CN105220361A - The preparation method of a kind of Tea Polyphenols/cellulose acetate nano fibrous membrane - Google Patents
The preparation method of a kind of Tea Polyphenols/cellulose acetate nano fibrous membrane Download PDFInfo
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- CN105220361A CN105220361A CN201510737447.1A CN201510737447A CN105220361A CN 105220361 A CN105220361 A CN 105220361A CN 201510737447 A CN201510737447 A CN 201510737447A CN 105220361 A CN105220361 A CN 105220361A
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Abstract
The invention discloses the preparation method of a kind of Tea Polyphenols/cellulose acetate nano fibrous membrane, cellulose acetate and absolute ethyl alcohol are placed in airtight container, stirred at ambient temperature, to being uniformly dispersed, obtains mixed liquor; Tea Polyphenols powder is added N-N dimethyl formamide liquid, sealing is placed in supersonic cell pulverizer, cycle pulse process; Cellulose acetate/absolute ethyl alcohol mixed liquor is poured in Tea Polyphenols/N-N dimethyl formamide solution, make the mixed solution that cellulose acetate mass fraction is 8 ~ 12%, stir until form the transparent spinning solution of complete and homogeneous, prepare Tea Polyphenols/cellulose acetate nano fibrous membrane by electrostatic spinning.The surface of the nanofiber that method of the present invention prepares is smooth and uniform, and this nano fibrous membrane can fully utilize the advantage of Tea Polyphenols and cellulose acetate bi-material, will be with a wide range of applications in the field such as health care, health care.
Description
Technical field
The invention belongs to technical field of nano material, relate to a kind of preparation method of nano fibrous membrane, be specifically related to the preparation method of a kind of Tea Polyphenols/cellulose acetate nano fibrous membrane.
Background technology
Nanofiber refers to that diameter is nanoscale and the larger filamentary material with certain draw ratio of length.In the narrow sense, the diameter of nanofiber is between 1 ~ 100nm; Broadly, fibre diameter can be called nanofiber lower than 1000nm.Nanofiber has the advantages such as size is small, specific area is high, stable mechanical performance, adsorption capacity are high, the micro/nano fibrous membrane material of the 3 D stereo loose structure piled up by nanofiber has the advantages such as aperture is little, porosity is high, connectedness is good, the fields such as biological medicine, isolated by filtration, electronic information, individual protection can be widely used in, there are wide market prospects.
Electrostatic spinning technique is one of main method of producing nanofiber, is that tractive force overcomes solution or smelt surface tension prepares the technology of nanofiber with inner viscous force by high-pressure electrostatic masterpiece.In electrostatic spinning process, polymer solution or melt are applied in the high-pressure electrostatic of tens thousand of volt, thus the electrostatic field that generation one is powerful between nozzle and receiving system, when the size of electrostatic force equals the viscous force sum of the surface tension of solution and inside, the solution in spin duct can form hemispheric droplet in syringe needle end; Along with the increase of electrostatic force, hemispheric drop is stretched formation taper; After the electrostatic force on drop is more than a critical value, the surface tension overcome on it and viscous force are formed jet; Band point jet is in the electric field by high-speed stretch afterwards, and solvent evaporates, jet solidifies, and finally forms nanofiber mats on the reception device.
Cellulose acetate (CelluloseAcetate is called for short CA), be otherwise known as cellulose acetate, and molecular formula is [C
6h
7o
2(OOCCH
3)
x(OH)
3-x]
n, be cellulosic a kind of esterification derivative.It is with low cost for acetate fiber procatarxis, and manufacture craft is simple and be widely used in the every field such as cigarette filter, textile garment, health care, filtration and infiltration.
Tea Polyphenols (TeaPolyphenol, be called for short TP) be the All Pure Nature antioxidant food extracted from tealeaves, have oxidation resistance strong, have no side effect, the feature such as free from extraneous odour, its content in tealeaves is many, distribution is wide, may be used for suppressing angiocardiopathy, auxiliary prevention and anticancer, auxiliary prevention and therapy radiation injury, in the field such as health care, health care, there is important using value.
The cellulose prepared by electrospinning process and cellulose derivative nanofiber have a lot of report, but there is no the report by electrospinning process being prepared by cellulose or derivatives thereof and Tea Polyphenols compound nanofiber in prior art.
Summary of the invention
In view of this, the object of the invention is to propose a kind of method being prepared nano fibrous membrane by electrostatic spinning Tea Polyphenols/cellulose acetate composite first.
