CN111501121A - Method for preparing collagen fiber by wet spinning - Google Patents
Method for preparing collagen fiber by wet spinning Download PDFInfo
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- CN111501121A CN111501121A CN201910099095.XA CN201910099095A CN111501121A CN 111501121 A CN111501121 A CN 111501121A CN 201910099095 A CN201910099095 A CN 201910099095A CN 111501121 A CN111501121 A CN 111501121A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F4/00—Monocomponent artificial filaments or the like of proteins; Manufacture thereof
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
- D06M2101/14—Collagen fibres
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Abstract
The invention relates to a method for preparing collagen fiber by wet spinning, which comprises the steps of firstly dissolving I type collagen in NaAc/HAc buffer solution with the pH value of 3.0 at room temperature to obtain collagen solution with high collagen content, carrying out vacuum-pumping defoaming treatment, adopting absolute ethyl alcohol as coagulating bath, preparing fiber with high collagen content by a wet spinning mode, and carrying out green crosslinking treatment on the fiber to obtain collagen fiber with good performance. Compared with the prior art, the invention adopts NaAc/HAc buffer solution as the green solvent of collagen, thereby greatly improving the content of collagen in the fiber; the collagen fiber is prepared by using absolute ethyl alcohol which is a coagulation bath which is not commonly used in the wet spinning of the collagen, and the ethyl alcohol is volatile and has no toxicity; the whole preparation method has mild conditions and green and simple process, and the prepared collagen fiber has good biocompatibility and excellent mechanical property, can achieve the purpose of adjustable degradation rate, and provides a new way for the preparation and application of the collagen-based medical composite fiber.
Description
Technical Field
The invention belongs to the field of preparation of biomedical materials, and particularly relates to a method for preparing collagen fibers by wet spinning.
Background
Collagen constitutes the skeleton of extracellular matrix, provides certain tensile strength and elasticity for cells as a biomacromolecule substance, plays a very important role in a living body, and is widely applied to the field of biomedical materials, such as surgical sutures, artificial skins, collagen sponges, artificial blood vessels and the like, cosmetics, food industry and the like. However, collagen has a specific triple-helix structure, and numerous secondary bond actions such as hydrogen bonds, ionic bonds, van der waals forces, hydrophobic bonds and the like exist in molecules, so that the collagen is difficult to dissolve in common solvents, and the application of the collagen is greatly limited.
At present, in the process of preparing collagen-based biomaterials, researchers at home and abroad often use organic solvents such as Hexafluoroisopropanol (HFIP) and trifluorides, weak acid systems such as phosphoric acid, acetic acid and hydrochloric acid, phosphate buffer solution/ethanol mixed systems, ionic liquids, and the like as collagen solvents. However, after HFIP dissolves collagen, the triple helix structure of collagen is destroyed, so that it is denatured and disordered structure is increased; the solubility of collagen in conventional weak acid solvents is low, which is not favorable for the performance of collagen characteristics, such as high toughness and high elasticity. Acetic acid is a common collagen dissolving mode, but the concentration of dissolved collagen is low, and a large amount of polyvinyl alcohol is often added for improving the spinnability of the composite spinning solution, so that the content of collagen in the composite fiber is reduced. Although the use of a (PBS)/ethanol mixed solvent can avoid the disadvantages of toxicity and the like of materials caused by HFIP, a large amount of salt is introduced in the system due to the use of PBS, and dialysis treatment is required; although the ionic liquid is used by the characteristics of low volatility, good solubility, stable property and the like, the ionic liquid also has potential toxicity, and the collagen is denatured due to overhigh dissolution temperature. Therefore, how to prepare the collagen nanofibers by adopting a green process, and further improve the performance and reduce the cost are the main directions for the future research and development of biomedical materials.
Disclosure of Invention
In order to solve the problems, the invention provides a method for preparing collagen fibers by wet spinning, which can be used as medical materials such as suture lines, brackets and the like, and greatly expands the application of the collagen-based composite fibers in the medical field.
The object of the invention is achieved in the following way:
a method for preparing collagen fibers by wet spinning comprises the following steps:
(1) dissolving I type collagen in NaAc/HAc buffer solution, and continuously stirring at room temperature until the I type collagen is completely dissolved to obtain collagen solution;
(2) carrying out vacuum-pumping defoaming treatment on the collagen solution to obtain a collagen spinning solution;
(3) carrying out wet spinning on the collagen spinning solution, and after the fibers obtained by the wet spinning are fully shaped, drawing and winding to obtain collagen fibers;
(4) and (3) airing the collagen fibers at room temperature, then carrying out crosslinking treatment, and airing the fibers subjected to crosslinking treatment at room temperature to obtain a finished collagen fiber product.
