CN107083674A - A kind of preparation method of silk nanofiber dispersion liquid - Google Patents
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Abstract
The invention discloses a kind of preparation method of silk nanofiber dispersion liquid, silk fiber is pre-processed through formic acid first, then carries out oxidation processes, is obtained finally by decentralized processing with the silk nanofiber dispersion liquid for stablizing nanofibrous structures.Carboxylic group with electronegativity is introduced natural silk fiber by the present invention by oxidation processes, and being aided with the scattered mode of mild mechanical realizes the efficient preparation for the single-silk nanofiber dispersion liquid for retaining preferable prototype structure.Silk nanofiber prepared by the present invention has pH responses simultaneously, precipitation separation and the redisperse of silk nanofiber can be realized by the regulation and control to pH value, is easy to store and transports, and builds field in correlation function material have very big potential value.
Description
Technical field
The invention belongs to nano-cellulose technical field, it is related to preparation method prepared by silk nanofiber and its dispersion liquid
Technical field, and in particular to aoxidize silk fiber using a kind of oxidation system, and silk nanofiber is prepared with reference to mechanical treatment
The method of dispersion liquid.
Background technology
In nature, animal silk is aroused widespread concern and interest with its excellent comprehensive mechanical property.So
And, the silk mechanical property obtained in silk cocoon can not show a candle to the true mechanical property of fibroin in itself, and this is due to curley waste
The process of silk and the follow-up process to silk fiber have had a strong impact on each level structure of silk fiber.Therefore, people are always
The imitated research of silk is directed to, wherein structure and performance are obtained from natural silk fiber retains more complete silk egg
White material is always the emphasis and difficult point of the area research.It is worth noting that, fibroin is with spontaneous in silk fiber
A kind of natural hierarchical structure that nanofiber assembles, although the silk fiber of separate sources（Such as mulberry silk and tussah silk）
It is otherwise varied on amino acid sequence, but its hierarchical structure is essentially identical.Therefore artificial material is being constructed using fibroin
When, researchers expect to retain these natural formations and character to greatest extent, in order to build the silk of excellent in mechanical performance
Nanofiber functional material.
Animal creates unique close, the labyrinth of silk-fibroin in the evolution of 1 years, from natural silk fiber
Stripping nano structure is faced with many difficulties, therefore is rarely reported.Although by spin processes prepared by the silk protein solution after regeneration
Method into fibre structure has a lot, but on the silk fiber performance that obtains of this kind of mode and pattern with natural silk fiber
Fine structure has very big difference, not discusses herein.For current research, though by peeling off or being partly dissolved natural silk
The Structure of Silk of nano-scale can be so obtained, but because of the limitation of preparation method, the silk nanofiber of acquisition is present
Structural instability, Size Distribution heterogeneity and the low defect of yield.The phases of document Appl. Phys. Lett. the 90th report of 2007
" Ultrasonic technique for extracting nanofibers from nature materials ", are adopted in road
Nanofibers can be peeled off from natural silk with strong ultrasonically treated mode, but the nanofiber separated is wrapped around one another
It is not easy to the structure of material；The phases of document J. Mater. Chem. B the 2nd of 2014 report " Silk dissolution
And regeneration at the nanofibril scale " are partly dissolved natural silkworm by the system of formic acid/calcium chloride
Silk fiber, acquisition nanofibrous structures are unstable in a solvent and can not be operated in aqueous phase；China Patent Publication No.
CN104532365 A, publication date is on April 22nd, 2015, entitled " a kind of preparation method of silk nanofiber "
The silk aggregation with nanotopography can be obtained by way of infiltration is aided with long-time mechanical treatment, but this mode
The silk fiber of acquisition is wrapped around one another closely gluey for class water-setting, does not possess single pattern and surface electronegativity, in addition by from
The heart can be settled；The phases of Adv. Mater. the 28th in 2016 report entitled " Liquid Exfoliated Natural Silk
Nanofi brils:Applications in Optical and Electrical Devices " pass through simply joint portion
Divide the method for dissolving and ultrasonic disperse, obtained silk nanofiber yield is relatively low.Therefore a kind of efficiently prepare of development has surely
The method for determining the silk nanofiber of nanofibrous structures is very necessary.