Concrete, the invention provides following technical scheme:
The preparation method of Tea Polyphenols of the present invention/cellulose acetate nano fibrous membrane, comprises the steps:
(1) cellulose acetate and absolute ethyl alcohol are placed in airtight container, stirred at ambient temperature, to being uniformly dispersed, obtains mixed liquor;
Preferably, described cellulose acetate and the mass ratio of absolute ethyl alcohol are 1:1 ~ 1:3.
Preferably, cellulose acetate and absolute ethyl alcohol are placed in beaker and seal, at room temperature stir at least 20min through magnetic stirring apparatus.
(2) Tea Polyphenols powder is added N-N dimethyl formamide liquid, sealing is placed in supersonic cell pulverizer, cycle pulse process at least 1 minute;
Preferably, Tea Polyphenols powder is added N-N dimethyl formamide liquid, sealing is placed in supersonic cell pulverizer, cycle pulse process 1 ~ 5 minute.
(3) cellulose acetate/absolute ethyl alcohol mixed liquor prepared by step (1) is poured in Tea Polyphenols/N-N dimethyl formamide solution prepared by step (2), make the mixed solution that cellulose acetate mass fraction is 8 ~ 12%, stir until form the transparent spinning solution of complete and homogeneous;
Preferably, by cellulose acetate mass fraction be 8 ~ 12% mixed solution to put into condition be that 60 ~ 80 DEG C of water-bath magnetic agitation pots stir 2 ~ 5 hours.
(4) adjustment operation indoor environment, temperature 20 ~ 25 DEG C, relative humidity 50 ~ 70%, spinning solution step (3) prepared sucks the syringe of configuration 0.3 ~ 0.6mm internal diameter metal needle as spinning head, spinning head is accessed high voltage source, aluminium foil receiver is by electric wire ground connection, open DC high-voltage source generator, stretch under the effect of band point jet high voltage electric field between spinning head and aluminium foil receiver, swing, refinement, the dash receiver of aluminium foil receiver obtains nano fibrous membrane, drying at room temperature is until solvent volatilizees completely, finally obtain Tea Polyphenols/cellulose acetate nano fibrous membrane.
Preferably, the distance on described spinning head and aluminium foil receiver surface is 10 ~ 20cm, DC high-voltage power supply voltage 10 ~ 30kV, and spinning solution flow velocity is 5 ~ 10ml/h.
Preferably, by obtained nano fibrous membrane at room temperature dry more than 3h.
The invention provides a kind of feasible method being prepared nano fibrous membrane by Tea Polyphenols/cellulose acetate, the surface of the nanofiber prepared is smooth and uniform, this nano fibrous membrane can fully utilize the advantage of Tea Polyphenols and cellulose acetate bi-material, will be with a wide range of applications in the field such as health care, health care.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme in the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing for the present invention in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
ESEM (SEM) figure of the CA/TP nano fibrous membrane that Fig. 1 prepares when being embodiment of the present invention 4CA mass fraction 10% and fiber diameter distribution profile;
The SEM figure of the CA/TP nano fibrous membrane that Fig. 2 prepares when being embodiment of the present invention 4CA mass fraction 11% and fiber diameter distribution profile;
The SEM figure of the CA/TP nano fibrous membrane that Fig. 3 prepares when being embodiment of the present invention 4CA mass fraction 12% and fiber diameter distribution profile;
The SEM figure of the CA/TP nano fibrous membrane that Fig. 4 prepares when being embodiment of the present invention 4CA mass fraction 13% and fiber diameter distribution profile;
Fig. 5 is the fiber diameter broken line graph of the CA/TP nano fibrous membrane that the different CA mass fraction of the embodiment of the present invention 4 prepares.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is described in detail.
Embodiment 1
Cellulose acetate and absolute ethyl alcohol are placed in beaker with the mass ratio of 5:8 seal, at room temperature stir 20min through magnetic stirring apparatus and cellulose acetate is disperseed, obtain mixed liquor.
Tea Polyphenols powder is placed in the sealing of N-N dimethyl formamide liquid and puts into supersonic cell pulverizer, adopt cycle pulse formula working method to mixed liquor process 5 minutes.
Pour the cellulose acetate made/absolute ethyl alcohol mixed liquor into Tea Polyphenols/N-N dimethyl formamide solution, make the mixed solution that cellulose acetate mass fraction is 8%, and condition of putting into is 60 DEG C of water-bath magnetic agitation pots stirrings 5 hours, until form the transparent solution of complete and homogeneous.
