Collagen multifilament fiber and its preparation method and application
Through the wet spinning method and three-stage coagulation bath technology, the problem of winding collagen multifilament fibers in the production process was solved, and high-performance collagen multifilament fibers suitable for textile and medical fields were prepared.
Patent Information
- Application Number
- CN202411202355.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-29
- Publication Date
- 2025-09-19
- Estimated Expiration
- 2044-08-29
AI Technical Summary
The existing technology is difficult to solve the problem of paralleling of collagen multifilament fibers during the production process, which hinders its industrialization process.
Collagen multifilament fibers were prepared by wet spinning method, through coagulation of collagen spinning solution in three-stage coagulation bath, combined with water-soluble cross-linking agent and high aspect ratio spinneret to prevent parallel yarn adhesion.
The stable production of collagen multifilament fibers has been achieved, which have excellent mechanical properties and are suitable for textile and medical fields.
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Figure CN118932517B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of new material textiles, and in particular to a collagen multifilament fiber and a preparation method and application thereof. Background Art
[0002] Collagen is a protein with a unique triple-helical structure. It is a structural protein in the extracellular matrix and the most abundant protein in animals, accounting for approximately 30% of total protein. The helical region of collagen is composed of multiple repeating sequences of Gly-XY, where Gly represents glycine. The X and Y positions can be any amino acid, but are typically proline (Pro) and hydroxyproline (Hyp). These repeating sequences give collagen its unique stability and structural properties. Collagen is composed of three α-polypeptide chains, each exhibiting a left-handed helical structure. These chains then interlock through hydrogen bonds to form a right-handed superhelical structure, a stable triple helix. This structure gives collagen excellent mechanical properties and biocompatibility. Furthermore, a collagen molecule is composed of three left-handed helical polypeptide chains (secondary structure), which intertwine to form a right-handed helix (tertiary structure) around a central molecular axis. A complete collagen molecule is approximately 280 nm in length and 1.5 nm in diameter. The diversity and complexity of collagen's structure and functions give it broad application prospects in numerous fields.
[0003] Currently, most collagen spinning research uses organic solvents or acids to dissolve collagen, and is primarily limited to the laboratory stage of producing monofilaments. For example, Patent Publication No. CN108977912A discloses a method for producing collagen fibers, using acid to dissolve collagen to produce collagen monofilaments. Patent Publication No. CN111235662A discloses a long collagen fiber with a natural structure, its preparation method, and application, using a fluoroalcohol as a solvent to dissolve collagen, also producing collagen monofilaments. The key research and development direction for the future is to develop collagen multifilament fibers that meet the requirements of industrial production and subsequent applications.
[0004] In addition, the viscosity of collagen colloidal dispersion is orders of magnitude higher than that of conventional polymer wet spinning solution. During the extrusion process of conventional wet spinning equipment, the extrusion swelling effect of collagen spinning solution is obvious, which is not conducive to spinning. Moreover, during the preparation of collagen multifilament, the single filaments are very likely to stick together, which seriously hinders its industrialization process.
[0005] Therefore, the present invention provides a collagen multifilament fiber and a preparation method and application thereof to solve the above problems. Summary of the Invention
[0006] The technical problem to be solved by the present invention is to provide a collagen multifilament fiber and a preparation method thereof, so as to solve the problem of paralleling of collagen multifilament fibers during the production process and lay the foundation for the subsequent industrial application of collagen multifilament fibers.
[0007] To solve the above technical problems, the technical solution of the present invention is: a method for preparing collagen multifilament fibers, the innovation of which is that the preparation method comprises the following steps:
[0008] Step (1), fully swelling bovine collagen in deionized water, adding a water-soluble crosslinking agent, and stirring at room temperature for 2 to 8 hours to obtain a collagen colloidal dispersion;
[0009] Step (2), filtering the collagen colloid dispersion through a filter screen and performing a centrifugal degassing treatment to obtain a collagen spinning solution;
[0010] Step (3): The collagen spinning solution is squeezed into a coagulation bath through a wet spinning device, and the collagen multifilament fibers are obtained through drawing, washing, stretching and drying.
