CN102425039A - Method for preparing water-soluble chitosan fibrous membrane - Google Patents
Method for preparing water-soluble chitosan fibrous membrane Download PDFInfo
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- CN102425039A CN102425039A CN2011102876488A CN201110287648A CN102425039A CN 102425039 A CN102425039 A CN 102425039A CN 2011102876488 A CN2011102876488 A CN 2011102876488A CN 201110287648 A CN201110287648 A CN 201110287648A CN 102425039 A CN102425039 A CN 102425039A
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Abstract
The invention relates to a method for preparing a water-soluble chitosan fibrous membrane. The method comprises the following steps of: dissolving water-soluble chitosan in a mixed solvent of water and ethanol to prepare a solution, and standing and carrying out ultrasonic treatment on the solution for 1 hour for completely separating out bubbles so as to obtain a water-soluble chitosan solution; and adding the prepared water-soluble chitosan electrostatic spinning solution into an injection pump, and carrying out electrostatic spinning to an aluminum foil in a temperature range of 10-40 DEG C while properly adjusting the spinning voltage, the distance from a spinning nozzle to a collecting board and the flow of a spinning solution at the spinning nozzle, so as to obtain the water-soluble chitosan nano fibrous membrane. According to the method provided by the invention, water-soluble chitosan is used as a raw material, an irritant solvent is not used, the biocompatibility of the obtained nano fibrous membrane is increased and the application range of the chitosan nano fibrous membrane is enlarged.
Description
Technical field
The present invention relates to a kind of method for preparing the water soluble chitosan tunica fibrosa.
Background technology
Shitosan [CS, chitosan, (1,4)-2-amino-2-deoxidation-β-D-glucose] is to take off a kind of linear macromolecule material that obtains after acetyl is handled by the natural polymer chitin, is a kind of natural biological macromolecular material with many advantageous properties.CS is owing to but characteristics such as its good antibiotic property and biocompatibility, inanimate object toxicity and Natural Degradation are widely used in biomedicine field.But CS can only be dissolved in the dilute acid soln of minority, can't be directly soluble in water, this big limitations the Application of Chitosan scope, people carry out chemical modification to amino or hydroxyl on the chitosan molecule chain and have obtained water soluble chitosan for this reason.Water soluble chitosan can directly be dissolved in the system of neutral and weakly acidic water environment, has greatly promoted CS as tissue engineering bracket material, drug carrier material and the application of wound repair material under the human body fluid environment.
The electricity spining technology is to utilize high-pressure electrostatic with polymer or have a kind of process technology that viscoelastic formulations prepared from solutions becomes the nanometer grade diameter fiber.Spinning solution receives the high-pressure electrostatic effect and has electric charge at spinning nozzle, and the mutual repulsion of surface charge makes liquid jet penetrate and obtain to stretch from spinning nozzle, is accompanied by the volatilization of solvent and solidifies, and finally on gatherer, obtains fiber.Initial electric spining technology is mainly used in preparation synthetic polymer nanofiber.Can a large amount of natural polymers be prepared into nanofiber through electrostatic spinning technique now.The electricity spinning fibre film is because its high-specific surface area, good bionic performance, carry at bioengineered tissue support, medicine release, there is higher using value aspect such as wound repair.CS is a kind of polycation natural polyelectrolyte, and strand is rigidity and owing to repels each other between the polyelectrolyte characteristic strand.Thereby be difficult to prepare into nano fibrous membrane owing to lacking necessary chain entanglement property through electrical spinning method for pure CS system.Through blending method with CS and synthetic high polymer such as polyethylene glycol oxide (PEO) or polyvinyl alcohol blend such as (PVA) after, prepare into nano fibrous membrane (Chinese patent CN1569254A) through electrical spinning method.Or through the cosolvent method regulate the spinning system parameter such as surface tension, electrical conductivity, viscosity and spinning technology parameter such as voltage, extruded velocity, put flight lead and leave etc. and to obtain CS nano fibrous membrane (Carbohydrate Polymers 77 (2009) 656-661; Macromol.Rapid Commun.2004,25,1600-1605).These methods are dissolved CS mostly in acid system, especially the cosolvent method must add concentration formic acid and high to reduce surface tension.Can there be small amount of residual in these acid in the CS tunica fibrosa of preparation, and influence the CS tunica fibrosa biocompatibility, increase its bio-toxicity, and then limited the range of application of CS.