Adjustment operation indoor environment humiture, guarantee that spinning environment temperature is at 20 DEG C, relative humidity is in the scope of 65%.The made spinning solution got ready is sucked the syringe of 10ml, and the metal needle configuring 0.5mm internal diameter is as spinning head.Spinning head is accessed high voltage source, and aluminium foil receiver is by electric wire ground connection.Open high voltage source generator, between spinning head and receiver, form high voltage electric field, band point jet carries out stretching under the effect that high-tension electricity is long, swing, refinement, finally on aluminium foil dash receiver, obtain nano fibrous membrane.
In electrostatic spinning process, the distance on spinning head and aluminium foil receiver surface is 15cm, DC high-voltage power supply voltage 20kV, and spinning solution flow velocity is 5ml/h.
After electrostatic spinning terminates, obtained nano fibrous membrane is at room temperature carried out dry 3h, to guarantee the volatilization completely of solvent.
Embodiment 2
Cellulose acetate and absolute ethyl alcohol are placed in beaker with the mass ratio of 5:8 seal, at room temperature stir 20min through magnetic stirring apparatus and cellulose acetate is disperseed, obtain mixed liquor.
Tea Polyphenols powder is placed in the sealing of N-N dimethyl formamide liquid and puts into supersonic cell pulverizer, adopt cycle pulse formula working method to mixed liquor process 5 minutes.
Pour the cellulose acetate made/absolute ethyl alcohol mixed liquor into Tea Polyphenols/N-N dimethyl formamide solution, make the mixed solution that cellulose acetate mass fraction is 8%, and condition of putting into is 60 DEG C of water-bath magnetic agitation pots stirrings 5 hours, until form the transparent solution of complete and homogeneous.
Adjustment operation indoor environment humiture, guarantee that spinning environment temperature is at 20 DEG C, relative humidity is in the scope of 65%.The made spinning solution got ready is sucked the syringe of 10ml, and the metal needle configuring 0.5mm internal diameter is as spinning head.Spinning head is accessed high voltage source, and aluminium foil receiver is by electric wire ground connection.Open high voltage source generator, between spinning head and receiver, form high voltage electric field, band point jet carries out stretching under the effect that high-tension electricity is long, swing, refinement, finally on aluminium foil dash receiver, obtain nano fibrous membrane.
In electrostatic spinning process, the distance on spinning head and aluminium foil receiver surface is 15cm, DC high-voltage power supply voltage 10kV, and spinning solution flow velocity is 5ml/h.
After electrostatic spinning terminates, obtained nano fibrous membrane is at room temperature carried out dry 3h, to guarantee the volatilization completely of solvent.
Embodiment 3
Cellulose acetate and absolute ethyl alcohol are placed in beaker with the mass ratio of 5:8 seal, at room temperature stir 20min through magnetic stirring apparatus and cellulose acetate is disperseed, obtain mixed liquor.
Tea Polyphenols powder is placed in the sealing of N-N dimethyl formamide liquid and puts into supersonic cell pulverizer, adopt cycle pulse formula working method to mixed liquor process 5 minutes.
Pour the cellulose acetate made/absolute ethyl alcohol mixed liquor into Tea Polyphenols/N-N dimethyl formamide solution, make the mixed solution that cellulose acetate mass fraction is 8%, and condition of putting into is 60 DEG C of water-bath magnetic agitation pots stirrings 5 hours, until form the transparent solution of complete and homogeneous.
Adjustment operation indoor environment humiture, guarantee that spinning environment temperature is at 20 DEG C, relative humidity is in the scope of 65%.The made spinning solution got ready is sucked the syringe of 10ml, and the metal needle configuring 0.5mm internal diameter is as spinning head.Spinning head is accessed high voltage source, and aluminium foil receiver is by electric wire ground connection.Open high voltage source generator, between spinning head and receiver, form high voltage electric field, band point jet carries out stretching under the effect that high-tension electricity is long, swing, refinement, finally on aluminium foil dash receiver, obtain nano fibrous membrane.
In electrostatic spinning process, the distance on spinning head and aluminium foil receiver surface is 15cm, DC high-voltage power supply voltage 30kV, and spinning solution flow velocity is 10ml/h.
After electrostatic spinning terminates, obtained nano fibrous membrane is at room temperature carried out dry 3h, to guarantee the volatilization completely of solvent.
