CN115354408A - Preparation method, product and application of nano tussah silk fiber - Google Patents
Preparation method, product and application of nano tussah silk fiber Download PDFInfo
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Abstract
The invention relates to a preparation method, a product and application of nano tussah silk fiber, wherein natural tussah silk fibroin is swelled through formic acid treatment, and then the tussah silk fibroin is peeled through mechanical action, so that tussah silk fibrils are separated from each other, and the nano tussah silk fiber is obtained. The nanometer tussah silk fiber prepared by the method is not chemically modified, and the amino acid sequence is completely consistent with that of natural tussah silk. In addition, the nano tussah silk fiber has large specific surface area, and a large amount of RGD sequences originally hidden in the tussah silk are exposed. The RGD sequence can promote platelet adhesion and aggregation; can promote M2 type polarization of macrophage, thereby inhibiting inflammation. Therefore, the nano tussah fiber prepared by the method has excellent hemostatic property, biocompatibility, degradability, cell migration promoting capacity, anti-inflammation and wound healing promoting capacity.
Description
Technical Field
The invention relates to the technical field of biomedicine, in particular to a preparation method, a product and application of nano tussah silk fiber.
Background
The arginine-glycine-aspartic acid (RGD) sequence can be specifically combined with integrin on the cell surface, and has multiple functions of promoting cell adhesion, regulating macrophage polarization, promoting angiogenesis and the like; the natural tussah silk has low price, and the amino acid composition of the silk fibroin is rich in RGD sequence, so the natural tussah silk is an ideal raw material for preparing RGD related biological materials; however, a large amount of RGD sequences are wrapped inside the tussah silk, and the tussah silk is directly used for preparing biological materials, so that the obtained biological functionality is very limited; although tussah silk can be dissolved to obtain regenerated silk fibroin, the RGD sequence inside the tussah silk is exposed, high-concentration lithium thiocyanate is needed during the tussah silk dissolution, and dialysis desalination is needed during the purification, so that the preparation process is high in cost and complicated in process, the environmental pollution caused by wastewater is large, and the industrial production is not facilitated; in addition, the regenerated tussah silk fibroin is unstable, is easy to be converted into beta-sheet conformation to be precipitated, and is not beneficial to processing and production.
Similar to the structure of mulberry silk, tussah silk is also composed of nano-scale fibrils which are arranged in parallel. If the fibrils can be peeled off by a physical method, the nano tussah fiber can be obtained. The nano tussah fiber has large specific surface area and a large amount of RGD sequences distributed on the surface, and can be used for preparing various biological materials on the basis of the RGD sequences. At present, the related research of preparing nano tussah silk by direct peeling is less, and mainly comprises the steps of oxidizing hydroxyl groups carried by serine in tussah silk protein into carboxyl groups by using oxides, ionizing the carboxyl groups under an alkaline condition, and enabling the tussah silk fibrils to be negatively charged and mutually exclusive, so that the fibrils are peeled. The method is relatively complicated to operate, and changes the chemical structure and amino acid composition of the tussah silk protein, so that the method also has great influence on the biological functionality of the nano tussah fiber. At present, no biomedical function report of the nano tussah fiber prepared by the method exists. Therefore, if a new processing method can be developed, on the premise of not changing the chemical structure and amino acid composition of tussah silk protein, the process is simplified, the cost is reduced, the production efficiency is improved, and the development and application of tussah silk related materials in the related fields of biomedicine can be greatly promoted.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of nano tussah silk fiber, a nano tussah silk fiber product and application of the nano tussah silk fiber aiming at the defects in the prior art.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a preparation method of nano tussah silk fiber is constructed, which comprises the following steps:
degumming tussah cocoons to obtain tussah fibroin;
soaking degummed tussah silk fibroin in formic acid solution with certain concentration at a certain temperature to obtain dispersion A;
carrying out suction filtration on the dispersion liquid A to obtain a dispersion liquid B;
performing wall breaking treatment on the dispersion liquid B to obtain a dispersion liquid C;
and carrying out suction filtration or centrifugal washing on the dispersion liquid C to be neutral to obtain a nano tussah silk fiber dispersion liquid D.
The method for preparing the nano tussah silk fiber of the invention is characterized in that the concentration range of the formic acid solution is 0.1-100 percent by weight.