The water-soluble CS that the present invention passes through to adopt modification through selecting suitable spinning process condition, has prepared good biocompatibility, nontoxic and biodegradable CS nano fibrous membrane as raw material.This tunica fibrosa all has higher using value at aspects such as organizational project, wound repair, medicament transport.
Summary of the invention
To the water soluble chitosan nano fibrous membrane of present preparation all in acid system electrostatic spinning obtain, the object of the present invention is to provide a kind of method for preparing the water soluble chitosan nano fibrous membrane.This method operating process mild condition, be easy to control, step is simple, with low cost.
A kind of method for preparing the water soluble chitosan nano fibrous membrane provided by the present invention may further comprise the steps:
(1) preparation of water soluble chitosan electricity spinning solution: in the water soluble chitosan powder is water-soluble, that ethanol the is formed mixed solvent; Be made into the solution that percentage by weight is 1～5wt%; Then solution is fully stirred; So that dissolving made bubble all separate out in 1 hour the solution left standstill ultrasonic wave and promptly obtains transparent water soluble chitosan solution fully.Described water soluble chitosan weight average molecular weight is 100,000～200,000, and the volume ratio of aqueous solvent, ethanol is 80/20～60/40.
(2) electrostatic spinning prepares the water soluble chitosan nanofiber: the water soluble chitosan electrostatic spinning solution of preparation in the step (1) is added syringe pump, and adjustment voltage is 15～30kV; Spinning head is to the distance 8～20cm of collecting board; The flow of spinning head spinning solution is 0.5～2.0mL/h; The spinning environment temperature is 10～40 ℃; Starting drive carries out the electrostatic spinning of water soluble chitosan, on collecting board, has obtained the water soluble chitosan nano fiber non-woven fabric, and distribution of fiber diameters is even, and fibre diameter is between 200nm～600nm.
Compared with prior art, the inventive method has the following advantages:
1) nanofiber that obtains of the inventive method, the tiny (200nm～600nm) of fibre diameter;
2) the inventive method is low for equipment requirements, and gathering-device, postprocessing working procedures are simple, have reduced cost;
3) the present invention adopts water-soluble CS system, does not contain the excitant solvent in the system, and gained nanometer fiber membrane biological compatibility is good.
Description of drawings
Fig. 1 is the nanofiber sem photograph by embodiment 1 preparation gained water soluble chitosan;
The specific embodiment
Embodiment 1
1) compound concentration is the aqueous solution of the ethanol of 20wt%;
2) be that 100,000 water soluble chitosan powder are distributed in the step 1) solution with weight average molecular weight, be made into the solution that percentage by weight is 1wt%;
3) then with step 2) in solution fully stir so that fully the dissolving, bubble is all separated out the solution left standstill ultrasonic wave and promptly obtains transparent hyaluronic acid solution;
4) solution in the step 3) is added syringe pump, adjustment voltage is 15kV; Spinning head is that the flow of 8cm spinning head spinning solution is 1mL/h to the distance of collecting board; The spinning environment temperature is 30 ℃;
5) starting drive carries out the electrostatic spinning of water soluble chitosan; Can on device, obtain good biocompatibility, nontoxic and biodegradable CS nano fibrous membrane on the collecting board, this tunica fibrosa all has higher using value at aspects such as organizational project, wound repair, medicament transport.
Embodiment 2
1) compound concentration is the aqueous solution of the ethanol of 20wt%;
2) be that 150,000 water soluble chitosan powder are distributed in the step 1) solution with weight average molecular weight, be made into the solution that percentage by weight is 1wt%;
3) then with step 2) in solution fully stir so that fully the dissolving, bubble is all separated out the solution left standstill ultrasonic wave and promptly obtains transparent hyaluronic acid solution;
4) solution in the step 3) is added syringe pump, adjustment voltage is 15kV; Spinning head is 8cm to the distance of collecting board; The flow of spinning head spinning solution is 1mL/h; The spinning environment temperature is 30 ℃;
5) starting drive carries out the electrostatic spinning of water soluble chitosan; Can on device, obtain good biocompatibility, nontoxic and biodegradable CS nano fibrous membrane on the collecting board, this tunica fibrosa all has higher using value at aspects such as organizational project, wound repair, medicament transport.