[0011] Furthermore, the water-soluble cross-linking agent in step (1) is glutaraldehyde, genipin or EDC / NHS, with a concentration of 0.01% to 1%, preferably a concentration of glutaraldehyde of 0.06% to 0.12%.
[0012] Furthermore, the concentration of the collagen colloid in the collagen colloid dispersion in step (1) is 10 mg / ml to 50 mg / ml, preferably 15 mg / ml to 35 mg / ml.
[0013] Furthermore, the mesh size of the filter in step (2) is 60-150 mesh, preferably 80-120 mesh.
[0014] Furthermore, the wet spinning device in step (3) includes an air compressor, a charging kettle, a candle filter, a metering pump, a spinneret, a stretching device, a drying device and a winding device;
[0015] The collagen spinning solution is placed in a charging kettle, filtered through a candle filter, extruded through a metering pump and a spinneret in sequence, and enters a coagulation bath to form primary collagen fibers. The primary collagen fibers are coagulated and formed in the coagulation bath, then enter a cleaning bath for cleaning and exit the bath. The fibers are stretched by a stretching device, dried by a drying device, and finally wound by a winding device to obtain collagen multifilament fibers.
[0016] Furthermore, the air compressor provides a pressure of 0.1 MPa to 0.6 MPa, preferably 0.3 MPa to 0.5 MPa, to the charging kettle;
[0017] The metering pump extrusion speed is 0.3 ml / min ~ 5 ml / min, the spinneret stretch ratio is 0.5~1, the preferred extrusion speed is 0.6 ml / min ~ 1.5 ml / min, and the preferred spinneret stretch ratio is 0.8~1;
[0018] The number of holes in the spinneret is ≥ 2, the hole diameter is 0.05 mm to 0.3 mm, and the aspect ratio is 20 to 200. The preferred hole diameter is 0.1 mm to 0.25 mm, and the preferred aspect ratio is 50 to 100.
[0019] The coagulation bath length is 0.5 m ~ 3 m, and the coagulation bath temperature is 15℃ ~ 45℃;
[0020] The cleaning bath is an ethanol solution with a concentration of 30% to 70%;
[0021] The exit speed is 0.2 m / min ~ 5 m / min;
[0022] The stretching ratio of the stretching device is 1 to 5, preferably 1 to 3;
[0023] The drying temperature of the drying device is 20℃ ~ 50℃;
[0024] The winding speed of the winding device is 0.2 m / min to 10 m / min, preferably 5 m / min to 10 m / min.
[0025] Furthermore, the coagulation bath in step (3) is a three-stage coagulation bath, which includes a first stage coagulation bath, a second stage coagulation bath, and a third stage coagulation bath arranged in sequence;
[0026] The first coagulation bath is an alkaline solution of PEG8000 with a mass concentration of 15% to 25% and a pH of 9 to 13;
[0027] The second coagulation bath is an alkaline solution of PEG20000 with a mass concentration of 20% to 30% and a pH of 9 to 13;
[0028] The third coagulation bath is an inorganic salt solution with a mass concentration of 20% to 60%.
[0029] Furthermore, the inorganic salt solution includes but is not limited to sodium chloride, sodium sulfate, sodium carbonate, sodium nitrate, potassium chloride, potassium sulfate, potassium carbonate, potassium nitrate, ammonium chloride, ammonium sulfate, ammonium carbonate, and ammonium nitrate.
[0030] By adopting the above technical solution, the collagen spinning solution coagulates when squeezed into the alkaline solution of the coagulation bath, forming collagen primary fibers. During the pulling process, the collagen primary fibers undergo double diffusion with the coagulation bath solution. Water in the collagen primary fibers diffuses into the solution, and solutes in the solution diffuse into the collagen primary fibers, causing the collagen primary fibers to gradually solidify and form. The PEG8000 alkaline solution in the first coagulation bath has a low viscosity, which reduces the resistance encountered during the pulling process of the collagen primary fibers, allowing the collagen primary fibers to be pulled stably. The PEG20000 alkaline solution in the second coagulation bath has a high viscosity and a faster diffusion rate of water into the solution, which further coagulates the collagen primary fibers. The inorganic salt solution in the third coagulation bath has a strong coagulation effect, which can completely coagulate the collagen primary fibers and effectively prevent the collagen multifilament fibers from sticking together during the collection process.