The preparation method of the nano tussah silk fiber provided by the invention is characterized in that the nano tussah silk fiber is soaked in formic acid solution at the temperature of 0-100 ℃ for 0.1-720 h.
The invention relates to a preparation method of nano tussah silk fiber, wherein the formic acid solution is soaked by the method comprising the following steps:
and (3) placing the degummed tussah silk in 20-100% formic acid solution for incubation for 0.6-24 h at the temperature of 4-100 ℃ to obtain the dispersion A.
The preparation method of the nano tussah silk fiber comprises the following steps of:
and carrying out suction filtration on the dispersion liquid A until the pH range is 5-9 to obtain a dispersion liquid B.
The preparation method of the nano tussah silk fiber provided by the invention is characterized in that the method for breaking the wall of the dispersion liquid B to obtain the dispersion liquid C comprises the following steps:
and stripping the dispersion liquid B by using mechanical action for 0.15-24 h to obtain a dispersion liquid C.
The preparation method of the nano tussah silk fiber comprises the following steps of:
and centrifuging the dispersion liquid C for 1-30 min under the centrifugal force of 1000-10000 g, or performing suction filtration and washing to obtain the nano tussah silk fiber dispersion liquid D with neutral pH.
A nano tussah silk fiber product is prepared according to the preparation method of the nano tussah silk fiber.
The application of the nano tussah silk fiber product is in one or more of hemostasis, inflammation inhibition and wound healing promotion.
The invention has the beneficial effects that:
firstly, the preparation method of the nano tussah silk fibroin fiber is simple, the nano tussah silk fibroin fiber can be obtained only through formic acid pretreatment and mechanical stripping, and the cost is low.
Secondly, the nano tussah silk fiber is not chemically modified, and the amino acid sequence and the chemical components are consistent with those of natural tussah silk.
Thirdly, the nanometer tussah silk fibroin fiber of the invention reserves the RGD structure of natural tussah.
The nano tussah fiber prepared by the method has good biocompatibility, degradability, cell migration promoting capability, hemostatic capability, anti-inflammation capability and wound healing promoting capability, and is a biomedical material with ideal performance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the present invention will be further described with reference to the accompanying drawings and embodiments, wherein the drawings in the following description are only part of the embodiments of the present invention, and for those skilled in the art, other drawings can be obtained without inventive efforts according to the accompanying drawings:
FIG. 1 is a flow chart of a method for preparing nano tussah silk fibers according to a preferred embodiment of the present invention;
FIG. 2 is a scanning electron micrograph of the degummed, formic acid pretreated and wall-broken samples of the inventive composition D2 and the comparative example E2;
FIG. 3 is a schematic diagram showing the comparison of biocompatibility between the nano tussah silk fiber D1 and the nano mulberry silk fiber E1;
FIG. 4 is a graph showing the results of macrophage polarization modulation in D3 of the present invention and comparative example E3;
FIG. 5 is a schematic diagram showing macrophage polarized fluorescence quantification of the present invention D3 and a comparative example E3;
FIG. 6 is a schematic representation of the cell migration results of the cell scratch assay of the present invention;
FIG. 7 is a photograph of a hemostatic experiment of the broken tail of a mouse according to the present invention;
FIG. 8 is a graph showing the effect of example D2 of the present invention and comparative example E2 on the treatment of rat full skin defects.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the following description will be made clearly and completely in conjunction with the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without inventive step, are within the scope of the present invention.
The preparation method of the nano tussah silk fiber in the preferred embodiment of the invention, as shown in fig. 1, comprises the following steps:
s01: degumming the tussah cocoons to obtain tussah silk fibroin;
s02: soaking degummed tussah silk fibroin in formic acid solution with certain concentration at a certain temperature to obtain dispersion A;
s03: carrying out suction filtration on the dispersion liquid A to obtain a dispersion liquid B;
s04: performing wall breaking treatment on the dispersion B to obtain a dispersion C;
s05: carrying out suction filtration or centrifugal washing on the dispersion liquid C to be neutral to obtain a nano tussah silk fiber dispersion liquid D;
the invention aims to provide a method for preparing nano tussah silk fibers, which has the advantages of low price, simple preparation and chemical structure and amino acid sequence consistent with those of natural tussah silk. The principle of the invention is as follows: the natural tussah silk fibroin is swelled through formic acid treatment, and then the tussah silk fibroin is peeled through mechanical action, so that the tussah silk fibrils are separated from each other, and the nanoscale tussah silk fiber is obtained.