Embodiment 3
1) compound concentration is the aqueous solution of the ethanol of 20wt%;
2) be that 200,000 water soluble chitosan powder are distributed in the step 1) solution with weight average molecular weight, be made into the solution that percentage by weight is 1wt%;
3) then with step 2) in solution fully stir so that fully the dissolving, bubble is all separated out the solution left standstill ultrasonic wave and promptly obtains transparent hyaluronic acid solution;
4) solution in the step 3) is added syringe pump, adjustment voltage is 15kV; Spinning head is 8cm to the distance of collecting board; The flow of spinning head spinning solution is 1mL/h; The spinning environment temperature is 30 ℃;
5) starting drive carries out the electrostatic spinning of water soluble chitosan; Can on device, obtain good biocompatibility, nontoxic and biodegradable CS nano fibrous membrane on the collecting board, this tunica fibrosa all has higher using value at aspects such as organizational project, wound repair, medicament transport.
Embodiment 4
1) compound concentration is the aqueous solution of the ethanol of 20wt%;
2) be that 150,000 water soluble chitosan powder are distributed in the step 1) solution with weight average molecular weight, be made into the solution that percentage by weight is 3wt%;
3) then with step 2) in solution fully stir so that fully the dissolving, bubble is all separated out the solution left standstill ultrasonic wave and promptly obtains transparent hyaluronic acid solution;
4) solution in the step 3) is added syringe pump, adjustment voltage is 15kV; Spinning head is 8cm to the distance of collecting board; The flow of spinning head spinning solution is 1mL/h; The spinning environment temperature is 30 ℃;
5) starting drive carries out the electrostatic spinning of water soluble chitosan; Can on device, obtain good biocompatibility, nontoxic and biodegradable CS nano fibrous membrane on the collecting board, this tunica fibrosa all has higher using value at aspects such as organizational project, wound repair, medicament transport.
Embodiment 5
1) compound concentration is the aqueous solution of the ethanol of 20wt%;
2) be that 150,000 water soluble chitosan powder are distributed in the step 1) solution with weight average molecular weight, be made into the solution that percentage by weight is 5wt%;
3) then with step 2) in solution fully stir so that fully the dissolving, bubble is all separated out the solution left standstill ultrasonic wave and promptly obtains transparent hyaluronic acid solution;
4) solution in the step 3) is added syringe pump, adjustment voltage is 15kV; Spinning head is 8cm to the distance of collecting board; The flow of spinning head spinning solution is 1mL/h; The spinning environment temperature is 30 ℃;
5) starting drive carries out the electrostatic spinning of water soluble chitosan; Can on device, obtain good biocompatibility, nontoxic and biodegradable CS nano fibrous membrane on the collecting board, this tunica fibrosa all has higher using value at aspects such as organizational project, wound repair, medicament transport.
Embodiment 6
1) compound concentration is the aqueous solution of the ethanol of 30wt%;
2) be that 150,000 water soluble chitosan powder are distributed in the step 1) solution with weight average molecular weight, be made into the solution that percentage by weight is 3wt%;
3) then with step 2) in solution fully stir so that fully the dissolving, bubble is all separated out the solution left standstill ultrasonic wave and promptly obtains transparent hyaluronic acid solution;
4) solution in the step 3) is added syringe pump, adjustment voltage is 15kV; Spinning head is 8cm to the distance of collecting board; The flow of spinning head spinning solution is 1mL/h; The spinning environment temperature is 30 ℃;
5) starting drive carries out the electrostatic spinning of water soluble chitosan; Can on device, obtain good biocompatibility, nontoxic and biodegradable CS nano fibrous membrane on the collecting board, this tunica fibrosa all has higher using value at aspects such as organizational project, wound repair, medicament transport.