And (3) adopting absolute ethyl alcohol as a coagulating bath in the wet spinning process.
And (3) the crosslinking agent adopted in the crosslinking treatment in the step (4) is genipin.
The pH value of the NaAc/HAc buffer solution in the step (1) is 2.8-3.2.
The pH of the NaAc/HAc buffer solution in the step (1) is 3.
The concentration of the type I collagen in the collagen solution in the step (1) is 50mg/m L-200 mg/m L.
The crosslinking treatment process in the step (4) comprises the following steps: first, genipin was dissolved in a mixed solution of acetone and water, acetone: the volume ratio of water is (8.5-9.5): 1, a cross-linking mixed solution is obtained, the mass concentration of genipin in the cross-linking mixed solution is 0.6% -1%, and then the fiber is taken out after being soaked in the cross-linking mixed solution for 24-48 h.
The preparation process of the NaAc/HAc buffer solution in the step (1) comprises the following steps: sodium acetate was dissolved in a mixed solution of acetic acid and H2O, and its pH was adjusted with glacial acetic acid.
The spinning temperature in the wet spinning in the step (3) is 25-30 ℃.
Compared with the prior art, the invention has the following advantages:
1. the NaAc/HAc buffer solution is used as a green solvent of collagen, so that the content of the collagen in the fiber is greatly improved;
2. the collagen fiber is prepared by using absolute ethyl alcohol which is a coagulation bath which is not commonly used in the wet spinning of the collagen, and the ethyl alcohol is volatile and has no toxicity;
3. the whole preparation method has mild conditions and green and simple process, the prepared collagen fiber has good biocompatibility and excellent mechanical property, and has a microporous structure, and the size of the prepared collagen fiber is controllable, so that the purpose of regulating and controlling the degradation rate can be achieved, and a new way is provided for the preparation and application of the collagen-based medical composite fiber.
Drawings
FIG. 1 is an SEM photograph (magnification of 5000) of the longitudinal structure of the collagen fibers obtained in example 2.
FIG. 2 is an SEM photograph (magnification: 10000 times) of a cross section of the collagen fiber obtained in example 2.
FIG. 3 is a schematic diagram of the collagen fibers obtained in example 2.
Detailed Description
Example 1
A method for preparing collagen fibers by wet spinning comprises the following steps:
(1) dissolving I type collagen in NaAc/HAc buffer solution, and continuously stirring at room temperature until the I type collagen is completely dissolved to obtain collagen solution;
(2) carrying out vacuum-pumping defoaming treatment on the collagen solution to obtain a collagen spinning solution;
(3) carrying out wet spinning on the collagen spinning solution, and after the fibers obtained by the wet spinning are fully shaped, drawing and winding to obtain collagen fibers;
(4) and (3) airing the collagen fibers at room temperature, then carrying out crosslinking treatment, and airing the fibers subjected to crosslinking treatment at room temperature to obtain a finished collagen fiber product.
And (3) adopting absolute ethyl alcohol as a coagulating bath in the wet spinning process.
And (3) the crosslinking agent adopted in the crosslinking treatment in the step (4) is genipin.
The pH value of the NaAc/HAc buffer solution in the step (1) is 2.8-3.2.
The pH of the NaAc/HAc buffer solution in the step (1) is 3.
The concentration of the type I collagen in the collagen solution in the step (1) is 50mg/m L-200 mg/m L.
The crosslinking treatment process in the step (4) comprises the following steps: first, genipin was dissolved in a mixed solution of acetone and water, acetone: the volume ratio of water is (8.5-9.5): 1, a cross-linking mixed solution is obtained, the mass concentration of genipin in the cross-linking mixed solution is 0.6% -1%, and then the fiber is taken out after being soaked in the cross-linking mixed solution for 24-48 h.
The preparation process of the NaAc/HAc buffer solution in the step (1) comprises the following steps: dissolving sodium acetate in acetic acid and H2And adjusting the pH value of the mixed solution of O by using glacial acetic acid.
The spinning temperature in the wet spinning in the step (3) is 25-30 ℃.