[0031] The collagen multifilament fiber prepared by the above preparation method has a fiber fineness of 10 dtex to 200 dtex.
[0032] The collagen multifilament fibers are used in the textile and medical fields.
[0033] The advantages of the present invention are:
[0034] (1) The present invention can produce collagen multifilament fibers with excellent mechanical properties, which can meet the textile requirements of textiles;
[0035] (2) The present invention distributes and solidifies the primary collagen fibers through a three-stage coagulation bath, which can effectively prevent the occurrence of parallel strand adhesion of collagen multifilament fibers;
[0036] (3) The present invention reduces the extrusion swell effect of the collagen spinning solution during the extrusion process by designing a spinneret with a high aspect ratio, making the spinning of collagen smoother;
[0037] (4) The preparation method of the present invention is simple to operate and requires relatively mild conditions, and can be industrialized for production. Fibers of different diameters can be prepared according to demand. BRIEF DESCRIPTION OF THE DRAWINGS
[0038] The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
[0039] Figure 1 This is a physical picture of the collagen multifilament fiber prepared by the preparation method of the present invention.
[0040] Figure 2 The electron microscope image shows the microscopic morphology of the collagen multifilament fiber prepared by the preparation method of the present invention.
[0041] Figure 3This is a diagram showing the mechanical properties of collagen multifilament fibers prepared by the preparation method of the present invention. DETAILED DESCRIPTION
[0042] In order to further illustrate the technical means and effects adopted by the present invention to achieve the predetermined purpose of the invention, the specific implementation methods, structures, features and effects of the present invention are described in detail below in conjunction with the accompanying drawings and preferred embodiments.
[0043] Example 1
[0044] This embodiment provides a method for preparing collagen multifilament fibers, comprising the following steps:
[0045] Step (1), fully swelling bovine collagen in deionized water, adding 0.05% glutaraldehyde, and stirring at room temperature for 5 hours to obtain a collagen colloid dispersion, wherein the concentration of the collagen colloid in the collagen colloid dispersion is 20 mg / ml;
[0046] Step (2), filtering the collagen colloid dispersion through a filter screen and performing a centrifugal degassing treatment, wherein the mesh size of the filter screen is 100 meshes, and obtaining a collagen spinning solution after centrifugal degassing;
[0047] Step (3): The collagen spinning solution is squeezed into a coagulation bath through a wet spinning device, and the collagen multifilament fibers are obtained through traction, a washing bath, stretching and drying. The detailed process is as follows:
[0048] After the collagen spinning solution is placed in the charging kettle, the air compressor provides a pressure of 0.3MPa in the charging kettle, enters the candle filter for filtration, and then is extruded into the first coagulation bath through the metering pump and the spinneret in sequence. The extrusion speed of the metering pump is 1.2ml / min, the spinneret stretching ratio is 0.8, the number of holes in the spinneret is 40, the diameter of the spinneret hole is 0.2mm, and the aspect ratio is 50. The collagen spinning solution enters the first coagulation bath and is initially coagulated into collagen. The raw fibers and primary collagen fibers were further coagulated in the second and third coagulation baths in sequence until they were completely coagulated. The coagulation bath length was 2 m and the coagulation bath temperature was 30°C. The first coagulation bath was an alkaline solution of PEG8000 with a mass concentration of 20% and a pH value of 13; the second coagulation bath was an alkaline solution of PEG20000 with a mass concentration of 25% and a pH value of 13; the third coagulation bath was an ammonium sulfate solution with a mass concentration of 30%.