The content of the invention
Goal of the invention：The structural instability and the low shortcoming of yield that exist, this hair are prepared for fibroin nanofiber
A kind of bright preparation method for providing silk nanofiber and its dispersion liquid, with the means modified silk fiber of oxidation, and is aided with light
The efficient preparation with the single-silk nanofiber for stablizing nanofibrous structures is realized in micromechanics processing.
Technical scheme：To realize above goal of the invention, the technical solution adopted by the present invention is as follows：
A kind of preparation method of silk nanofiber dispersion liquid, silk fiber is pre-processed through formic acid first, is then carried out at oxidation
Reason, is obtained with the silk nanofiber dispersion liquid for stablizing nanofibrous structures finally by decentralized processing.
The formic acid pretreatment, the concentration of formic acid is more than 30%wt, processing 0.5 ~ 72.
Described oxidation processes chemical oxidizing agent or (and) biology enzyme oxidant.
Described chemical oxidizing agent is any of hypohalogenous acids, hypohalite, hydrogen peroxide, ozone, peracid；Described
Biological enzyme agent is any of hydrogen peroxide and oxidation enzymatic mixture, laccase, peroxidase, and oxidant is preferably secondary
Sodium chlorate.
Described decentralized processing is mechanical dispersion processing.
Described silk includes mulberry silk, tussah silk, spider silk and other silks.
The silk nanofiber dispersion liquid that the preparation method of described silk nanofiber dispersion liquid is obtained.
Described silk nanofiber dispersion liquid, with pH responses, can realize silk nanometer by the regulation of pH value
Fiber precipitation separation, and redisperse turns into the stable silk nanofiber dispersion liquid of performance.
A kind of silk nanofiber obtained from described silk nanofiber dispersion liquid, carboxyl-content is relative to institute
State 0.3 more than mmol/g of the weight of silk nanofiber.
Described silk nanofiber, it is characterised in that a diameter of 50-500 nm of the silk nanofiber, length
For 10 μm of 50 nm-.
Beneficial effect：Compared with prior art, the present invention is introduced the carboxylic group with electronegativity by oxidation processes
Natural silk fiber, being aided with the scattered mode of mild mechanical realizes the silk nanofiber dispersion liquid for retaining preferable prototype structure
Efficient preparation.Silk nanofiber prepared by the present invention has pH responses simultaneously, can be realized by the regulation and control to pH value
The precipitation separation of silk nanofiber and redisperse, are easy to store and transport, and have pole in correlation function material structure field
Big potential value.
Brief description of the drawings
Fig. 1 is silk nanofiber transmission electron microscope picture；Wherein, left figure is silkworm nanofiber, and right figure is tussah Nanowire
Dimension；
Fig. 2 is titration curve figure before and after the oxidation of mulberry silk nanofiber；Left figure is original mulberry silk fiber titration curve, and right figure is
Mulberry silk fiber titration curve after oxidation；
Fig. 3 is that silk nanofiber precipitates redisperse phenomenon under different pH；Left figure is mulberry silk nanofiber, and right figure is tussah
Silk nanofiber.
Embodiment
Below in conjunction with specific embodiment, the invention will be further elaborated.Embodiment is for illustrative and not limiting hair
It is bright.Any those of ordinary skill in this area can do appropriate it will be appreciated that these embodiments do not limit the present invention in any way
Modification and without prejudice to the present invention essence and deviate the scope of the present invention.
