability of polyglutamic acid-Pullulan nanometer fiber film |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102277659A (en) * | 2011-07-20 | 2011-12-14 | 东华大学 | Preparation method of water stability gamma-polyglutamic acid nanometer fibers |
| CN103013106A (en) * | 2013-01-10 | 2013-04-03 | 天津工业大学 | Preparation method of gamma-polyglutamic acid/Pulullan composite hydrogel |
| WO2014160019A1 (en) * | 2013-03-14 | 2014-10-02 | Lifenet Health | Aligned fiber and method of use thereof |
| CN104611783A (en) * | 2015-01-27 | 2015-05-13 | 大连工业大学 | Method for preparing nanofiber by electrostatic spinning, nanofiber obtained with method and application of nanofiber |
| CN104762753A (en) * | 2014-12-26 | 2015-07-08 | 天津北洋百川生物技术有限公司 | Preparation method of gamma-polyglutamic pullulan nanometer fiber film of load drug |
-
2015
- 2015-12-07 CN CN201510886796.XA patent/CN105544096A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102277659A (en) * | 2011-07-20 | 2011-12-14 | 东华大学 | Preparation method of water stability gamma-polyglutamic acid nanometer fibers |
| CN103013106A (en) * | 2013-01-10 | 2013-04-03 | 天津工业大学 | Preparation method of gamma-polyglutamic acid/Pulullan composite hydrogel |
| WO2014160019A1 (en) * | 2013-03-14 | 2014-10-02 | Lifenet Health | Aligned fiber and method of use thereof |
| CN104762753A (en) * | 2014-12-26 | 2015-07-08 | 天津北洋百川生物技术有限公司 | Preparation method of gamma-polyglutamic pullulan nanometer fiber film of load drug |
| CN104611783A (en) * | 2015-01-27 | 2015-05-13 | 大连工业大学 | Method for preparing nanofiber by electrostatic spinning, nanofiber obtained with method and application of nanofiber |
Non-Patent Citations (1)
| Title |
|---|
| 孙晓斌等: "普鲁兰多糖纳米纤维膜制备及交联工艺研究", 《合成纤维》 * |
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