Example 2
A method for preparing collagen fibers by wet spinning comprises the following steps:
(1) dissolving I type collagen in NaAc/HAc buffer solution with pH of 3.0, soaking overnight, stirring in water bath at constant temperature of 25 ℃ until completely dissolving to obtain collagen solution, wherein the concentration of the I type collagen is 100mg/m L;
(2) filtering, vacuumizing and defoaming the collagen spinning solution to obtain the collagen spinning solution;
(3) adding the defoamed collagen spinning solution into a wet spinning experimental device, pushing out the spinning solution from a needle at the speed of 5m L/h through an injection pump, feeding the spinning solution into a coagulating bath taking absolute ethyl alcohol as a coagulating bath agent, and drafting and winding after fibers obtained by a wet spinning process are fully shaped to obtain collagen fibers, wherein the inner diameter of the needle of the injector is 0.08mm, and the spinning temperature is 25 ℃.
(4) Drying the collagen fiber at room temperature, and then performing crosslinking treatment, wherein the crosslinking treatment process comprises the following steps: 0.6% genipin was dissolved in acetone: soaking the collagen fibers in a solvent with the water ratio of 9:1 for 24 hours, taking out, and airing at room temperature to obtain a finished product of the collagen fibers.
The obtained collagen fiber finished product is tested, the breaking strength of the collagen fiber can reach 245.8N/dtex, the breaking elongation of the collagen fiber is 46 percent, and the fiber has better mechanical strength and flexibility. Scanning the collagen with an electron microscope to obtain SEM images as shown in FIGS. 1 and 2, wherein the SEM images show that the collagen fibers are continuous and have smooth surfaces as shown in FIG. 1; from the cross section of fig. 2, the collagen fiber shows irregular shape, which is caused by incomplete setting and drafting of the spinning solution in the coagulating bath during the drafting process of the wet spinning fiber, and granular micropore structure exists in the middle of the fiber section, which is caused by the outward diffusion of the solvent in the fiber, the diffusion of the coagulant into the fiber, and the double diffusion effect. Fig. 3 is a real image of collagen fiber, and it can be seen that the fiber has uniform size, good flexibility, and can be fixedly wound.
Example 3
A method for preparing collagen fibers by wet spinning comprises the following steps:
(1) dissolving type I collagen in NaAc/HAc buffer solution with pH of 2.8, and stirring at constant temperature in water bath at room temperature until the type I collagen is completely dissolved to obtain collagen solution, wherein the concentration of the type I collagen is 50mg/m L;
(2) filtering, vacuumizing and defoaming the collagen spinning solution to obtain the collagen spinning solution;
(3) adding the defoamed collagen spinning solution into a wet spinning experimental device, pushing out the spinning solution from a needle at the speed of 5m L/h through an injection pump, feeding the spinning solution into a coagulating bath taking absolute ethyl alcohol as a coagulating bath agent, and drafting and winding after fibers obtained by a wet spinning process are fully shaped to obtain collagen fibers, wherein the inner diameter of the needle of the injector is 0.08mm, and the spinning temperature is 25 ℃.
(4) Drying the collagen fiber at room temperature, and then performing crosslinking treatment, wherein the crosslinking treatment process comprises the following steps: 0.6% genipin was dissolved in acetone: soaking the collagen fiber in a solvent with the water ratio of 8.5:1 for 24h, taking out, and airing at room temperature to obtain a finished collagen fiber product. The finished product of the collagen fiber obtained by the method is tested, and the fiber has better mechanical strength and flexibility.
Example 4
A method for preparing collagen fibers by wet spinning comprises the following steps:
(1) dissolving type I collagen in NaAc/HAc buffer solution with pH of 3.2, soaking overnight, stirring in water bath at constant temperature of 25 ℃ until the type I collagen is completely dissolved, wherein the concentration of the type I collagen is 200mg/m L;
(2) filtering, vacuumizing and defoaming the collagen spinning solution to obtain the collagen spinning solution;
(3) adding the defoamed collagen spinning solution into a wet spinning experimental device, pushing out the spinning solution from a needle at the speed of 5m L/h through an injection pump, feeding the spinning solution into a coagulating bath taking absolute ethyl alcohol as a coagulating bath agent, and drafting and winding after fibers obtained by a wet spinning process are fully shaped to obtain collagen fibers, wherein the inner diameter of the needle of the injector is 0.08mm, and the spinning temperature is 30 ℃.
