CN105755673A - Manufacturing method for antibacterial high selectivity nanofiber membrane - Google Patents
Manufacturing method for antibacterial high selectivity nanofiber membrane Download PDFInfo
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- CN105755673A CN105755673A CN201410774884.6A CN201410774884A CN105755673A CN 105755673 A CN105755673 A CN 105755673A CN 201410774884 A CN201410774884 A CN 201410774884A CN 105755673 A CN105755673 A CN 105755673A
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Abstract
The invention discloses a manufacturing method for an antibacterial high selectivity nanofiber membrane. The method is characterized by comprising the following steps: (1) preparing a chitosan acetic acid solution; (2) performing an electrostatic spinning process; (3) performing heat treatment; (4) and manufacturing the nanofiber membrane. The chitosan is selected as an absorbing carrier, and the chitosan has good adhesion and permeability, and is non-toxic to human bodies. The obtained nanofiber membrane has microfiber effect. Through gently controlling electrospinning technical parameters, the composite nanofiber membrane has good biocompatibility and long-term stability, and does not easily deform. Through processing by a solidification liquid, the nanofiber membrane still has excellent antibacterial property after being dried. The method is applied in fields of medicine and sanitation, and has obvious advantages.
Description
Technical field
The invention belongs to the technical field of nano fibrous membrane, the preparation method being specifically related to a kind of antibacterial high-selectivity nano fiber membrane.
Background technology
Nanofiber refers to the fibre diameter super-micro-fine fibres less than 100 nanometers.Nowadays a lot of enterprises are for the effect of publicity of commodity, having dosed the fiber of nanoscale (namely less than 100nm) powder filler also referred to as nanofiber.Nanofiber the thinnest at present is single carbon atom chain, and China scientist can produce the diameter carbon pipe less than 0.4nm, is in world lead level.This CNT is described as the king of nano material, and this thin material being all difficult to observe by general instrument of its reason has the ability of mystery: superelevation magnetic pliable and tough, strange strong, super.
Having many uses of nanofiber, as nanofiber is implanted fabric face, can form gas membrane one layer stable, makes double; two thin property interfaces fabric, both waterproof, again can be grease proofing, antifouling；The senior protective garment made with nanofiber, its fabric porous and have film, air permeable can not only be made, tool can respiratory, moreover it is possible to keeps out the wind and filters minuteness particle, aerosol is had block, can anti-chemical and biological weapons and noxious substance.Additionally, nanofiber can be additionally used in the purification of the product such as chemical industry, medicine, filtration etc..
Chitosan is a kind of avirulence, non-irritating very safe machine body material.Owing to chitosan molecule containing substantial amounts of amino (-NH2) and hydroxyl (-OH) group, major part metal ion is respectively provided with stronger complexing power, therefore chelate can be formed as part with metal ion, can from various aqueous solution heavy-metal ion removals.Simultaneously, the fiber and the film that prepare with chitosan for raw material have good adhesiveness, permeability and physical and mechanical properties, to human non-toxic, but also there is fento effect, electric property, and mechanical property is such as very big specific surface area, flexible and superpower mechanical behavior (such as hardness and tensile strength), exchange is fast with elution speed, can the outstanding advantages such as multiple application form application such as fiber and its products.Therefore, particularly when not using the material that human body is poisonous, the application of chitosan nano fiber membrane has significant advantage.The characteristic of these excellences makes chitosan nano fiber membrane be more suitable for pharmaceutical sanitary field.
Adopt Electrospinning by the report of water soluble polymer fiber Yu noble metal compound although existing at present, but all inevitably add additional reducing agent and carry out synthesizing nano-particle, or introduce stable in water after chemical cross-linking agent makes these fibrous membrane molding use.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of antibacterial high-selectivity nano fiber membrane, the nano fibrous membrane obtained has fento effect, by leniently controlling Electrospinning parameter, composite nano-fiber membrane is made to have good biocompatibility and long-time stability, it is unlikely to deform, processed by solidification liquid, still there is the anti-microbial property of excellence after drying.
The technical scheme that the present invention takes is:
The preparation method of a kind of antibacterial high-selectivity nano fiber membrane, it is characterised in that comprise the steps:
(1) configuration chitosan acetic acid solution: it is that in 3-4% acetic acid aqueous solution, stirring and dissolving is solution uniformly that the chitosan that degree of deacetylation is 60-80% is dissolved in mass concentration, is configured to the chitosan acetic acid solution that mass concentration is 35-45g/L；
(2) electrostatic spinning process: be injected in micro-injection pump by chitosan acetic acid solution, in connection, electrostatic generator carries out electrostatic spinning, and the fiber obtained is received by the container equipped with solidification liquid, dry；
(3) heat treatment: be placed in gas-protecting sintering stove by SiBONC powder, carries out heat treatment under nitrogen protection to material, controls temperature and is 1300-1800 DEG C, isothermal holding 2-3h；
(4) composite nano-fiber membrane processed: the nano fibrous membrane after above-mentioned heat treatment is placed in the baking oven of 120-140 DEG C and processes 3-5h, obtain Nanocomposites nano fibrous membrane.