In following examples, used assay method is as follows：Silk fiber carboxyl-content is aoxidized to determine：By 0.1 g oxygen
Silk fiber after change is added in 60 mL distilled water, and stirring 30 min by magnetic rotor makes suspension be uniformly dispersed；With 0.1
The pH of mixed system is adjusted to 3 and stable 5min by M HCl；0.05M NaOH are then added dropwise to mixing with 0.1mL/min speed
The pH of system is 11.The conductance value changes of mixed system and the NaOH consumptions consumed, pass through titration in record said process
Curve calculates carboxyl-content.
Embodiment 1：The formic acid processing of boiled silk fiber
Silk fiber after 10g degummings is taken, with 1：20 solid-to-liquid ratio is added in 30 wt% formic acid solution, centrifugation point after 48 h of immersion
From silk fiber and formic acid solution.Silk fiber is cleaned to neutrality with distilled water in case using；Centrifugation obtains formic acid solution can
To reuse.
Embodiment 2：The formic acid processing of boiled silk fiber
Silk fiber after 10 g degummings is taken, with 1：20 solid-to-liquid ratio is added in 80 wt% formic acid solution, centrifugation point after 2 h of immersion
From silk fiber and formic acid solution.Silk fiber is cleaned to neutrality with distilled water in case using；Centrifugation obtains formic acid solution can
To reuse.
Embodiment 3：Hypochlorite oxidation prepares silk nanofiber
Weigh the silk fiber after the processing of 1 g formic acid to be scattered in 100 mL distilled water, 0.1 mM NaClO are added, with 200 r/
Min speed is stirred, and it is 10 times 1 h of room temperature reaction to maintain pH.Reaction terminate after using 0.5 mol/L HCl by system pH adjust to
Neutrality, 10 min are centrifuged with 10000 r/min, and sediment fraction is centrifuged repeatedly cleaning 5 times.Now water-insoluble fraction mass recovery
For 95.9%.Water-insoluble fraction is placed in 100 mL deionized waters in ultrasonic 2 min under 19.5 kHz, 300 W power, 5 are repeated
It is secondary；It is silk nanofiber dispersion liquid that centrifugation, which obtains supernatant fraction,.
Embodiment 4：Hypochlorous acid oxidization prepares silk nanofiber
Weigh the silk fiber after the processing of 1 g formic acid to be scattered in 100 mL distilled water, 15 mM HClO are added, with 200 r/
Min speed is stirred, and it is 10 times 1 h of room temperature reaction to maintain pH.Reaction terminate after using 0.5 mol/L HCl by system pH adjust to
Neutrality, 10 min are centrifuged with 10000 r/min, and sediment fraction is centrifuged repeatedly cleaning 5 times.Now water-insoluble fraction mass recovery
For 58.6%.Water-insoluble fraction is placed in 100 mL deionized waters in ultrasonic 2 min under 19.5 kHz, 300 W power, 5 are repeated
It is secondary；It is silk nanofiber dispersion liquid that centrifugation, which obtains supernatant fraction,.
Embodiment 5：Hypochlorite oxidation prepares silk nanofiber
The silk fiber after the processing of 1 g formic acid is weighed, adds and is sufficiently stirred in 100 mL distilled water, silk fiber is fully divided
Dissipate.Add 15 mM NaClO to be aoxidized at room temperature, stirred with 200 r/min speed, it is 10 times 2 h of reaction to maintain pH.Instead
System pH is adjusted to neutrality using 0.5 mol/L HCl after should terminating, 10 min, sediment fraction are centrifuged with 10000 r/min
It is centrifuged repeatedly cleaning 5 times；Now water-insoluble fraction mass recovery is 73.3%.Water-insoluble fraction is placed in 100 mL deionizations
In 19.5 kHz in water, ultrasonic 2 min, is repeated 5 times under 300 W power；It is silk Nanowire that centrifugation, which obtains supernatant fraction,
Tie up dispersion liquid.