The nano tussah silk fiber prepared by the method is not subjected to chemical modification, the amino acid sequence is completely consistent with that of natural tussah silk, in addition, the specific surface area of the nano tussah silk fiber is large, the RGD sequence originally hidden in the tussah silk is greatly exposed, and the RGD sequence can promote the adhesion and aggregation of blood platelets; can promote M2 type polarization of macrophage, thereby inhibiting inflammation.
Therefore, the nano tussah fiber prepared by the method has excellent hemostatic property, biocompatibility, degradability, cell migration promoting capacity, anti-inflammation and wound healing promoting capacity.
It should be noted that:
tussah silk fibroin is obtained by degumming tussah cocoons, the existing technical means is adopted, and the common mode is as follows: adding Na with certain concentration into tussah cocoon at certain temperature 2 CO 3 Tussah fibroin is obtained after the solution degumming, and other existing modes are available;
solvents for the formic acid solution include, but are not limited to, water; formic acid concentrations include, but are not limited to, 0.1 to 100% (w/v), e.g., 2%, 5%, 8%, 16%, 19%, 23%, 28%, 29%, 35%, 37%, 41%, 43%, 56%, 59%, 76%, 82%, 92%, 95%, 97%, etc. are selected;
it is understood that formic acid solution can be replaced by other existing acidic solution which can be used for soaking natural tussah silk fibroin, and equivalent replacement of the conventional means also belongs to the protection scope of the present application.
When natural tussah silk is treated by formic acid solution, nano tussah fiber can be obtained at different soaking temperatures and time durations, wherein the blending temperature includes but is not limited to 0-100 ℃, and the soaking time includes but is not limited to 0.1-720 h.
The degummed tussah silk is placed in 20-100% formic acid solution to be incubated for 0.6-24 hours at the temperature of 4-100 ℃ to obtain dispersion A, and relatively good effect can be obtained;
the temperature can be selected, for example, at 5 deg.C, 10 deg.C, 15 deg.C, 20 deg.C, 25 deg.C, 30 deg.C, 35 deg.C, 40 deg.C, 45 deg.C, 50 deg.C, 55 deg.C, 60 deg.C, 65 deg.C, 70 deg.C, 75 deg.C, 80 deg.C, 85 deg.C, 90 deg.C, 95 deg.C, 100 deg.C, etc.;
optional times are, for example, 1h, 1.5h, 2.5h, 3.5h, 4h, 5.5h, 7h, 8h, 10h, 11.5h, 13h, 14h, 16.5h, 18h, 20h, 21h, 23h, and the like.
Preferably, the dispersion liquid A is filtered by suction to obtain the dispersion liquid B by the following method: and carrying out suction filtration on the dispersion liquid A until the pH range is 5-9 to obtain a dispersion liquid B.
Preferably, the method for breaking the wall of the dispersion liquid B to obtain the dispersion liquid C comprises the following steps: and stripping the dispersion liquid B by using mechanical action for 0.15-24 h to obtain a dispersion liquid C.
Preferably, the dispersion liquid C is subjected to suction filtration or centrifugal washing to be neutral to obtain the nano tussah silk fiber dispersion liquid D by the following method: centrifuging the dispersion C at a centrifugal force of 1000-10000 g for 1-30 min, or performing suction filtration and washing to obtain a nano tussah silk fiber dispersion D with neutral pH;
a nano tussah silk fiber product is prepared according to the preparation method of the nano tussah silk fiber.
An application of a nano tussah silk fiber product, wherein the nano tussah silk fiber product is applied to one or more of hemostasis, inflammation inhibition and wound healing promotion.
The present invention will be described in further detail with reference to specific embodiments.
Example 1
1) Weighing formic acid to prepare 5w/v%,10w/v%,30w/v% and 60w/v% aqueous solutions A1, A2, A3 and A4;
2) Weighing 4g of degummed natural tussah silk, and averagely dividing into 4 parts;
3) Respectively adding 4 parts of tussah silk into A1-A4, and respectively incubating at 100, 60, 40 and 20 ℃ for 1h.