(4) Drying the collagen fiber at room temperature, and then performing crosslinking treatment, wherein the crosslinking treatment process comprises the following steps: dissolve 1% genipin in acetone: soaking the collagen fiber in a solvent with the water ratio of 9.5:1 for 48h, taking out, and airing at room temperature to obtain a finished collagen fiber product. The finished product of the collagen fiber obtained by the method is tested, and the fiber has better mechanical strength and flexibility.
Example 5
A method for preparing collagen fibers by wet spinning comprises the following steps:
(1) dissolving I type collagen in NaAc/HAc buffer solution with pH of 2.9, soaking overnight, stirring in water bath at constant temperature of 25 ℃ until completely dissolving to obtain collagen solution, wherein the concentration of the I type collagen is 60mg/m L;
(2) filtering, vacuumizing and defoaming the collagen spinning solution to obtain the collagen spinning solution;
(3) adding the defoamed collagen spinning solution into a wet spinning experimental device, pushing out the spinning solution from a needle at the speed of 5m L/h through an injection pump, feeding the spinning solution into a coagulating bath taking absolute ethyl alcohol as a coagulating bath agent, and drafting and winding after fibers obtained by a wet spinning process are fully shaped to obtain collagen fibers, wherein the inner diameter of the needle of the injector is 0.08mm, and the spinning temperature is 25 ℃.
(4) Drying the collagen fiber at room temperature, and then performing crosslinking treatment, wherein the crosslinking treatment process comprises the following steps: 0.8% genipin was dissolved in acetone: soaking the collagen fiber in a solvent with the water ratio of 8.7:1 for 24 hours, taking out, and airing at room temperature to obtain a finished collagen fiber product. The finished product of the collagen fiber obtained by the method is tested, and the fiber has better mechanical strength and flexibility.
Example 6
A method for preparing collagen fibers by wet spinning comprises the following steps:
(1) dissolving I type collagen in NaAc/HAc buffer solution with the pH value of 2.8, soaking for one night, then stirring in water bath at constant temperature of 25 ℃ until the I type collagen is completely dissolved to obtain collagen solution, wherein the concentration of the I type collagen is 180mg/m L;
(2) filtering, vacuumizing and defoaming the collagen spinning solution to obtain the collagen spinning solution;
(3) adding the defoamed collagen spinning solution into a wet spinning experimental device, pushing out the spinning solution from a needle at the speed of 5m L/h through an injection pump, feeding the spinning solution into a coagulating bath taking absolute ethyl alcohol as a coagulating bath agent, and drafting and winding after fibers obtained by a wet spinning process are fully shaped to obtain collagen fibers, wherein the inner diameter of the needle of the injector is 0.08mm, and the spinning temperature is 25 ℃.
(4) Drying the collagen fiber at room temperature, and then performing crosslinking treatment, wherein the crosslinking treatment process comprises the following steps: 0.6% genipin was dissolved in acetone: soaking the collagen fiber in a solvent with the water ratio of 8.5:1 for 48h, taking out, and airing at room temperature to obtain a finished collagen fiber product. The finished product of the collagen fiber obtained by the method is tested, and the fiber has better mechanical strength and flexibility.
Example 7
A method for preparing collagen fibers by wet spinning comprises the following steps:
(1) dissolving I type collagen in NaAc/HAc buffer solution with pH of 3.2, soaking overnight, stirring in water bath at constant temperature of 25 ℃ until completely dissolving to obtain collagen solution, wherein the concentration of the I type collagen is 50mg/m L;
(2) filtering, vacuumizing and defoaming the collagen spinning solution to obtain the collagen spinning solution;
(3) adding the defoamed collagen spinning solution into a wet spinning experimental device, pushing out the spinning solution from a needle at the speed of 5m L/h through an injection pump, feeding the spinning solution into a coagulating bath taking absolute ethyl alcohol as a coagulating bath agent, and drafting and winding after fibers obtained by a wet spinning process are fully shaped to obtain collagen fibers, wherein the inner diameter of the needle of the injector is 0.08mm, and the spinning temperature is 25 ℃.
(4) Drying the collagen fiber at room temperature, and then performing crosslinking treatment, wherein the crosslinking treatment process comprises the following steps: dissolve 1% genipin in acetone: soaking collagen fibers in a solvent with the water ratio of 9.5:1 for 40h, taking out, and airing at room temperature to obtain a finished collagen fiber product. The finished product of the collagen fiber obtained by the method is tested, and the fiber has better mechanical strength and flexibility.