[0049] The completely coagulated primary collagen fibers were placed in a cleaning bath with a mass concentration of 50% ethanol solution to clean the PEG and ammonium sulfate on the fiber surface and then removed from the bath at a speed of 4 m / min. The fibers were stretched by a stretching device with a stretching ratio of 1.5. After stretching, they were dried by a drying device at a drying temperature of 40°C. After drying, they were finally wound by a winding device at a speed of 6 m / min to obtain collagen multifilament fibers.
[0050] The actual picture of collagen multifilament fiber Figure 1 As shown, the fiber single filament fineness of the collagen multifilament fiber is 12.7 dtex;
[0051] Field emission scanning electron microscopy was used to characterize the surface micromorphology of collagen multifilament fibers. Figure 2 As shown;
[0052] The mechanical properties of the obtained collagen multifilament fibers were tested using a multifilament yarn strength tester. The mechanical properties are shown in the figure below. Figure 3 As shown, the breaking elongation of the collagen multifilament fiber is 16.2%, and the breaking strength is 1.83 cN / dtex.
[0053] Example 2
[0054] This embodiment provides a method for preparing collagen multifilament fibers, comprising the following steps:
[0055] Step (1), fully swelling bovine collagen in deionized water, adding 0.05% glutaraldehyde, and stirring at room temperature for 5 hours to obtain a collagen colloid dispersion, wherein the concentration of the collagen colloid in the collagen colloid dispersion is 30 mg / ml;
[0056] Step (2), filtering the collagen colloid dispersion through a filter screen and performing a centrifugal degassing treatment, wherein the mesh size of the filter screen is 100 meshes, and obtaining a collagen spinning solution after centrifugal degassing;
[0057] Step (3): The collagen spinning solution is squeezed into a coagulation bath through a wet spinning device, and the collagen multifilament fibers are obtained through traction, a washing bath, stretching and drying. The detailed process is as follows:
[0058] After the collagen spinning solution is placed in the charging kettle, the air compressor provides a pressure of 0.3MPa in the charging kettle, enters the candle filter for filtration, and then is extruded into the first coagulation bath through the metering pump and the spinneret in sequence. The extrusion speed of the metering pump is 1.2ml / min, the spinneret stretching ratio is 0.8, the number of holes in the spinneret is 40, the diameter of the spinneret hole is 0.2mm, and the aspect ratio is 50. The collagen spinning solution enters the first coagulation bath and is initially coagulated into collagen. The raw fibers and primary collagen fibers were further coagulated in the second and third coagulation baths in sequence until they were completely coagulated. The coagulation bath length was 2 m and the coagulation bath temperature was 30°C. The first coagulation bath was an alkaline solution of PEG8000 with a mass concentration of 20% and a pH value of 13; the second coagulation bath was an alkaline solution of PEG20000 with a mass concentration of 25% and a pH value of 13; the third coagulation bath was an ammonium sulfate solution with a mass concentration of 30%.
[0059] The completely coagulated primary collagen fibers were placed in a cleaning bath with a mass concentration of 50% ethanol solution to clean the PEG and ammonium sulfate on the fiber surface and then removed from the bath at a speed of 4 m / min. The fibers were stretched by a stretching device with a stretching ratio of 1.5. After stretching, they were dried by a drying device at a drying temperature of 40°C. After drying, they were finally wound by a winding device at a speed of 6 m / min to obtain collagen multifilament fibers.
[0060] The collagen multifilament fibers obtained in this embodiment have a single filament fineness of 15.1 dtex, an elongation at break of 14.7%, and a breaking strength of 2.01 cN / dtex.
