CN100355975C - Natural nanometer fiber preparation method - Google Patents
Natural nanometer fiber preparation method Download PDFInfo
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- CN100355975C CN100355975C CNB2005100862517A CN200510086251A CN100355975C CN 100355975 C CN100355975 C CN 100355975C CN B2005100862517 A CNB2005100862517 A CN B2005100862517A CN 200510086251 A CN200510086251 A CN 200510086251A CN 100355975 C CN100355975 C CN 100355975C
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Abstract
The present invention discloses a natural nanometer fiber preparation method, particularly a natural nanometer fiber preparation method used for composite reinforcement materials of tissue engineer (such as a cell culture support frame, a drug transmission system, osseous mineralization, etc.) air filtering, clothing cloth and aerospace, and the present invention in particular relates to a preparation method for natural nanometer spider silk fibers and natural nanometer silkworm silk fibers. Natural nanometer fibers of which the diameter range is from 30 nanometers to 100 nanometers can be finally prepared through certain solvent soaking and ultrasonic dissociation, and the prepared natural nanometer fibers have wide application foreground for composite reinforcement materials of tissue engineer (such as a cell culture support frame, a drug transmission system, osseous mineralization, etc.) air filtering, clothing cloth and aerospace. The present invention has the advantages of simple and convenient operation, few procedures, simple equipment, little energy consumption and low input investment, and is suitable for laboratory research preparation and large scale industrial production.
Description
Technical field
The present invention relates to a kind of preparation method who is used for the natural-nanometer fiber of organizational project (as mineralising of cell culturing bracket, drug delivery system and bone etc.), air filtration, clothing cloth and aerospace composite reinforcing material, specially refer to the preparation method of natural nano spider silk fiber and natural nano silk fiber.
Background technology
In the preparation method of existing spider silk nanofiber and silk nanofiber, what often adopt is method of electrostatic spinning and self-assembling method.
Method of electrostatic spinning is at first to prepare spidroin solution or fibroin protein solution, then joins in the plastic tube that has a capillary end, then a copper electrode that links to each other with the power supply positive high voltage is inserted in the precursor solution.A ground connection iron drum that can rotate is installed in the place ahead of plastic tube, and its upper berth one deck aluminium foil is as dash receiver.Between shower nozzle and dash receiver, form an electric field, from the protein solution of shower nozzle ejection under the electric field force effect, the filament that pulled into the about 30～400nm of diameter in several seconds is fallen on the dash receiver of rotation, thereby can prepare regenerated spider silk nanofiber and regenerated silk nanofiber.
Self-assembling method is at first to prepare very high spider silk fibroin of purity or fibroin protein, then prepares regenerated spider silk nanofiber and regenerated silk nanofiber in certain solvent.
The electrospinning process complex procedures, energy consumption is big, and it is big that equipment relates to electric power, and the early investment fund is more, and the nanofiber of preparing belongs to the regeneration nanofiber;
Self-assembling method need be prepared highly purified spider silk fibroin or fibroin protein earlier, and the nanofiber of preparing is the regeneration nanofiber, and can not mass preparation.
Summary of the invention
The objective of the invention is to: overcome the shortcoming of existing preparation natural-nanometer fiber, provide a kind of very easy, operation is few, equipment is simple, energy consumption is little, infusion of financial resources less, be fit to the method for preparing natural-nanometer fiber of laboratory research preparation and large-scale industrial production.
The object of the present invention is achieved like this:
A kind of preparation method of natural-nanometer fiber, the natural biologic material of it is multiple dimensioned at having (from macroscopic view, microcosmic to Na Guan etc.) hierarchy may further comprise the steps:
(1) natural biologic material is immersed in the container of certain solvent;
(2) ultrasonic unit of the certain power of unlatching certain frequency deeply is mounted with the ultrasonic wave transmitting probe in the container of natural biologic material solution, and the ultrasonic wave that carries out certain hour dissociates;
By step (1), step (2), thus can prepare natural-nanometer fiber on a large scale.
Described natural biologic material has the hierarchy with different scales such as little fibril, fibril, fibers, comprises spider silk, domestic silkworm silk, tussah, wool, fish scale, bamboo fibre, collagenous fiber, xylon.
Described solvent is characterized in that, is weak acid, weak base, pure water or ultra-pure water.
Described ultrasonic wave comprises: launch hyperacoustic instrument and equipment, frequency is at 10 KHzs～10 megahertzes, and power is at 100 watts～2000 watts; Power and frequency are big more, and required ultrasonic wave time of dissociating is short more.
