Method for producing milk protein fiber by using milk protein
By adding modified cerium oxide and the cross-linking agent glutaraldehyde to milk casein solution and combining it with chitosan, milk protein fiber was prepared using a spinning process. This solved the problem of insufficient mechanical properties and antibacterial properties of milk protein fiber, and achieved a significant improvement in both antibacterial and mechanical properties.
Patent Information
- Application Number
- CN202411636960.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-15
- Publication Date
- 2025-01-07
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
Existing milk protein fibers have shortcomings in terms of mechanical properties and antibacterial properties, which limits their application in high-end textiles.
Milk protein fibers were prepared by adding modified cerium oxide and the crosslinking agent glutaraldehyde to milk casein solution and combining it with chitin, using a spinning process. The modified cerium oxide was coated with polyvinylpyrrolidone to optimize its structure.
It significantly improves the antibacterial and mechanical properties of milk protein fiber, broadening its application scope in the textile industry.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of protein fibers, and in particular to a method for producing milk protein fibers by utilizing milk protein. Background Art
[0002] As a new type of green and environmentally friendly fiber material, milk protein fiber has received widespread attention in the textile field for its soft feel, good moisture absorption and biocompatibility.
[0003] At present, the improvement of milk protein fiber mainly improves its mechanical properties and antibacterial properties by optimizing protein molecular structure, improving spinning process, adding antibacterial agents and surface modification. However, the existing milk protein fiber still has certain deficiencies in mechanical properties and antibacterial properties, which limits its application in high-end textiles.
[0004] Therefore, it is necessary to conduct in-depth research on the performance defects of milk protein fiber and propose effective improvement methods to improve the mechanical properties and antibacterial properties of milk protein fiber and broaden the application of milk protein fiber in the textile industry. Summary of the invention
[0005] The present invention provides a method for producing milk protein fiber by utilizing milk protein, which solves the problem of poor antibacterial and mechanical properties of milk protein fiber in the related art.
[0006] The technical solution of the present invention is as follows: The present invention provides a method for producing milk protein fiber by utilizing milk protein, comprising the following steps: S1, mixing milk casein and water to obtain a milk casein solution; S2, mixing the milk casein solution, modified cerium oxide and a cross-linking agent, and spinning to obtain milk protein fibers; The preparation method of the modified cerium oxide comprises the following steps: A1, polyacrylonitrile is dissolved and mixed with cerium oxide, and dried to obtain polyacrylonitrile modified cerium oxide; A2. Mixing the polyacrylonitrile modified cerium oxide and alkali solution, adding chitosan and continuing to mix, and drying to obtain modified cerium oxide.
[0007] As a further technical solution, the mass ratio of milk casein to water is 1~5:10.
[0008] As a further technical solution, the alkali solution is an aqueous sodium hydroxide solution with a concentration of 1 to 1.2 mol / L.
[0009] As a further technical solution, the mass ratio of polyacrylonitrile to cerium oxide is 0.1-0.3:2.
[0010] As a further technical solution, the mass ratio of the cerium oxide to the chitin is 6:1-3.
[0011] In the present invention, chitosan is combined with cerium oxide, and when the mass ratio of cerium oxide to chitosan is 6:1-3, the antibacterial property and mechanical property of milk protein fiber are further improved.
[0012] As a further technical solution, the particle size of the cerium oxide is 1-2 μm.
[0013] As a further technical solution, the modified cerium oxide is polyvinyl pyrrolidone-coated modified cerium oxide.
[0014] As a further technical solution, the method for preparing the polyvinyl pyrrolidone-coated modified cerium oxide comprises the following steps: dissolving polyvinyl pyrrolidone, mixing the mixture with the modified cerium oxide, and drying the mixture to obtain the polyvinyl pyrrolidone-coated modified cerium oxide.
[0015] In the present invention, polyvinyl pyrrolidone is used to coat the modified cerium oxide, thereby further improving the antibacterial property and mechanical properties of the milk protein fiber.
[0016] As a further technical solution, the mass ratio of polyvinyl pyrrolidone to chitosan is 2-5:3.
[0017] In the present invention, when the mass ratio of polyvinyl pyrrolidone to chitin is 2-5:3, the antibacterial property and mechanical properties of the milk protein fiber are further improved.
[0018] As a further technical solution, the mass ratio of the cross-linking agent to milk casein is 1~3:100.
[0019] As a further technical solution, the cross-linking agent includes one or both of dialdehyde compounds and isocyanate.
[0020] The working principle and beneficial effects of the present invention are: In the present invention, milk protein is used to produce milk protein fiber, modified cerium oxide is added to a milk casein solution to prepare the milk protein fiber, and chitosan is combined with cerium oxide to synergistically enhance the antibacterial and mechanical properties of the milk protein fiber. DETAILED DESCRIPTION
[0021] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0022] In the following examples and comparative examples, the weight average molecular weight of polyacrylonitrile is 90,000; the model of polyvinyl pyrrolidone is PVPK100.