Embodiment 6：Hypochlorite oxidation prepares silk nanofiber
The silk fiber after the processing of 1 g formic acid is weighed, adds and is sufficiently stirred in 100 mL distilled water, silk fiber is fully divided
Dissipate.Add 30 mM NaClO to be aoxidized at room temperature, stirred with 200 r/min speed, it is 10 times 2 h of reaction to maintain pH.Instead
System pH is adjusted to neutrality using 0.5 mol/L HCl after should terminating, 10 min, sediment fraction are centrifuged with 10000 r/min
It is centrifuged repeatedly cleaning 5 times；Now water-insoluble fraction mass recovery is 50.2%.Water-insoluble fraction is placed in 100 mL deionizations
In 19.5 kHz in water, ultrasonic 2 min, is repeated 5 times under 300 W power；It is silk Nanowire that centrifugation, which obtains supernatant fraction,
Tie up dispersion liquid.
Embodiment 7：Silk nanofiber dispersion liquid precipitate redisperse
50 mL silkworm nanofiber dispersion liquid are taken, dispersion liquid pH is adjusted to 5, portion must be precipitated with 5000 r/min centrifuging and takings
Point, it is 20.6% to be calculated respectively by constant weight method and obtain the moisture of precipitation, and now solid recovery rate is 80.1%.
By the silk nanofiber mixed system pH precipitated under acid condition by 0.05 M NaOH adjust to pH 7 with
On；Or after aqueous precipitate is centrifuged, the min of magnetic agitation 10 in distilled water, can make the silk nanometer of precipitation again
Fiber re-forms the dispersion liquid of stable uniform.
Embodiment 8：Silk nanofiber dispersion liquid precipitate redisperse
50 mL silkworm nanofiber dispersion liquid are taken, dispersion liquid pH is adjusted to 3, portion must be precipitated with 5000 r/min centrifuging and takings
Point, it is 21.2% to be calculated respectively by constant weight method and obtain the moisture of precipitation, and now solid recovery rate is 93.6%.
By the silk nanofiber mixed system pH precipitated under acid condition by 0.05 M NaOH adjust to pH 7 with
On；Or after aqueous precipitate is centrifuged, the min of magnetic agitation 10 in distilled water, can make the silk nanometer of precipitation again
Fiber re-forms the dispersion liquid of stable uniform.
Embodiment 9：Silk nanofiber performance measurement
The silk nanofiber prepared by above-described embodiment 4 is selected to carry out performance measurement, it is as a result as follows：
1）Silk nanofiber transmission electron microscope picture is as shown in figure 1, left figure is mulberry silk nanofiber, and right figure is tussah silk Nanowire
Dimension.As shown in Figure 1, the nanofiber dispersion that prepared by this oxidation system is uniform, and the diameter of silk nanofiber is in 100 nm or so
And length can reach several microns.
2）Mulberry silk titration curve change before and after oxidation is right as shown in Fig. 2 left figure is original mulberry silk fiber titration curve
Figure is mulberry silk fiber titration curve after oxidation.It can be seen that oxidizing process make it that carboxyl-content produces obvious increase in silk fiber.
3）Silk nanofiber precipitate redisperse phenomenon under different pH as shown in figure 3, left figure be mulberry silk nanofiber,
Right figure is tussah silk nanofiber.From figure can no matter mulberry silk or tussah silk nanofiber, have at acidic bright
Aobvious deposited phenomenon, and as pH replys neutral, it can be separated into the nanofiber dispersion liquid of stable homogeneous again.
Claims (10)
1. a kind of preparation method of silk nanofiber dispersion liquid, it is characterised in that silk fiber is pre-processed through formic acid first, so
After carry out oxidation processes, obtained finally by decentralized processing with stablizing the silk nanofiber dispersion liquid of nanofibrous structures.
2. the preparation method of silk nanofiber dispersion liquid according to claim 1, it is characterised in that the formic acid is located in advance
Reason, the concentration of formic acid is more than 30%wt, handles 0.5 ~ 72h.
3. the preparation method of silk nanofiber dispersion liquid according to claim 1 or 2, it is characterised in that described oxygen
Change processing chemical oxidizing agent or (and) biology enzyme oxidant.