[0061] Example 3
[0062] This embodiment provides a method for preparing collagen multifilament fibers, comprising the following steps:
[0063] Step (1), fully swelling bovine collagen in deionized water, adding 0.1% glutaraldehyde, and stirring at room temperature for 5 hours to obtain a collagen colloid dispersion, wherein the concentration of the collagen colloid in the collagen colloid dispersion is 20 mg / ml;
[0064] Step (2), filtering the collagen colloid dispersion through a filter screen and performing a centrifugal degassing treatment, wherein the mesh size of the filter screen is 100 meshes, and obtaining a collagen spinning solution after centrifugal degassing;
[0065] Step (3): The collagen spinning solution is squeezed into a coagulation bath through a wet spinning device, and the collagen multifilament fibers are obtained through traction, a washing bath, stretching and drying. The detailed process is as follows:
[0066] After the collagen spinning solution is placed in the charging kettle, the air compressor provides a pressure of 0.3MPa in the charging kettle, enters the candle filter for filtration, and then is extruded into the first coagulation bath through the metering pump and the spinneret in sequence. The extrusion speed of the metering pump is 1.2ml / min, the spinneret stretching ratio is 0.8, the number of holes in the spinneret is 40, the diameter of the spinneret hole is 0.2mm, and the aspect ratio is 50. The collagen spinning solution enters the first coagulation bath and is initially coagulated into collagen. The raw fibers and primary collagen fibers were further coagulated in the second and third coagulation baths in sequence until they were completely coagulated. The coagulation bath length was 2 m and the coagulation bath temperature was 30°C. The first coagulation bath was an alkaline solution of PEG8000 with a mass concentration of 20% and a pH value of 13; the second coagulation bath was an alkaline solution of PEG20000 with a mass concentration of 25% and a pH value of 13; the third coagulation bath was an ammonium sulfate solution with a mass concentration of 30%.
[0067] The completely coagulated primary collagen fibers were placed in a cleaning bath with a mass concentration of 50% ethanol solution to clean the PEG and ammonium sulfate on the fiber surface and then removed from the bath at a speed of 4 m / min. The fibers were stretched by a stretching device with a stretching ratio of 1.5. After stretching, they were dried by a drying device at a drying temperature of 40°C. After drying, they were finally wound by a winding device at a speed of 6 m / min to obtain collagen multifilament fibers.
[0068] The collagen multifilament fibers obtained in this embodiment have a single filament fineness of 13.1 dtex, an elongation at break of 12.0%, and a breaking strength of 2.37 cN / dtex.
[0069] Example 4
[0070] This embodiment provides a method for preparing collagen multifilament fibers, comprising the following steps:
[0071] Step (1), fully swelling bovine collagen in deionized water, adding 0.05% glutaraldehyde, and stirring at room temperature for 5 hours to obtain a collagen colloid dispersion, wherein the concentration of the collagen colloid in the collagen colloid dispersion is 20 mg / ml;
[0072] Step (2), filtering the collagen colloid dispersion through a filter screen and performing a centrifugal degassing treatment, wherein the mesh size of the filter screen is 100 meshes, and obtaining a collagen spinning solution after centrifugal degassing;
[0073] Step (3): The collagen spinning solution is squeezed into a coagulation bath through a wet spinning device, and the collagen multifilament fibers are obtained through traction, a washing bath, stretching and drying. The detailed process is as follows:
[0074] After the collagen spinning solution is placed in the charging kettle, the air compressor provides a pressure of 0.3MPa in the charging kettle, enters the candle filter for filtration, and then is extruded into the first coagulation bath through the metering pump and the spinneret in sequence. The extrusion speed of the metering pump is 1.2ml / min, the spinneret stretching ratio is 0.8, the number of holes in the spinneret is 40, the diameter of the spinneret hole is 0.2mm, and the aspect ratio is 50. The collagen spinning solution enters the first coagulation bath and is initially coagulated into collagen. The raw fibers and primary collagen fibers were further coagulated in the second and third coagulation baths in sequence until they were completely coagulated. The coagulation bath length was 2 m and the coagulation bath temperature was 30 ° C. The first coagulation bath was an alkaline solution of PEG8000 with a mass concentration of 25% and a pH value of 13; the second coagulation bath was an alkaline solution of PEG20000 with a mass concentration of 30% and a pH value of 13; the third coagulation bath was an ammonium sulfate solution with a mass concentration of 50%.
[0075] The completely coagulated primary collagen fibers were placed in a cleaning bath with a mass concentration of 50% ethanol solution to clean the PEG and ammonium sulfate on the fiber surface and then removed from the bath at a speed of 4 m / min. The fibers were stretched by a stretching device with a stretching ratio of 1.5. After stretching, they were dried by a drying device at a drying temperature of 40°C. After drying, they were finally wound by a winding device at a speed of 6 m / min to obtain collagen multifilament fibers.