Electrostatic spinning process parameter in described step (2) is: voltage 15-25kv, and flow is 0.08-0.2mL/h, ambient temperature 10-50 DEG C, receiving range 5-30cm.
Solidification liquid in described step (2) is that formaldehyde and citric acid are according to the weight ratio 3:1 mixture formed.
In SiBONC powder in described step (3), the mol ratio of Si/B is 5:3.
The invention have the benefit that
The present invention selects chitosan as absorption carrier, there is good adhesiveness and permeability, to human non-toxic, the nano fibrous membrane obtained has fento effect, by leniently controlling Electrospinning parameter, makes composite nano-fiber membrane have good biocompatibility and long-time stability, it is unlikely to deform, being processed by solidification liquid, still have the anti-microbial property of excellence after drying, the field such as medicine, health that is applied at present has significant advantage.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of antibacterial high-selectivity nano fiber membrane, it is characterised in that comprise the steps:
(1) configuration chitosan acetic acid solution: it is that in 3% acetic acid aqueous solution, stirring and dissolving is solution uniformly that the chitosan that degree of deacetylation is 60% is dissolved in mass concentration, is configured to the chitosan acetic acid solution that mass concentration is 35g/L；
(2) electrostatic spinning process: chitosan acetic acid solution is injected in micro-injection pump, in connection, electrostatic generator carries out electrostatic spinning, electrostatic spinning process parameter is: voltage 15kv, flow is 0.08mL/h, ambient temperature 20 DEG C, receiving range 20cm, the fiber obtained is by being received according to the container of the weight ratio 3:1 solidification liquid formed equipped with formaldehyde and citric acid, dry；
(3) heat treatment: be placed in gas-protecting sintering stove by the SiBONC powder that the mol ratio of Si/B is 5:3, carries out heat treatment under nitrogen protection to material, and controlling temperature is 1300 DEG C, isothermal holding 3h；
(4) composite nano-fiber membrane processed: be placed in the baking oven of 120 DEG C by the nano fibrous membrane after above-mentioned heat treatment process-5h, obtains Nanocomposites nano fibrous membrane.
Embodiment 2
The preparation method of a kind of antibacterial high-selectivity nano fiber membrane, it is characterised in that comprise the steps:
(1) configuration chitosan acetic acid solution: it is that in 3.5% acetic acid aqueous solution, stirring and dissolving is solution uniformly that the chitosan that degree of deacetylation is 70% is dissolved in mass concentration, is configured to the chitosan acetic acid solution that mass concentration is 40g/L；
(2) electrostatic spinning process: chitosan acetic acid solution is injected in micro-injection pump, in connection, electrostatic generator carries out electrostatic spinning, electrostatic spinning process parameter is: voltage 20kv, flow is 0.1mL/h, ambient temperature 20 DEG C, receiving range 20cm, the fiber obtained is by being received according to the container of the weight ratio 3:1 solidification liquid formed equipped with formaldehyde and citric acid, dry；
(3) heat treatment: be placed in gas-protecting sintering stove by the SiBONC powder that the mol ratio of Si/B is 5:3, carries out heat treatment under nitrogen protection to material, and controlling temperature is 1500 DEG C, isothermal holding 2.5h；
(4) composite nano-fiber membrane processed: the nano fibrous membrane after above-mentioned heat treatment is placed in the baking oven of 130 DEG C and processes 4h, obtain Nanocomposites nano fibrous membrane.