Example 8
A method for preparing collagen fibers by wet spinning comprises the following steps:
(1) dissolving I type collagen in NaAc/HAc buffer solution with pH of 3.1, soaking overnight, stirring in water bath at constant temperature of 25 ℃ until completely dissolving to obtain collagen solution, wherein the concentration of the I type collagen is 140mg/m L;
(2) filtering, vacuumizing and defoaming the collagen spinning solution to obtain the collagen spinning solution;
(3) adding the defoamed collagen spinning solution into a wet spinning experimental device, pushing out the spinning solution from a needle at the speed of 5m L/h through an injection pump, feeding the spinning solution into a coagulating bath taking absolute ethyl alcohol as a coagulating bath agent, and drafting and winding after fibers obtained by a wet spinning process are fully shaped to obtain collagen fibers, wherein the inner diameter of the needle of the injector is 0.08mm, and the spinning temperature is 27 ℃.
(4) Drying the collagen fiber at room temperature, and then performing crosslinking treatment, wherein the crosslinking treatment process comprises the following steps: 0.9% genipin was dissolved in acetone: soaking the collagen fiber in a solvent with the water ratio of 9.2:1 for 30h, taking out, and airing at room temperature to obtain a finished collagen fiber product. The finished product of the collagen fiber obtained by the method is tested, and the fiber has better mechanical strength and flexibility.
Example 9
A method for preparing collagen fibers by wet spinning comprises the following steps:
(1) dissolving I type collagen in NaAc/HAc buffer solution with the pH value of 2.8, soaking for one night, then stirring in water bath at constant temperature of 25 ℃ until the I type collagen is completely dissolved to obtain collagen solution, wherein the concentration of the I type collagen is 80mg/m L;
(2) filtering, vacuumizing and defoaming the collagen spinning solution to obtain the collagen spinning solution;
(3) adding the defoamed collagen spinning solution into a wet spinning experimental device, pushing out the spinning solution from a needle at the speed of 5m L/h through an injection pump, feeding the spinning solution into a coagulating bath taking absolute ethyl alcohol as a coagulating bath agent, and drafting and winding after fibers obtained by a wet spinning process are fully shaped to obtain collagen fibers, wherein the inner diameter of the needle of the injector is 0.08mm, and the spinning temperature is 30 ℃.
(4) Drying the collagen fiber at room temperature, and then performing crosslinking treatment, wherein the crosslinking treatment process comprises the following steps: 0.6% genipin was dissolved in acetone: soaking the collagen fiber in a solvent with the water ratio of 8.5:1 for 35h, taking out, and airing at room temperature to obtain a finished collagen fiber product. The finished product of the collagen fiber obtained by the method is tested, and the fiber has better mechanical strength and flexibility.
Example 10
A method for preparing collagen fibers by wet spinning comprises the following steps:
(1) dissolving I type collagen in NaAc/HAc buffer solution with pH of 3.0, soaking overnight, stirring in water bath at constant temperature of 25 ℃ until completely dissolving to obtain collagen solution, wherein the concentration of the I type collagen is 200mg/m L;
(2) filtering, vacuumizing and defoaming the collagen spinning solution to obtain the collagen spinning solution;
(3) adding the defoamed collagen spinning solution into a wet spinning experimental device, pushing out the spinning solution from a needle at the speed of 5m L/h through an injection pump, feeding the spinning solution into a coagulating bath taking absolute ethyl alcohol as a coagulating bath agent, and drafting and winding after fibers obtained by a wet spinning process are fully shaped to obtain collagen fibers, wherein the inner diameter of the needle of the injector is 0.08mm, and the spinning temperature is 30 ℃.
(4) Drying the collagen fiber at room temperature, and then performing crosslinking treatment, wherein the crosslinking treatment process comprises the following steps: dissolve 1% genipin in acetone: soaking the collagen fiber in a solvent with the water ratio of 8.5:1 for 24h, taking out, and airing at room temperature to obtain a finished collagen fiber product. The finished product of the collagen fiber obtained by the method is tested, and the fiber has better mechanical strength and flexibility.