Embodiment 4
Cellulose acetate and absolute ethyl alcohol are placed in beaker with the mass ratio of 5:8 seal, at room temperature stir 20min through magnetic stirring apparatus and cellulose acetate is disperseed, obtain mixed liquor.
Tea Polyphenols powder is placed in the sealing of N-N dimethyl formamide liquid and puts into supersonic cell pulverizer, adopt cycle pulse formula working method to mixed liquor process 5 minutes.
Pour the cellulose acetate made/absolute ethyl alcohol mixed liquor into Tea Polyphenols/N-N dimethyl formamide solution, make the mixed solution that cellulose acetate mass fraction is respectively 10%, 11%, 12% and 13%, and condition of putting into is 60 DEG C of water-bath magnetic agitation pots stirrings 5 hours, until form the transparent solution of complete and homogeneous.
Adjustment operation indoor environment humiture, guarantee that spinning environment temperature is at 20 DEG C, relative humidity is in the scope of 65%.The made spinning solution got ready is sucked the syringe of 10ml, and the metal needle configuring 0.5mm internal diameter is as spinning head.Spinning head is accessed high voltage source, and aluminium foil receiver is by electric wire ground connection.Open high voltage source generator, between spinning head and receiver, form high voltage electric field, band point jet carries out stretching under the effect that high-tension electricity is long, swing, refinement, finally on aluminium foil dash receiver, obtain nano fibrous membrane.
In electrostatic spinning process, the distance on spinning head and aluminium foil receiver surface is 17cm, DC high-voltage power supply voltage 30kV, and spinning solution flow velocity is 6ml/h.
After electrostatic spinning terminates, obtained nano fibrous membrane is at room temperature carried out dry 3h, to guarantee the volatilization completely of solvent.
The CA/TP nano fibrous membrane of the different CA concentration prepared by embodiment 4, accompanying drawing 1 ~ 4 shows its surface topography and diameter distribution situation, and as can be seen from the figure, the surface of the nanofiber in CA mass concentration 10 ~ 13% scope is smooth and uniform; Wherein, the diameter distribution of the nanofiber that CA mass concentration 10 ~ 12% obtains is more concentrated, and the diameter wider distribution of the nanofiber obtained during CA mass concentration 13%, this as can be seen from the average diameter in accompanying drawing 5 also, this mainly adds the cause of the winding of strand due to the increase along with CA mass concentration.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this description is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of description is only for clarity sake, those skilled in the art should by description integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (7)
1. a preparation method for Tea Polyphenols/cellulose acetate nano fibrous membrane, is characterized in that, comprise the steps:
(1) cellulose acetate and absolute ethyl alcohol are placed in airtight container, stirred at ambient temperature, to being uniformly dispersed, obtains mixed liquor;
(2) Tea Polyphenols powder is added N-N dimethyl formamide liquid, sealing is placed in supersonic cell pulverizer, cycle pulse process at least 1 minute;
(3) cellulose acetate/absolute ethyl alcohol mixed liquor prepared by step (1) is poured in Tea Polyphenols/N-N dimethyl formamide solution prepared by step (2), make the mixed solution that cellulose acetate mass fraction is 8 ~ 12%, stir until form the transparent spinning solution of complete and homogeneous;
(4) adjustment operation indoor environment, temperature 20 ~ 25 DEG C, relative humidity 50 ~ 70%, spinning solution step (3) prepared sucks the syringe of configuration 0.3 ~ 0.6mm internal diameter metal needle as spinning head, spinning head is accessed high voltage source, aluminium foil receiver is by electric wire ground connection, open DC high-voltage source generator, stretch under the effect of band point jet high voltage electric field between spinning head and aluminium foil receiver, swing, refinement, the dash receiver of aluminium foil receiver obtains nano fibrous membrane, drying at room temperature is until solvent volatilizees completely, finally obtain Tea Polyphenols/cellulose acetate nano fibrous membrane.
2. preparation method according to claim 1, is characterized in that: in step (1), and described cellulose acetate and the mass ratio of absolute ethyl alcohol are 1:1 ~ 1:3.
3. preparation method according to claim 1, is characterized in that: in step (1), cellulose acetate and absolute ethyl alcohol are placed in beaker and seal, at room temperature stir at least 20min through magnetic stirring apparatus.
4. preparation method according to claim 1, is characterized in that: in step (2), Tea Polyphenols powder is added N-N dimethyl formamide liquid, and sealing is placed in supersonic cell pulverizer, cycle pulse process 1 ~ 5 minute.