4) And respectively breaking the walls of the tussah silk samples by using a wall breaking machine for 0.5h, and then performing suction filtration until the pH value of the dispersion is 7 to obtain nano tussah silk samples D1, D2, D3 and D4.
Comparative example 2
Weighing formic acid to prepare 5w/v%,10w/v%,30w/v% and 60w/v% aqueous solutions A1, A2, A3 and A4;
2) Weighing 4g of degummed natural mulberry silk, and averagely dividing into 4 parts;
3) Adding 4 parts of mulberry silk into the A1-A4 respectively, and incubating for 1h at 100, 60, 40 and 20 ℃.
4) And respectively treating for 0.5h by using a wall breaking machine, and then performing suction filtration until the pH value is 7 to obtain nano mulberry silk samples E1, E2, E3 and E4.
Example of effects:
the properties of the tussah silk fibers D1 to D4 and the mulberry silk fibers E1 to E4 prepared in example 1 and comparative example 2 were measured.
Effect example 1: characterization of surface topography
After degumming, formic acid pretreatment and wall breaking of the nano tussah silk fiber and the mulberry silk fiber prepared in the embodiment 1 and the comparative example 2, a certain amount of sample is respectively taken for scanning electron microscope observation. FIG. 2 is a scanning electron microscope image of the degumming, formic acid pretreatment and wall breaking of the comparative example E2 and example D2. Table 1 shows the filament fiber diameters as counted by scanning electron microscopy.
FIG. 2: the silk degumming agent comprises (a) degummed tussah silk, x 500, (b) tussah silk subjected to formic acid pretreatment, x 500, (c) tussah silk subjected to wall breaking, x 3000, (d) degummed mulberry silk, x 500, (e) mulberry silk subjected to formic acid pretreatment, x 500, (f) mulberry silk subjected to wall breaking, and x 3000;
table 1: statistical results of silk fiber diameter
As can be seen from fig. 2 and table 1, after the formic acid pretreatment, the fibrils originally arranged in close parallel in the natural tussah silk were partially peeled off, and the average diameter of the nano tussah fiber prepared in example 1 was about 100 nm.
Effect example 2: determination of biocompatibility
Macrophages of 2X 104 cells/well were seeded onto 96-well plates for overnight culture. A certain amount of the nano tussah fiber D1 (ApNSF) prepared in example 1 and the nano mulberry fiber E1 (BmNSF) prepared in control example 2 are respectively incubated with cells for 24 hours, and then 100 mu L of MTT is added for incubation for 4 hours, and then the OD value is detected.
As can be seen from fig. 3, the nano tussah fiber prepared in example 1 has good biocompatibility, and the cell viability thereof is greater than 80%.
Effect example 3: measurement of anti-inflammatory Effect
Aiming at the anti-inflammatory function of the nano tussah silk fibroin fiber, 4 multiplied by 105 cell/hole macrophages are inoculated on a six-hole plate for overnight culture in order to confirm the effect. The macrophage polarization is induced by 0.5 mug/mL LPS, then certain amount of nano tussah fiber D3 of the embodiment and nano mulberry fiber E3 of the comparison example are respectively taken to be incubated with the macrophages for 24h, iNOS and MRC-1 are respectively added for incubation overnight, finally, CD86 and CD206 are respectively used for immunostaining M1 type and M2 type macrophages, and the fluorescence value is quantified. FIG. 4 shows the macrophage polarization modulation results of example D3 (ApNSF) and control example E3 (BmNSF), and FIG. 5 is a fluorescence quantification chart. Tables 2-1 and 2-2 show the results of fluorescence quantification of the polarization effect.
FIG. 4: m1 type macrophage polarization (left), M2 type macrophage polarization (right);
FIG. 5: m1 type macrophage polarization fluorescence quantification (left), M2 type macrophage polarization fluorescence quantification (right);
TABLE 2-1 fluorescence quantification of macrophage M1-type polarization for example D3 and control example E3
| Negative control | Postive control | D3 | E3 | |
| MFI | 3.832 | 11.285 | 4.234 | 4.903 |
Table 2-2 fluorescence quantification of macrophage M2-type polarization in example B3 and control C3
| Negative control | Postive control | D3 | E3 | |
| MFI | 3.226 | 3.718 | 7.183 | 4.343 |
Fig. 4, fig. 5, tables 2-1 and 2-2 show that the nano tussah fiber prepared in example 1 can promote the conversion of macrophages from pro-inflammatory M1 type macrophages to anti-inflammatory M2 type macrophages, and has a remarkable anti-inflammatory effect.