[0023] Example 1 The method for producing milk protein fiber by utilizing milk protein comprises the following steps: S1, mixing milk casein and water in a mass ratio of 1:10 to obtain a milk casein solution; S2, mixing the milk casein solution, modified cerium oxide and glutaraldehyde, and spinning to obtain milk protein fibers; Among them, the mass ratio of glutaraldehyde to milk casein was 1:100; The preparation method of modified cerium oxide comprises the following steps: A1, polyacrylonitrile is dissolved and mixed with cerium oxide with a particle size of 1 μm, and dried to obtain polyacrylonitrile modified cerium oxide; the mass ratio of polyacrylonitrile to cerium oxide is 0.1:2; A2. Polyacrylonitrile-modified cerium oxide and 1 mol / L sodium hydroxide aqueous solution are mixed at a mass ratio of 1:10, chitin is added and continued to be mixed, and dried to obtain modified cerium oxide; the mass ratio of cerium oxide to chitin is 3:2.
[0024] Example 2 The method for producing milk protein fiber by utilizing milk protein comprises the following steps: S1, mixing milk casein and water in a mass ratio of 5:10 to obtain a milk casein solution; S2, mixing the milk casein solution, modified cerium oxide and glutaraldehyde, and spinning to obtain milk protein fibers; Among them, the mass ratio of glutaraldehyde to milk casein was 3:100; The preparation method of modified cerium oxide comprises the following steps: A1, polyacrylonitrile is dissolved and mixed with cerium oxide with a particle size of 2 μm, and dried to obtain polyacrylonitrile modified cerium oxide; the mass ratio of polyacrylonitrile to cerium oxide is 0.3:2; A2. Polyacrylonitrile-modified cerium oxide and 1.2 mol / L sodium hydroxide aqueous solution were mixed at a mass ratio of 1:10, chitin was added and continued to mix, and dried to obtain modified cerium oxide; the mass ratio of cerium oxide to chitin was 3:2.
[0025] Example 3 The method for producing milk protein fiber by utilizing milk protein comprises the following steps: S1, mixing milk casein and water in a mass ratio of 3:10 to obtain a milk casein solution; S2, mixing the milk casein solution, modified cerium oxide and glutaraldehyde, and spinning to obtain milk protein fibers; Among them, the mass ratio of glutaraldehyde to milk casein was 2:100; The preparation method of modified cerium oxide comprises the following steps: A1, polyacrylonitrile is dissolved and mixed with cerium oxide with a particle size of 1 μm, and dried to obtain polyacrylonitrile modified cerium oxide; the mass ratio of polyacrylonitrile to cerium oxide is 0.2:2; A2. Polyacrylonitrile-modified cerium oxide and 1.2 mol / L sodium hydroxide aqueous solution were mixed at a mass ratio of 1:10, chitin was added and continued to mix, and dried to obtain modified cerium oxide; the mass ratio of cerium oxide to chitin was 3:2.
[0026] Example 4 The only difference between this embodiment and embodiment 3 is that the mass ratio of cerium oxide to chitin is 6:0.5.
[0027] Example 5 The only difference between this embodiment and embodiment 3 is that the mass ratio of cerium oxide to chitin is 6:1.
[0028] Example 6 The only difference between this embodiment and embodiment 3 is that the mass ratio of cerium oxide to chitin is 2:1.
[0029] Example 7 The only difference between this embodiment and embodiment 6 is that the preparation method of modified cerium oxide comprises the following steps: A1, polyacrylonitrile is dissolved and mixed with cerium oxide with a particle size of 1 μm, and dried to obtain polyacrylonitrile modified cerium oxide; the mass ratio of polyacrylonitrile to cerium oxide is 0.2:2; A2, polyacrylonitrile modified cerium oxide and 1.2 mol / L sodium hydroxide aqueous solution were mixed at a mass ratio of 1:10, chitin was added and continued to mix, and dried to obtain modified cerium oxide; the mass ratio of cerium oxide to chitin was 2:1; A3. Dissolve polyvinyl pyrrolidone in 70% by volume ethanol, mix with modified cerium oxide, and dry to obtain polyvinyl pyrrolidone-coated modified cerium oxide; the mass ratio of polyvinyl pyrrolidone to chitin is 2:1; the mass ratio of polyvinyl pyrrolidone to ethanol is 1:30.
[0030] Example 8 The only difference between this embodiment and embodiment 6 is that the mass ratio of polyvinyl pyrrolidone to chitin is 1:3.
[0031] Example 9 The only difference between this embodiment and embodiment 6 is that the mass ratio of polyvinyl pyrrolidone to chitin is 5:3.
[0032] Example 10 The only difference between this embodiment and embodiment 6 is that the mass ratio of polyvinyl pyrrolidone to chitin is 2:3.
[0033] Embodiment 11 The difference between this embodiment and embodiment 6 is only that the method for producing milk protein fiber using milk protein comprises the following steps: S1, mixing milk casein and water in a mass ratio of 3:10 to obtain a milk casein solution; S2. Mix the milk casein solution with modified cerium oxide, polyvinyl pyrrolidone and glutaraldehyde, and spin them to obtain milk protein fibers; the mass ratio of polyvinyl pyrrolidone to chitin is 2:3.