Embodiment 7
1) compound concentration is the aqueous solution of the ethanol of 40wt%;
2) be that 150,000 water soluble chitosan powder are distributed in the step 1) solution with weight average molecular weight, be made into the solution that percentage by weight is 3wt%;
3) then with step 2) in solution fully stir so that fully the dissolving, bubble is all separated out the solution left standstill ultrasonic wave and promptly obtains transparent hyaluronic acid solution;
4) solution in the step 3) is added syringe pump, adjustment voltage is 15kV; Spinning head is 8cm to the distance of collecting board; The flow of spinning head spinning solution is 1mL/h; The spinning environment temperature is 30 ℃;
5) starting drive carries out the electrostatic spinning of water soluble chitosan; Can on device, obtain good biocompatibility, nontoxic and biodegradable CS nano fibrous membrane on the collecting board, this tunica fibrosa all has higher using value at aspects such as organizational project, wound repair, medicament transport.
Embodiment 8
1) compound concentration is the aqueous solution of the ethanol of 20wt%;
2) be that 150,000 water soluble chitosan powder are distributed in the step 1) solution with weight average molecular weight, be made into the solution that percentage by weight is 3wt%;
3) then with step 2) in solution fully stir so that fully the dissolving, bubble is all separated out the solution left standstill ultrasonic wave and promptly obtains transparent hyaluronic acid solution;
4) solution in the step 3) is added syringe pump, adjustment voltage is 15kV; Spinning head is that the flow of 8cm spinning head spinning solution is 0.5mL/h to the distance of collecting board; The spinning environment temperature is 30 ℃;
5) starting drive carries out the electrostatic spinning of water soluble chitosan; Can on device, obtain good biocompatibility, nontoxic and biodegradable CS nano fibrous membrane on the collecting board, this tunica fibrosa all has higher using value at aspects such as organizational project, wound repair, medicament transport.
Embodiment 9
1) compound concentration is the aqueous solution of the ethanol of 20wt%;
2) be that 150,000 water soluble chitosan powder are distributed in the step 1) solution with weight average molecular weight, be made into the solution that percentage by weight is 3wt%;
3) then with step 2) in solution fully stir so that fully the dissolving, bubble is all separated out the solution left standstill ultrasonic wave and promptly obtains transparent hyaluronic acid solution;
4) solution in the step 3) is added syringe pump, adjustment voltage is 15kV; Spinning head is 8cm to the distance of collecting board; The flow of spinning head spinning solution is 2mL/h; The spinning environment temperature is 30 ℃;
5) starting drive carries out the electrostatic spinning of water soluble chitosan; Can on device, obtain good biocompatibility, nontoxic and biodegradable CS nano fibrous membrane on the collecting board, this tunica fibrosa all has higher using value at aspects such as organizational project, wound repair, medicament transport.
Embodiment 10
1) compound concentration is the aqueous solution of the ethanol of 20wt%;
2) be that 150,000 water soluble chitosan powder are distributed in the step 1) solution with weight average molecular weight, be made into the solution that percentage by weight is 3wt%;
3) then with step 2) in solution fully stir so that fully the dissolving, bubble is all separated out the solution left standstill ultrasonic wave and promptly obtains transparent hyaluronic acid solution;
4) solution in the step 3) is added syringe pump, adjustment voltage is 25kV; Spinning head is 8cm to the distance of collecting board; The flow of spinning head spinning solution is 1mL/h; The spinning environment temperature is 30 ℃;
5) starting drive carries out the electrostatic spinning of water soluble chitosan; Can on device, obtain good biocompatibility, nontoxic and biodegradable CS nano fibrous membrane on the collecting board, this tunica fibrosa all has higher using value at aspects such as organizational project, wound repair, medicament transport.
Embodiment 11
1) compound concentration is the aqueous solution of the ethanol of 20wt%;
2) be that 150,000 water soluble chitosan powder are distributed in the step 1) solution with weight average molecular weight, be made into the solution that percentage by weight is 3wt%;
3) then with step 2) in solution fully stir so that fully the dissolving, bubble is all separated out the solution left standstill ultrasonic wave and promptly obtains transparent hyaluronic acid solution;
4) solution in the step 3) is added syringe pump, adjustment voltage is 30kV; Spinning head is 8cm to the distance of collecting board; The flow of spinning head spinning solution is 1mL/h; The spinning environment temperature is 30 ℃;
5) starting drive carries out the electrostatic spinning of water soluble chitosan; Can on device, obtain good biocompatibility, nontoxic and biodegradable CS nano fibrous membrane on the collecting board, this tunica fibrosa all has higher using value at aspects such as organizational project, wound repair, medicament transport.