Ultrasonic wave of the present invention dissociates and is based on hyperacoustic sound cavitation effect, i.e. the process of concentrating the sound field energy and discharging rapidly.When the ultrasonic wave of sufficient intensity passes through liquid, if surpass the liquid internal static pressure in sound wave negative pressure half period sound pressure amplitude, the micro-bubble (cavitation nucleus) that is present in the liquid will increase rapidly, in the sound wave malleation cycle of coming one after the other, bubble is adiabatic compression and collapsing again, in the extremely of short duration strong pressure pulses of collapse moment generation, can produce high temperature in the middle of the bubble near 5000K, pressure surpasses 50MPa, the temperature at the interface of bubble and liquid can reach 2000K, after continuing several microseconds, this focus cools off (rate of temperature change reaches 109K/s) thereupon, and with strong shock wave (for the homogeneous liquid medium) and the speed per hour jet (for heterogeneous medium) up to 400km, this has just created an extreme physical environment for the preparation of natural-nanometer fiber.Therefore,, under the effect of sound cavitation effect, constantly dissociate, dissociate to microcosmic, dissociate to Na Guan, thereby prepare the nanofiber of pure natural from microcosmic from macroscopic view for natural biologic material with different scale, hierarchy.Phonochemical reaction mainly comes from acoustic cavitation---formation, the vibration in liquid hollow chamber, physics, the chemical change of growing, being contracted to collapse and cause.
The present invention provides a kind of preparation method of natural-nanometer fiber owing to adopted the ultrasonic acoustic cavitation effect,
(1) simple, the less energy consumption of technology of the present invention, fund input are few, workable, easy to implement, and environmentally friendly, pollution-free;
(2) the present invention is suitable wide, as long as have the natural biologic material of different scale hierarchy, all can adopt the present invention to prepare corresponding natural-nanometer fiber;
(3) natural-nanometer fiber prepared of the present invention directly dissociates from natural biologic material and gets, and is not the regeneration nanofiber;
(4) diameter of natural-nanometer fiber of the present invention has controllability, can realize by frequency of ultrasonic, power and solvent composition.
Description of drawings
Fig. 1 is ultrasonic wave that a kind of the present invention the adopts appliance arrangement schematic diagram that dissociates.
Fig. 2 is the stereoscan photograph of the natural spider silk nanofiber prepared of the embodiment of the invention 1.
Fig. 3 is the stereoscan photograph of the natural silk fiber prepared of the embodiment of the invention 3 of the present invention.
The specific embodiment
Below in conjunction with drawings and Examples the present invention is described in detail.
Fig. 1 is the dissociate photo of device (supersonic cell crusher) of ultrasonic wave that a kind of the present invention adopts, and its model is JY92-II type (manufacturer is the new sesame bio tech ltd in Ningbo), and its specification is: frequency 20 KHzs, 900 watts of peak powers.
Obviously, embodiment is in order the present invention to be described rather than to limit of the present inventionly, can also adopting other can produce the ultrasonic wave generating apparatus of satisfactory frequency and power in the present invention.
Similarly this kind equipment also has ultrasonic cell disruptor, ultrasonic plastic welder, ultrasonic drilling machine, ultrasonic wave nanometer draft machine, ultrasonic oscillator, ultrasonic wave refiner etc. to have the ultrasonic wave class device of supersonic generator and ultrasonic vibration system (mainly comprising ultrasonic transducer, ultrasonic variable amplitude bar and ultrasonic probe).
Embodiment 1
Adopt device as shown in Figure 1, preparation natural-nanometer fiber: spider silk is immersed in the beaker that ultra-pure water is housed; Hyperacoustic power is 600 watts, and frequency is 20 KHzs, and the probe of supersonic generator is deep in the beaker, and ultrasonic cavitation 2.5 hours can be prepared the natural spider silk nanofiber of 30～120 nanometers, as shown in Figure 2.
Embodiment 2
Adopt device as shown in Figure 1, spider silk is immersed in the beaker that formic acid solvent is housed; Hyperacoustic power is 600 watts, and frequency is 20 KHzs, and the probe of supersonic generator is deep in the beaker, and ultrasonic cavitation 2.0 hours can be prepared the natural spider silk nanofiber of 30～120 nanometers.
Embodiment 3
Adopt device as shown in Figure 1, the mulberry silk that will come unstuck is immersed in the beaker that ultra-pure water is housed; Hyperacoustic power is 600 watts, and frequency is 20 KHzs, and the probe of supersonic generator is deep in the beaker, and ultrasonic cavitation 2.5 hours can be prepared the natural silk nanofiber of 30～120 nanometers, as shown in Figure 3.
Adopt device as shown in Figure 1, the mulberry silk that will come unstuck is immersed in the beaker that formic acid solvent is housed; Hyperacoustic power is 600 watts, and frequency is 20 KHzs, and the probe of supersonic generator is deep in the beaker, and ultrasonic cavitation 2.0 hours can be prepared the natural silk nanofiber of 30～120 nanometers.