Effect example 4: measurement of cell migration promoting Property
Aiming at the cell migration promoting capability of the nano tussah silk fibroin fiber material, in order to confirm the effect, 7 × 105 cell/hole L929 cells are inoculated on a six-hole plate for overnight culture, a 200 μ L gun head is used for scratching, after PBS is used for cleaning once, the nano tussah silk fiber D4 (ApNSF) of the embodiment and the nano tussah silk fiber E4 (BmNSF) of the comparison example are respectively incubated with fibroblasts for 24h and 48h, and then the migration distance of the fibroblasts is observed and counted. FIG. 6 shows the cell migration results of the cell scratch test. Table 3 is a quantitative result of the scratch residual ratio.
FIG. 6: migration results after L929 cell scratch
TABLE 3 scratch residue ratio
| Group of | Control | D4 | E4 |
| Scratch residue (24 h) | 93.28％ | 95.59％ | 90.89％ |
| Scratch residue (48 h) | 89.90％ | 65.37％ | 88.27％ |
Fig. 6 and table 3 prove that the nano tussah silk prepared in the example has good ability of promoting cell migration.
Effect example 5: measurement of hemostatic Properties
Aiming at the hemostatic function of the nano tussah silk fibroin fiber, in order to confirm the effect, a mouse tail-broken hemostatic experiment is carried out. Cutting 3cm of mouse tail, treating wound with nanometer tussah fiber D2 (ApNSF) of example and nanometer mulberry fiber E2 (BmNSF) of control example after natural bleeding for 30s, and recording mouse tail hemostasis time and bleeding amount at 30, 60 and 120s respectively. Positive control group was blood cotton. Fig. 7 is a photograph of the mouse tail-broken hemostasis experiment, and table 4 shows the quantitative hemostasis time and bleeding amount.
FIG. 7 photographs of hemostatic experiment of mouse after tail-broken
TABLE 4 hemostasis time and bleeding volume
| Negative Control | Positive Control | D2 | E2 | |
| Amount of hemostasis (mg) | 620.5 | 157.53 | 145.3 | 654.3 |
| Hemostasis time(s) | 160.6 | 86.6 | 73.6 | 124.3 |
Fig. 7 and table 4 demonstrate that the nano tussah fiber prepared in example 1 has good hemostatic effect.
Effect example 6: determination of degradation Properties
In order to confirm the effect of the degradation performance of the nano tussah fiber of the present invention, the nano tussah fiber B1 of the example and the nano tussah fiber C1 of the comparative example were degraded with proteinase K and papain, respectively, and the fiber residual weights after the enzyme treatment were weighed at 0, 48, 96, 144, and 192 hours, respectively. Tables 5-1 and 5-2 show the degradation rates of example D1 and comparative example E1.
TABLE 5-1 degradation Rate of the Nano tussah fibers D1 of the examples
| 0h | 48h | 96h | 192h | |
| Proteinase K | 95.67％ | 77.17％ | 76.48％ | 67.63％ |
| Papain | 98.60％ | 90.91％ | 88.56％ | 86.65％ |
TABLE 5-2 degradation rates of the comparative examples of the NanoBombyx mori fibre E1
| 0h | 48h | 96h | 192h | |
| Proteinase K | 92.54％ | 73.25％ | 70.27％ | 67.49％ |
| Papain | 92.83％ | 93.13％ | 91.77％ | 90.26％ |
Tables 5-1 and 5-2 prove that the nano tussah silk has good degradability.
Effect example 7: determination of wound healing
In order to determine the capability of the nano tussah fiber in promoting wound healing, a rat full-skin defect model with the diameter of 1cm is constructed, and the nano tussah fiber D2 (ApNSF) of the embodiment and the nano mulberry fiber E2 (BmNSF) of the control example are respectively used for treatment.
Fig. 8 is a photograph of wound condition at 0, 3, 5, 7, 9, 11 and 12 days post-surgery.
FIG. 8 therapeutic effect of example D2 (ApNSF) and control E2 (BmNSF) on rat full skin defects.