[0076] The collagen multifilament fibers obtained in this embodiment have a single filament fineness of 13.8 dtex, an elongation at break of 10.3%, and a breaking strength of 1.58 cN / dtex.
[0077] Example 5
[0078] This embodiment provides a method for preparing collagen multifilament fibers, comprising the following steps:
[0079] Step (1), fully swelling bovine collagen in deionized water, adding 0.05% glutaraldehyde, and stirring at room temperature for 5 hours to obtain a collagen colloid dispersion, wherein the concentration of the collagen colloid in the collagen colloid dispersion is 20 mg / ml;
[0080] Step (2), filtering the collagen colloid dispersion through a filter screen and performing a centrifugal degassing treatment, wherein the mesh size of the filter screen is 100 meshes, and obtaining a collagen spinning solution after centrifugal degassing;
[0081] Step (3): The collagen spinning solution is squeezed into a coagulation bath through a wet spinning device, and the collagen multifilament fibers are obtained through traction, a washing bath, stretching and drying. The detailed process is as follows:
[0082] After the collagen spinning solution is placed in the charging kettle, the air compressor provides a pressure of 0.3MPa in the charging kettle, enters the candle filter for filtration, and then is extruded into the first coagulation bath through the metering pump and the spinneret in sequence. The extrusion speed of the metering pump is 1.2ml / min, the spinneret stretching ratio is 0.8, the number of holes in the spinneret is 40, the diameter of the spinneret hole is 0.2mm, and the aspect ratio is 50. The collagen spinning solution enters the first coagulation bath and is initially coagulated into collagen. The raw fibers and primary collagen fibers were further coagulated in the second and third coagulation baths in sequence until they were completely coagulated. The coagulation bath length was 2 m and the coagulation bath temperature was 30°C. The first coagulation bath was an alkaline solution of PEG8000 with a mass concentration of 20% and a pH value of 13; the second coagulation bath was an alkaline solution of PEG20000 with a mass concentration of 25% and a pH value of 13; the third coagulation bath was an ammonium sulfate solution with a mass concentration of 30%.
[0083] The completely coagulated collagen primary fibers were placed in a cleaning bath with a mass concentration of 50% ethanol solution to clean the PEG and ammonium sulfate on the fiber surface and then removed from the bath at a speed of 5 m / min. The fibers were stretched by a stretching device with a stretching ratio of 1.8. After stretching, they were dried by a drying device at a drying temperature of 40°C. After drying, they were finally wound by a winding device at a speed of 9 m / min to obtain collagen multifilament fibers.
[0084] The collagen multifilament fibers obtained in this embodiment have a single filament fineness of 11.5 dtex, an elongation at break of 11.5%, and a breaking strength of 2.09 cN / dtex.
[0085] The parameters of the preparation methods of Examples 1 to 5 and the mechanical properties of the obtained collagen multifilament fibers are shown in Table 1.
[0086] Table 1 Parameters of the preparation methods of various examples and mechanical properties of collagen multifilament fibers
[0087]
[0088] The preparation method of the present invention is simple to operate, requires relatively mild conditions, can be industrialized for production, can prepare fibers of different diameters as required, and can effectively prevent the occurrence of strand adhesion in collagen multifilament fibers by distributing and coagulating the primary collagen fibers through a three-stage coagulation bath. The collagen multifilament fibers prepared by the preparation method of the present invention have excellent mechanical properties and can be applied in the textile and medical fields.
[0089] The above description is merely a preferred embodiment of the present invention and does not constitute any form of limitation to the present invention. Although the present invention has been disclosed as above in terms of a preferred embodiment, it is not intended to limit the present invention. Any person skilled in the art can, without departing from the scope of the technical solution of the present invention, make some changes or modifications to equivalent embodiments using the technical contents disclosed above. However, any brief modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention are still within the scope of the technical solution of the present invention.