Example 11
A method for preparing collagen fibers by wet spinning comprises the following steps:
(1) dissolving I type collagen in NaAc/HAc buffer solution with pH of 3.2, soaking overnight, stirring in water bath at constant temperature of 25 ℃ until completely dissolving to obtain collagen solution, wherein the concentration of the I type collagen is 50mg/m L;
(2) filtering, vacuumizing and defoaming the collagen spinning solution to obtain the collagen spinning solution;
(3) adding the defoamed collagen spinning solution into a wet spinning experimental device, pushing out the spinning solution from a needle at the speed of 5m L/h through an injection pump, feeding the spinning solution into a coagulating bath taking absolute ethyl alcohol as a coagulating bath agent, and drafting and winding after fibers obtained by a wet spinning process are fully shaped to obtain collagen fibers, wherein the inner diameter of the needle of the injector is 0.08mm, and the spinning temperature is 25 ℃.
(4) Drying the collagen fiber at room temperature, and then performing crosslinking treatment, wherein the crosslinking treatment process comprises the following steps: dissolve 1% genipin in acetone: soaking the collagen fiber in a solvent with the water ratio of 9.5:1 for 24h, taking out, and airing at room temperature to obtain a finished collagen fiber product. The finished product of the collagen fiber obtained by the method is tested, and the fiber has better mechanical strength and flexibility.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the overall concept of the invention, and these should be considered as the protection scope of the present invention, which will not affect the effect of the implementation of the present invention and the practicability of the patent.
Claims (9)
1. A method for preparing collagen fibers by wet spinning is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
(1) dissolving I type collagen in NaAc/HAc buffer solution, and continuously stirring at room temperature until the I type collagen is completely dissolved to obtain collagen solution;
(2) carrying out vacuum-pumping defoaming treatment on the collagen solution to obtain a collagen spinning solution;
(3) carrying out wet spinning on the collagen spinning solution, and after the fibers obtained by the wet spinning are fully shaped, drawing and winding to obtain collagen fibers;
(4) and (3) airing the collagen fibers at room temperature, then carrying out crosslinking treatment, and airing the fibers subjected to crosslinking treatment at room temperature to obtain a finished collagen fiber product.
2. The method for preparing collagen fibers by wet spinning according to claim 1, wherein: and (3) adopting absolute ethyl alcohol as a coagulating bath in the wet spinning process.
3. The method for preparing collagen fibers by wet spinning according to claim 1 or 2, wherein: and (3) the crosslinking agent adopted in the crosslinking treatment in the step (4) is genipin.
4. The method for preparing collagen fibers by wet spinning according to claim 1, wherein: the pH value of the NaAc/HAc buffer solution in the step (1) is 2.8-3.2.
5. The method for preparing collagen fibers by wet spinning according to claim 4, wherein: the pH of the NaAc/HAc buffer solution in the step (1) is 3.
6. The method for preparing collagen fiber by wet spinning according to claim 1, wherein the concentration of type I collagen in the collagen solution of step (1) is 50mg/m L-200 mg/m L.
7. A method of wet spinning collagen fibers as claimed in claim 3, wherein: the crosslinking treatment process in the step (4) comprises the following steps: first, genipin was dissolved in a mixed solution of acetone and water, acetone: the volume ratio of water is (8.5-9.5): 1, a cross-linking mixed solution is obtained, the mass concentration of genipin in the cross-linking mixed solution is 0.6% -1%, and then the fiber is taken out after being soaked in the cross-linking mixed solution for 24-48 h.
8. The method for preparing collagen fibers by wet spinning according to claim 1, wherein: the preparation process of the NaAc/HAc buffer solution in the step (1) comprises the following steps: dissolving sodium acetate in acetic acid and H2And adjusting the pH value of the mixed solution of O by using glacial acetic acid.
9. The method for preparing collagen fibers by wet spinning according to claim 1, wherein: the spinning temperature in the wet spinning in the step (3) is 25-30 ℃.
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| CN110607570A (en) * | 2019-09-29 | 2019-12-24 | 袁春雅 | Medical absorbable biomaterial filament |
| CN114182381A (en) * | 2022-01-24 | 2022-03-15 | 浙江启宏新材料科技有限责任公司 | Preparation method of collagen fiber, collagen fiber and application |
| KR20220050369A (en) * | 2020-10-16 | 2022-04-25 | 주식회사 파이버엔텍 | Process Of Producing High-Strength Collagen Filament |
| CN115559009A (en) * | 2022-10-31 | 2023-01-03 | 得福乐(南通)科技有限公司 | Collagen filament with collagen microfiber structure and preparation method thereof |
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| CN115559009A (en) * | 2022-10-31 | 2023-01-03 | 得福乐(南通)科技有限公司 | Collagen filament with collagen microfiber structure and preparation method thereof |
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