FIG. 8 shows that the nano tussah fiber prepared by the embodiment can obviously promote the wound healing of the full-skin defect.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (10)
1. The preparation method of the nano tussah silk fiber is characterized by comprising the following steps:
degumming the tussah cocoons to obtain tussah silk fibroin;
soaking degummed tussah silk fibroin in formic acid solution with certain concentration at a certain temperature to obtain dispersion A;
carrying out suction filtration on the dispersion liquid A to obtain a dispersion liquid B;
performing wall breaking treatment on the dispersion liquid B to obtain a dispersion liquid C;
and carrying out suction filtration or centrifugal washing on the dispersion liquid C to be neutral to obtain a nano tussah silk fiber dispersion liquid D.
2. The method for preparing nano tussah silk fiber according to claim 1, wherein the concentration of formic acid solution is 0.1-100% w/v.
3. The method for preparing the nano tussah silk fiber according to claim 2, wherein the soaking temperature is 0-100 ℃ and the soaking time is 0.1-720 h.
4. The method for preparing the nano tussah silk fiber according to claim 3, wherein the formic acid solution soaking treatment adopts a method comprising the following steps:
and (3) placing the degummed tussah silk in 20-100% formic acid solution for incubation for 0.6-24 h at the temperature of 4-100 ℃ to obtain the dispersion A.
5. The method for preparing nano tussah silk fiber according to any one of claims 1 to 4, wherein the dispersion A is filtered to obtain the dispersion B by the following method:
and carrying out suction filtration on the dispersion liquid A until the pH range is 5-9 to obtain a dispersion liquid B.
6. The method for preparing the nano tussah silk fiber according to any one of claims 1 to 4, wherein the method for breaking the wall of the dispersion solution B to obtain the dispersion solution C comprises the following steps:
and stripping the dispersion liquid B by using mechanical action for 0.15-24 h to obtain a dispersion liquid C.
7. The method for preparing nano tussah silk fiber according to any one of claims 1 to 4, wherein the dispersion C is filtered or washed by centrifugation to neutral to obtain nano tussah silk fiber dispersion D by the following method:
and centrifuging the dispersion liquid C for 1-30 min under the centrifugal force of 1000-10000 g, or performing suction filtration and washing to obtain the nano tussah silk fiber dispersion liquid D with neutral pH.
8. The method for preparing the nano tussah silk fiber according to any one of claims 1 to 4, wherein the tussah silk fibroin obtained by degumming tussah cocoons is obtained by a method comprising the following steps:
adding Na with certain concentration into tussah cocoon at certain temperature 2 CO 3 Obtaining tussah silk fibroin after degumming the solution.
9. A nano tussah silk fiber product, which is characterized in that the nano tussah silk fiber product is prepared according to the preparation method of the nano tussah silk fiber of any one of claims 1 to 8.
10. The use of the nano tussah silk fiber product of claim 9 for one or more of hemostasis, inflammation inhibition, and wound healing.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2017070873A1 (en) * | 2015-10-28 | 2017-05-04 | 南通纺织丝绸产业技术研究院 | High performance natural silk fiber and preparation method thereof |
| CN106884033A (en) * | 2017-03-16 | 2017-06-23 | 江苏鑫缘丝绸科技有限公司 | A kind of nanometer fibroin powder and preparation method thereof |
| CN107083674A (en) * | 2017-05-25 | 2017-08-22 | 南京林业大学 | A kind of preparation method of silk nanofiber dispersion liquid |
| US20200181213A1 (en) * | 2016-05-04 | 2020-06-11 | Trustees Of Tufts College | Silk Nanofibrils and Uses Thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017070873A1 (en) * | 2015-10-28 | 2017-05-04 | 南通纺织丝绸产业技术研究院 | High performance natural silk fiber and preparation method thereof |
| US20200181213A1 (en) * | 2016-05-04 | 2020-06-11 | Trustees Of Tufts College | Silk Nanofibrils and Uses Thereof |
| CN106884033A (en) * | 2017-03-16 | 2017-06-23 | 江苏鑫缘丝绸科技有限公司 | A kind of nanometer fibroin powder and preparation method thereof |
| CN107083674A (en) * | 2017-05-25 | 2017-08-22 | 南京林业大学 | A kind of preparation method of silk nanofiber dispersion liquid |
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