[0034] Comparative Example 1 The difference between this comparative example and Example 3 is that the modified cerium oxide is replaced by cerium oxide and chitin; The method for producing milk protein fiber by utilizing milk protein comprises the following steps: S1, mixing milk casein and water in a mass ratio of 3:10 to obtain a milk casein solution; S2. Mix the milk casein solution with cerium oxide, chitin and glutaraldehyde, and spin them to obtain milk protein fibers; the mass ratio of cerium oxide to chitin is 3:2.
[0035] Comparative Example 2 The difference between this comparative example and Example 3 is that the modified cerium oxide is replaced by chitosan.
[0036] Comparative Example 3 The difference between this comparative example and Example 3 is only that the modified cerium oxide is replaced by cerium oxide.
[0037] The antibacterial and mechanical properties of the milk protein fibers prepared in Examples 1 to 11 and Comparative Examples 1 to 3 were tested respectively: Antibacterial property: According to the standard FZ / T 73023-2006 "Antibacterial knitwear", the milk protein fiber was made into antibacterial fabric, and the antibacterial rate against Staphylococcus aureus and the antibacterial rate after 100 washes were measured; Mechanical properties: Breaking strength (dry breaking strength) test is carried out in accordance with standard GB / T 14337-2022 "Test method for tensile properties of chemical staple fibers"; The results are shown in Table 1 below.
[0038] Table 1 Test results of milk protein fiber performance
[0039] Compared with Comparative Examples 1 to 3, the antibacterial rate of the milk protein fibers prepared in Examples 1 to 11 and the antibacterial rate after washing 100 times are higher, and the breaking strength is stronger, indicating that adding modified cerium oxide to the milk casein solution to prepare milk protein fibers and combining chitosan with cerium oxide significantly improves the antibacterial and mechanical properties of the milk protein fibers.
[0040] Compared with Examples 3 to 4, the antibacterial rate of the milk protein fiber prepared in Examples 5 to 6 and the antibacterial rate after washing 100 times are both higher, and the breaking strength is stronger, indicating that when chitosan is combined with cerium oxide and the mass ratio of cerium oxide to chitosan is 6:1 to 3, the antibacterial and mechanical properties of the milk protein fiber are further improved.
[0041] Compared with Example 6, the antibacterial rate of the milk protein fibers prepared in Examples 7 to 10 and the antibacterial rate after washing 100 times are higher, and the breaking strength is stronger, indicating that the use of polyvinyl pyrrolidone-coated modified cerium oxide further improves the antibacterial and mechanical properties of the milk protein fibers.
[0042] Compared with Examples 7 to 8, the antibacterial rate of the milk protein fiber prepared in Examples 9 to 10 and the antibacterial rate after washing 100 times are higher, and the breaking strength is stronger, indicating that when the mass ratio of polyvinyl pyrrolidone to chitin is 2 to 5:3, the antibacterial and mechanical properties of the milk protein fiber are further improved.
[0043] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.
Claims
1. A method for producing milk protein fiber using milk protein, characterized in that: The following steps are involved: S1, mixing milk casein and water to obtain a milk casein solution; S2, mixing the milk casein solution, modified cerium oxide and a cross-linking agent, and spinning to obtain milk protein fibers; The preparation method of the modified cerium oxide comprises the following steps: A1, polyacrylonitrile is dissolved and mixed with cerium oxide, and dried to obtain polyacrylonitrile modified cerium oxide; A2. Mixing the polyacrylonitrile modified cerium oxide and alkali solution, adding chitosan and continuing to mix, and drying to obtain modified cerium oxide.
2. The method for producing milk protein fiber using milk protein according to claim 1, characterized in that: The mass ratio of the milk casein to water is 1-5:
10.
3. The method for producing milk protein fiber using milk protein according to claim 1, characterized in that: The mass ratio of the polyacrylonitrile to cerium oxide is 0.1-0.3:
2.
4. The method for producing milk protein fiber using milk protein according to claim 1, characterized in that: The mass ratio of the cerium oxide to the chitin is 6:1-3.
5. The method for producing milk protein fiber using milk protein according to claim 1, characterized in that: The particle size of the cerium oxide is 1-2 μm.
6. The method for producing milk protein fiber using milk protein according to claim 1, characterized in that: The modified cerium oxide is polyvinyl pyrrolidone-coated modified cerium oxide.
7. The method for producing milk protein fiber using milk protein according to claim 6, characterized in that: The method for preparing the polyvinyl pyrrolidone-coated modified cerium oxide comprises the following steps: dissolving polyvinyl pyrrolidone, mixing the mixture with the modified cerium oxide, and drying the mixture to obtain the polyvinyl pyrrolidone-coated modified cerium oxide.
8. The method for producing milk protein fiber using milk protein according to claim 7, characterized in that: The mass ratio of the polyvinyl pyrrolidone to chitin is 2-5:
20.
9. The method for producing milk protein fiber using milk protein according to claim 1, characterized in that: The mass ratio of the cross-linking agent to milk casein is 1-3:
100.
10. The method for producing milk protein fiber using milk protein according to claim 1, characterized in that: The cross-linking agent includes one or both of dialdehyde compounds and isocyanate.