4. the preparation method of silk nanofiber dispersion liquid according to claim 3, it is characterised in that described chemical oxygen
Agent is any of hypohalogenous acids, hypohalite, hydrogen peroxide, ozone, peracid；Described biological enzyme agent is peroxidating
Any of hydrogen and oxidation enzymatic mixture, laccase, peroxidase, oxidant is preferably sodium hypochlorite.
5. the preparation method of silk nanofiber dispersion liquid according to claim 1, it is characterised in that described scattered place
Manage as mechanical dispersion processing.
6. the preparation method of silk nanofiber dispersion liquid according to claim 1, it is characterised in that described silk bag
Include mulberry silk, tussah silk, spider silk and other silks.
What 7. the preparation method of the silk nanofiber dispersion liquid described in claim 1 was obtained receives with electronegativity single-silk
Rice fiber dispersion.
8. silk nanofiber dispersion liquid according to claim 7, it is characterised in that described silk nanofiber dispersion
Liquid has pH responses, and the precipitation separation of silk nanofiber can be realized by the regulation of pH value, and redisperse turns into performance
Stable silk nanofiber dispersion liquid.
9. a kind of silk nanofiber obtained from the silk nanofiber dispersion liquid described in claim 7, it is characterised in that
The carboxyl-content of the silk nanofiber is 0.3 more than mmol/g of the weight relative to the silk nanofiber.
10. silk nanofiber according to claim 9, it is characterised in that the diameter of the single-silk nanofiber
For 50-500 nm, length is 10 μm of 50 nm-.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109161975A (en) * | 2018-09-18 | 2019-01-08 | 南京林业大学 | PH responsive type fibroin nanofiber and its dispersion liquid, preparation method and application |
| CN109957848A (en) * | 2019-02-28 | 2019-07-02 | 常州市协旺纺织品有限公司 | A kind of preparation method of modification regeneration fibroin fiber |
| CN112442190A (en) * | 2019-08-29 | 2021-03-05 | 武汉大学 | Preparation method of silk nano material |
| CN113818238A (en) * | 2021-08-24 | 2021-12-21 | 南京林业大学 | Preparation method and application of functional fibroin nanofiber, dispersion liquid and composite material |
| CN114703651A (en) * | 2022-03-14 | 2022-07-05 | 安徽农业大学 | Method for extracting silk micro/nano fibers through oxidation modification and application of silk micro/nano fibers |
| CN115354408A (en) * | 2022-08-17 | 2022-11-18 | 西南大学 | Preparation method, product and application of nano tussah silk fiber |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109161975A (en) * | 2018-09-18 | 2019-01-08 | 南京林业大学 | PH responsive type fibroin nanofiber and its dispersion liquid, preparation method and application |
| CN109161975B (en) * | 2018-09-18 | 2021-02-02 | 南京林业大学 | PH-sensitive fibroin nanofiber, and dispersion liquid, preparation method and application thereof |
| CN109957848A (en) * | 2019-02-28 | 2019-07-02 | 常州市协旺纺织品有限公司 | A kind of preparation method of modification regeneration fibroin fiber |
| CN112442190A (en) * | 2019-08-29 | 2021-03-05 | 武汉大学 | Preparation method of silk nano material |
| CN112442190B (en) * | 2019-08-29 | 2022-04-01 | 武汉大学 | Preparation method of silk nano material |
| CN113818238A (en) * | 2021-08-24 | 2021-12-21 | 南京林业大学 | Preparation method and application of functional fibroin nanofiber, dispersion liquid and composite material |
| CN114703651A (en) * | 2022-03-14 | 2022-07-05 | 安徽农业大学 | Method for extracting silk micro/nano fibers through oxidation modification and application of silk micro/nano fibers |
| CN115354408A (en) * | 2022-08-17 | 2022-11-18 | 西南大学 | Preparation method, product and application of nano tussah silk fiber |
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