Embodiment 5
Adopt similar device shown in Figure 1, the mulberry silk that will come unstuck is immersed in the beaker that pure water is housed; Hyperacoustic power is 900 watts, and frequency is 20 KHzs, and the probe of supersonic generator is deep in the beaker, and ultrasonic cavitation 0.3 hour can be prepared the natural silk nanofiber of 50～150 nanometers.
Embodiment 6
Adopt device shown in Figure 1, the mulberry silk that will come unstuck is immersed in the beaker that pure water is housed; Hyperacoustic power is 300 watts, and frequency is 10 KHzs, and the probe of supersonic generator is deep in the beaker, and ultrasonic cavitation 2.5 hours can be prepared the natural silk nanofiber of 100～250 nanometers.
The present invention can be easy, operation is few, equipment is simple, energy consumption is little, infusion of financial resources less, prepare natural-nanometer fiber in the laboratory or on the large-scale industrial production.
Claims (2)
1, a kind of preparation method of natural-nanometer fiber is characterized in that, this preparation method may further comprise the steps:
(1) natural biologic material is immersed in the container that fills weak acid, weak base, pure water or ultra-pure water;
(2) open frequency is that 10 KHzs～10 megahertzes and power are the ultrasonic unit of 10 watts～200O watt, the ultrasonic wave transmitting probe deeply is mounted with in the container of natural biologic material solution, carry out ultrasonic wave and dissociate, thereby prepare a kind of natural-nanometer fiber.
2, the preparation method of a kind of natural-nanometer fiber according to claim 1 is characterized in that, described natural biologic material comprises spider silk, domestic silkworm silk, tussah, wool, fish scale, bamboo fibre, collagenous fiber, xylon.
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| CNB2005100862517A CN100355975C (en) | 2005-08-19 | 2005-08-19 | Natural nanometer fiber preparation method |
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| CNB2005100862517A CN100355975C (en) | 2005-08-19 | 2005-08-19 | Natural nanometer fiber preparation method |
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| CN100355975C true CN100355975C (en) | 2007-12-19 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100394988C (en) * | 2006-06-30 | 2008-06-18 | 清华大学 | Preparation of natural-nanometer fiber-base tissue engineering cell stand |
| US20100068517A1 (en) * | 2006-09-12 | 2010-03-18 | National University Of Singapore | Enhanced silk protein material having improved mechanical performance and method of forming the same |
| FI123988B (en) | 2010-10-27 | 2014-01-31 | Upm Kymmene Corp | Cell Culture Materials |
| FI125965B (en) | 2012-09-25 | 2016-04-29 | Upm Kymmene Corp | Three-dimensional cell culture |
| CN104818539A (en) * | 2015-05-11 | 2015-08-05 | 湖州哲豪丝绸有限公司 | Regeneration spider silk fiber based on ionic liquid and preparation method of regeneration spider silk fiber |
| CN104928804B (en) * | 2015-07-07 | 2017-10-03 | 哈尔滨工业大学 | A kind of preparation method of polymer nanofiber |
| CN105862144A (en) * | 2016-04-05 | 2016-08-17 | 西南大学 | Efficient preparing method for fibroin nano-fiber and application of fibroin nano-fiber |
| CN105714432A (en) * | 2016-05-09 | 2016-06-29 | 西南大学 | Fiber division method of silk fibroin fibers |
| CN106283782B (en) * | 2016-07-29 | 2017-12-01 | 华南理工大学 | Low-intensity ultrasonic auxiliary amino acid ion liquid prepares the method and its application of nano-cellulose |
| CN110512301A (en) * | 2019-09-12 | 2019-11-29 | 中国科学院青岛生物能源与过程研究所 | A method of quick, low cost prepares silk nanofiber |
| CN114908433A (en) * | 2021-02-07 | 2022-08-16 | 浙江大学 | Method for preparing fibroin nano-fiber by physical method and product |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08325930A (en) * | 1995-03-31 | 1996-12-10 | Japan Vilene Co Ltd | Nonwoven fabric and its production |
| CN1479821A (en) * | 2000-12-06 | 2004-03-03 | 伍尔马克(欧洲)有限公司 | Fibrillation of natural fibres |
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2005
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08325930A (en) * | 1995-03-31 | 1996-12-10 | Japan Vilene Co Ltd | Nonwoven fabric and its production |
| CN1479821A (en) * | 2000-12-06 | 2004-03-03 | 伍尔马克(欧洲)有限公司 | Fibrillation of natural fibres |
Non-Patent Citations (3)
| Title |
|---|
| 用超声波使动物纤维改性 李凤绵.北京纺织，第19卷第2期 1998 * |
| 超声波在纺织品加工中的应用 万震等.纺织导报，第2期 2001 * |
| 超声波处理对纤维素纤维形态结构的影响 唐爱民等.纤维素科学与技术，第13卷第1期 2005 * |
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