Claims
1. A method for preparing collagen multifilament fiber, characterized in that: The preparation method comprises the following steps: Step (1), fully swelling bovine collagen in deionized water, adding a water-soluble crosslinking agent, and stirring at room temperature for 2 to 8 hours to obtain a collagen colloidal dispersion; Step (2), filtering the collagen colloid dispersion through a filter screen and performing a centrifugal degassing treatment to obtain a collagen spinning solution; Step (3), extruding the collagen spinning solution into a coagulation bath through a wet spinning device, and obtaining collagen multifilament fibers through drawing, washing, stretching and drying; The coagulation bath length is 0.5 m ~ 3 m, and the coagulation bath temperature is 15℃ ~ 45℃; The coagulation bath in step (3) is a three-stage coagulation bath, which includes a first stage coagulation bath, a second stage coagulation bath, and a third stage coagulation bath arranged in sequence; The first coagulation bath is an alkaline solution of PEG8000 with a mass concentration of 15% to 25% and a pH of 9 to 13; The second coagulation bath is an alkaline solution of PEG20000 with a mass concentration of 20% to 30% and a pH of 9 to 13; The third coagulation bath is an inorganic salt solution with a mass concentration of 20% to 60%.
2. The method for preparing collagen multifilament fiber according to claim 1, characterized in that: The water-soluble cross-linking agent in step (1) is glutaraldehyde, genipin or EDC / NHS, with a concentration of 0.01% to 1%.
3. The method for preparing collagen multifilament fiber according to claim 1, wherein: The concentration of the collagen colloid in the collagen colloid dispersion in step (1) is 10 mg / ml to 50 mg / ml.
4. The method for preparing collagen multifilament fiber according to claim 1, wherein: The mesh size of the filter in step (2) is 60-150 mesh.
5. The method for preparing collagen multifilament fiber according to claim 1, wherein: The wet spinning device in step (3) includes an air compressor, a charging kettle, a candle filter, a metering pump, a spinneret, a stretching device, a drying device and a winding device; The collagen spinning solution is placed in a charging kettle, filtered through a candle filter, extruded through a metering pump and a spinneret in sequence, and enters a coagulation bath to form primary collagen fibers. The primary collagen fibers are coagulated and formed in the coagulation bath, then enter a cleaning bath for cleaning and exit the bath. The fibers are stretched by a stretching device, dried by a drying device, and finally wound by a winding device to obtain collagen multifilament fibers.
6. The method for preparing collagen multifilament fiber according to claim 5, characterized in that: The air compressor provides a pressure of 0.1 MPa to 0.6 MPa for the charging kettle; The metering pump extrusion speed is 0.3 ml / min ~ 5 ml / min, and the spinneret stretch ratio is 0.5~1; The number of holes in the spinneret is ≥2, the hole diameter is 0.05 mm ~ 0.3 mm, and the aspect ratio is 20 ~ 200; The cleaning bath is an ethanol solution with a concentration of 30% to 70%; The exit speed is 0.2 m / min ~ 5 m / min; The stretching ratio of the stretching device is 1 to 5; The drying temperature of the drying device is 20℃ ~ 50℃; The winding speed of the winding device is 0.2 m / min ~ 10 m / min.
7. The method for preparing collagen multifilament fiber according to claim 1, characterized in that: The inorganic salt solution includes but is not limited to sodium chloride, sodium sulfate, sodium carbonate, sodium nitrate, potassium chloride, potassium sulfate, potassium carbonate, potassium nitrate, ammonium chloride, ammonium sulfate, ammonium carbonate, and ammonium nitrate.
8. A collagen multifilament fiber obtained by the preparation method according to any one of claims 1 to 7, characterized in that: The fiber fineness of the collagen multifilament fiber is 10 dtex to 200 dtex.
9. The use of the collagen multifilament fiber according to claim 8, characterized in that: The collagen multifilament fiber is used in the textile field and the medical field.
Citation Information
Patent Citations
Collagen long fibers with natural structure, preparation method and application thereof
CN111235662A
Preparation method of collagen fibers
CN108977912A
Preparation method for collagen fiber, collagen fiber, and use
EP4394098A1