5. preparation method according to claim 1, is characterized in that: in step (3), by cellulose acetate mass fraction be 8 ~ 12% mixed solution to put into condition be that 60 ~ 80 DEG C of water-bath magnetic agitation pots stir 2 ~ 5 hours.
6. preparation method according to claim 1, is characterized in that: in step (4), and the distance on described spinning head and aluminium foil receiver surface is 10 ~ 20cm, DC high-voltage power supply voltage 10 ~ 30kV, and spinning solution flow velocity is 5 ~ 10ml/h.
7. preparation method according to claim 1, is characterized in that: in step (4), by obtained nano fibrous membrane at room temperature dry more than 3h.
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Cited By (11)
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| CN105803671A (en) * | 2016-05-11 | 2016-07-27 | 复旦大学 | Electrostatic spinning organic/inorganic composite fiber material as well as preparation method and application thereof |
| CN106048764A (en) * | 2016-06-14 | 2016-10-26 | 南通那芙尔服饰有限公司 | Nanometer cellulose fiber and reinforced composite material with same |
| CN106521671A (en) * | 2016-12-15 | 2017-03-22 | 宜宾屏山辉瑞油脂有限公司 | Tea polyphenol cellulose fiber and preparation method thereof |
| CN106757464A (en) * | 2016-11-15 | 2017-05-31 | 天津捷盛东辉保鲜科技有限公司 | Food oxydating resistance cellulose acetate nanofiber preservative film |
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| CN112088882A (en) * | 2020-09-04 | 2020-12-18 | 浙大宁波理工学院 | Antibacterial nanocellulose microcapsule and preparation method thereof |
| CN115748090A (en) * | 2022-11-17 | 2023-03-07 | 安徽农业大学 | Nanofiber indicating membrane with core-shell structure and preparation method and application thereof |
| CN116035163A (en) * | 2023-01-09 | 2023-05-02 | 厦门绿进食品有限公司 | Preparation method for keeping color of meat product prefabricated dish |
| CN118130410A (en) * | 2024-05-08 | 2024-06-04 | 云南商测质量检验技术服务有限公司 | Method for measuring content of tea polyphenol in tea leaves |
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| CN106521671B (en) * | 2016-12-15 | 2018-12-28 | 宜宾屏山辉瑞油脂有限公司 | A kind of tea polyphenols cellulose fibre and preparation method thereof |
| CN106521671A (en) * | 2016-12-15 | 2017-03-22 | 宜宾屏山辉瑞油脂有限公司 | Tea polyphenol cellulose fiber and preparation method thereof |
| CN107447369A (en) * | 2017-09-27 | 2017-12-08 | 武汉轻工大学 | A kind of anthocyanin composite nano-fiber membrane and preparation method thereof |
| CN108295675A (en) * | 2018-02-10 | 2018-07-20 | 河南省科学院能源研究所有限公司 | A kind of antibacterial air filter film and preparation method thereof based on polyacrylonitrile/graphene oxide/tea polyphenol compound |
| CN108295675B (en) * | 2018-02-10 | 2020-01-24 | 河南省科学院能源研究所有限公司 | Antibacterial air filter membrane based on polyacrylonitrile/graphene oxide/tea polyphenol compound and preparation method thereof |
| CN109457395A (en) * | 2018-11-06 | 2019-03-12 | 温州医科大学 | A kind of tannic acid static spinning membrane and its preparation method and application |
| CN112088882A (en) * | 2020-09-04 | 2020-12-18 | 浙大宁波理工学院 | Antibacterial nanocellulose microcapsule and preparation method thereof |
| CN112088882B (en) * | 2020-09-04 | 2022-05-20 | 浙大宁波理工学院 | Antibacterial nanocellulose microcapsule and preparation method thereof |
| CN115748090A (en) * | 2022-11-17 | 2023-03-07 | 安徽农业大学 | Nanofiber indicating membrane with core-shell structure and preparation method and application thereof |
| CN115748090B (en) * | 2022-11-17 | 2024-06-18 | 安徽农业大学 | Nanofiber indicating membrane with core-shell structure and preparation method and application thereof |
| CN116035163A (en) * | 2023-01-09 | 2023-05-02 | 厦门绿进食品有限公司 | Preparation method for keeping color of meat product prefabricated dish |
| CN118130410A (en) * | 2024-05-08 | 2024-06-04 | 云南商测质量检验技术服务有限公司 | Method for measuring content of tea polyphenol in tea leaves |
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