Embodiment 3
The preparation method of a kind of antibacterial high-selectivity nano fiber membrane, it is characterised in that comprise the steps:
(1) configuration chitosan acetic acid solution: it is that in 4% acetic acid aqueous solution, stirring and dissolving is solution uniformly that the chitosan that degree of deacetylation is 80% is dissolved in mass concentration, is configured to the chitosan acetic acid solution that mass concentration is 45g/L；
(2) electrostatic spinning process: chitosan acetic acid solution is injected in micro-injection pump, in connection, electrostatic generator carries out electrostatic spinning, electrostatic spinning process parameter is: voltage 25kv, flow is 0.2mL/h, ambient temperature 20 DEG C, receiving range 20cm, the fiber obtained is by being received according to the container of the weight ratio 3:1 solidification liquid formed equipped with formaldehyde and citric acid, dry；
(3) heat treatment: be placed in gas-protecting sintering stove by the SiBONC powder that the mol ratio of Si/B is 5:3, carries out heat treatment under nitrogen protection to material, and controlling temperature is 1800 DEG C, isothermal holding 2h；
(4) composite nano-fiber membrane processed: the nano fibrous membrane after above-mentioned heat treatment is placed in the baking oven of 140 DEG C and processes 3h, obtain Nanocomposites nano fibrous membrane.
Claims (4)
1. the preparation method of an antibacterial high-selectivity nano fiber membrane, it is characterised in that comprise the steps:
(1) configuration chitosan acetic acid solution: it is that in 3-4% acetic acid aqueous solution, stirring and dissolving is solution uniformly that the chitosan that degree of deacetylation is 60-80% is dissolved in mass concentration, is configured to the chitosan acetic acid solution that mass concentration is 35-45g/L；
(2) electrostatic spinning process: be injected in micro-injection pump by chitosan acetic acid solution, in connection, electrostatic generator carries out electrostatic spinning, and the fiber obtained is received by the container equipped with solidification liquid, dry；
(3) heat treatment: be placed in gas-protecting sintering stove by SiBONC powder, carries out heat treatment under nitrogen protection to material, controls temperature and is 1300-1800 DEG C, isothermal holding 2-3h；
(4) composite nano-fiber membrane processed: the nano fibrous membrane after above-mentioned heat treatment is placed in the baking oven of 120-140 DEG C and processes 3-5h, obtain Nanocomposites nano fibrous membrane.
2. the preparation method of a kind of antibacterial high-selectivity nano fiber membrane according to claim 1, it is characterized in that, the electrostatic spinning process parameter in described step (2) is: voltage 15-25kv, and flow is 0.08-0.2mL/h, ambient temperature 10-50 DEG C, receiving range 5-30cm.
3. the preparation method of a kind of antibacterial high-selectivity nano fiber membrane according to claim 1, it is characterised in that the solidification liquid in described step (2) is that formaldehyde and citric acid are according to the weight ratio 3:1 mixture formed.
4. the preparation method of a kind of antibacterial high-selectivity nano fiber membrane according to claim 1, it is characterised in that in the SiBONC powder in described step (3), the mol ratio of Si/B is 5:3.
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| CN201410774884.6A CN105755673A (en) | 2014-12-16 | 2014-12-16 | Manufacturing method for antibacterial high selectivity nanofiber membrane |
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| CN201410774884.6A CN105755673A (en) | 2014-12-16 | 2014-12-16 | Manufacturing method for antibacterial high selectivity nanofiber membrane |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106835495A (en) * | 2016-12-22 | 2017-06-13 | 马鞍山市鑫程纳米新材料科技有限公司 | One kind has high performance non-woven fabrics |
| CN111820503A (en) * | 2020-07-24 | 2020-10-27 | 蒿薇薇 | Anti-virus mask made of nanofiber material |
| CN113529274A (en) * | 2021-08-19 | 2021-10-22 | 澜海生态农业(杭州)有限公司 | Nanofiber membrane and application thereof, nanofiber membrane sterilization liquid and application method thereof |
| CN115554864A (en) * | 2022-11-11 | 2023-01-03 | 北京大学 | Chitosan-based electrostatic spinning fibrous membrane capable of efficiently recovering gold element in water body |
-
2014
- 2014-12-16 CN CN201410774884.6A patent/CN105755673A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106835495A (en) * | 2016-12-22 | 2017-06-13 | 马鞍山市鑫程纳米新材料科技有限公司 | One kind has high performance non-woven fabrics |
| CN111820503A (en) * | 2020-07-24 | 2020-10-27 | 蒿薇薇 | Anti-virus mask made of nanofiber material |
| CN113529274A (en) * | 2021-08-19 | 2021-10-22 | 澜海生态农业(杭州)有限公司 | Nanofiber membrane and application thereof, nanofiber membrane sterilization liquid and application method thereof |
| CN115554864A (en) * | 2022-11-11 | 2023-01-03 | 北京大学 | Chitosan-based electrostatic spinning fibrous membrane capable of efficiently recovering gold element in water body |
| CN115554864B (en) * | 2022-11-11 | 2023-07-11 | 北京大学 | Chitosan-based electrostatic spinning fiber membrane capable of efficiently recovering gold element in water |
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Application publication date: 20160713 |