Embodiment 12
1) compound concentration is the aqueous solution of the ethanol of 20wt%;
2) be that 150,000 water soluble chitosan powder are distributed in the step 1) solution with weight average molecular weight, be made into the solution that percentage by weight is 3wt%;
3) then with step 2) in solution fully stir so that fully the dissolving, bubble is all separated out the solution left standstill ultrasonic wave and promptly obtains transparent hyaluronic acid solution;
4) solution in the step 3) is added syringe pump, adjustment voltage is 15kV; Spinning head is 15cm to the distance of collecting board; The flow of spinning head spinning solution is 1mL/h; The spinning environment temperature is 30 ℃;
5) starting drive carries out the electrostatic spinning of water soluble chitosan; Can on device, obtain good biocompatibility, nontoxic and biodegradable CS nano fibrous membrane on the collecting board, this tunica fibrosa all has higher using value at aspects such as organizational project, wound repair, medicament transport.
Embodiment 13
1) compound concentration is the aqueous solution of the ethanol of 20wt%;
2) be that 150,000 water soluble chitosan powder are distributed in the step 1) solution with weight average molecular weight, be made into the solution that percentage by weight is 3wt%;
3) then with step 2) in solution fully stir so that fully the dissolving, bubble is all separated out the solution left standstill ultrasonic wave and promptly obtains transparent hyaluronic acid solution;
4) solution in the step 3) is added syringe pump, adjustment voltage is 15kV; Spinning head is 20cm to the distance of collecting board; The flow of spinning head spinning solution is 1mL/h; The spinning environment temperature is 30 ℃;
5) starting drive carries out the electrostatic spinning of water soluble chitosan; Can on device, obtain good biocompatibility, nontoxic and biodegradable CS nano fibrous membrane on the collecting board, this tunica fibrosa all has higher using value at aspects such as organizational project, wound repair, medicament transport.
Embodiment 14
1) compound concentration is the aqueous solution of the ethanol of 20wt%;
2) be that 150,000 water soluble chitosan powder are distributed in the step 1) solution with weight average molecular weight, be made into the solution that percentage by weight is 3wt%;
3) then with step 2) in solution fully stir so that fully the dissolving, bubble is all separated out the solution left standstill ultrasonic wave and promptly obtains transparent hyaluronic acid solution;
4) solution in the step 3) is added syringe pump, adjustment voltage is 15kV; Spinning head is 8cm to the distance of collecting board; The flow of spinning head spinning solution is 1mL/h; The spinning environment temperature is 20 ℃;
5) starting drive carries out the electrostatic spinning of water soluble chitosan; Can on device, obtain good biocompatibility, nontoxic and biodegradable CS nano fibrous membrane on the collecting board, this tunica fibrosa all has higher using value at aspects such as organizational project, wound repair, medicament transport.
Embodiment 15
1) compound concentration is the aqueous solution of the ethanol of 20wt%;
2) be that 150,000 water soluble chitosan powder are distributed in the step 1) solution with weight average molecular weight, be made into the solution that percentage by weight is 3wt%;
3) then with step 2) in solution fully stir so that fully the dissolving, bubble is all separated out the solution left standstill ultrasonic wave and promptly obtains transparent hyaluronic acid solution;
4) solution in the step 3) is added syringe pump, adjustment voltage is 15kV; Spinning head is that the flow of 8cm spinning head spinning solution is 1mL/h to the distance of collecting board; The spinning environment temperature is 40 ℃;
5) starting drive carries out the electrostatic spinning of water soluble chitosan; Can on device, obtain good biocompatibility, nontoxic and biodegradable CS nano fibrous membrane on the collecting board, this tunica fibrosa all has higher using value at aspects such as organizational project, wound repair, medicament transport.
Claims (5)
1. method for preparing the water soluble chitosan nano fiber non-woven fabric is characterized in that may further comprise the steps:
(1) with in the water-soluble solvent of forming with ethanol of water soluble chitosan powder; Be made into the solution that percentage by weight is 1～5wt%; Then solution is fully stirred, so that dissolving fully, bubble is all separated out the solution left standstill ultrasonic wave and promptly obtain water soluble chitosan solution.
(2) the water soluble chitosan electrostatic spinning solution with preparation in the step (1) adds syringe pump, and the adjustment spinning voltage does; Spinning head is to the distance of collecting board; The flow of spinning head spinning solution does; The spinning environment temperature.Starting drive carries out the electrostatic spinning of water soluble chitosan, on collecting board, has obtained the water soluble chitosan nano fiber non-woven fabric;
2. according to the preparation method of claim 1, it is characterized in that the water soluble chitosan weight average molecular weight described in the step (1) is 100,000～200,000;
3. according to the preparation method of claim 1, the volume ratio that it is characterized in that aqueous solvent described in the step (1) and ethanol is 80/20～60/40, and the percentage by weight of water soluble chitosan solution is 1wt%～5wt%;
4. according to the preparation method of claim 1, it is characterized in that the voltage described in the step (2) is 15～30kV; Spinning head is 8～20cm to the distance of collecting board;
5. according to the preparation method of claim 1, it is characterized in that the spinning environment temperature described in the step (2) is 10～40 ℃.
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| CN102677391A (en) * | 2012-05-07 | 2012-09-19 | 东华大学 | Preparation method of high-selectivity nano fiber membrane |
| CN103061037A (en) * | 2013-01-11 | 2013-04-24 | 东华大学 | Method for manufacturing polyaspartic acid nano-fiber mat by electrostatic spinning |
| CN105605339A (en) * | 2016-03-16 | 2016-05-25 | 刘志光 | High-strength antibacterial oxygen-resistant PP-RCT composite pipe |
| CN105926053A (en) * | 2016-06-08 | 2016-09-07 | 海南大学 | Electrostatic spinning method of chitosan |
| CN106757788A (en) * | 2016-12-23 | 2017-05-31 | 杭州安诺过滤器材有限公司 | A kind of filter for infusion filtering nano fibrous membrane and preparation method thereof |
| CN106963973A (en) * | 2017-03-17 | 2017-07-21 | 广州润虹医药科技有限公司 | A kind of chitosan combine dressing and preparation method thereof |
| CN111020745A (en) * | 2019-12-31 | 2020-04-17 | 泰州市榕兴医疗用品股份有限公司 | Preparation method of sodium alginate and chitosan composite nanofiber |
| CN113186649A (en) * | 2021-04-30 | 2021-07-30 | 河北宁纺集团有限责任公司 | Colorful antibacterial nanofiber membrane and preparation method and application thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102677391A (en) * | 2012-05-07 | 2012-09-19 | 东华大学 | Preparation method of high-selectivity nano fiber membrane |
| CN103061037A (en) * | 2013-01-11 | 2013-04-24 | 东华大学 | Method for manufacturing polyaspartic acid nano-fiber mat by electrostatic spinning |
| CN105605339A (en) * | 2016-03-16 | 2016-05-25 | 刘志光 | High-strength antibacterial oxygen-resistant PP-RCT composite pipe |
| CN105926053A (en) * | 2016-06-08 | 2016-09-07 | 海南大学 | Electrostatic spinning method of chitosan |
| CN106757788A (en) * | 2016-12-23 | 2017-05-31 | 杭州安诺过滤器材有限公司 | A kind of filter for infusion filtering nano fibrous membrane and preparation method thereof |
| CN106757788B (en) * | 2016-12-23 | 2019-07-30 | 杭州安诺过滤器材有限公司 | A kind of filter for infusion filtering nano fibrous membrane and preparation method thereof |
| CN106963973A (en) * | 2017-03-17 | 2017-07-21 | 广州润虹医药科技有限公司 | A kind of chitosan combine dressing and preparation method thereof |
| CN111020745A (en) * | 2019-12-31 | 2020-04-17 | 泰州市榕兴医疗用品股份有限公司 | Preparation method of sodium alginate and chitosan composite nanofiber |
| CN113186649A (en) * | 2021-04-30 | 2021-07-30 | 河北宁纺集团有限责任公司 | Colorful antibacterial nanofiber membrane and preparation method and application thereof |
| CN113186649B (en) * | 2021-04-30 | 2022-11-08 | 河北宁纺集团有限责任公司 | Colorful antibacterial nanofiber membrane and preparation method and application thereof |
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Application publication date: 20120425 |