Method for producing animal protein fiber and cashmere by using animal protein
By mixing cashmere protein with milk protein solution and adding specific components, the problem of poor mechanical properties of animal protein fibers is solved, significantly improving the breaking strength and elongation of the fibers, and broadening its application in textile products.
Patent Information
- Application Number
- CN202411683631.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-22
- Publication Date
- 2025-01-17
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The existing animal protein fibers produced by using animal proteins have poor mechanical properties, the fibers are prone to breaking strength and poor toughness, which limits their application in textile products.
Animal protein fibers are prepared by mixing cashmere protein with milk protein solution and adding initiators, crosslinking agents and modifiers. The specific steps include dissolution, filtration, mixing and spinning, using sodium hydroxide and acidic The pH value and temperature are controlled by alkaline aqueous solution, and components such as polyacrylamide, glutaraldehyde, dextran are added to improve the mechanical properties of the fiber.
It significantly improves the break strength and elongation of animal protein fibers, improves its mechanical properties, and makes it more suitable for use in textile products such as cashmere.
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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 animal protein fibers and cashmere by utilizing animal protein. Background Art
[0002] The main sources of protein in natural animal protein fibers include animal hair, silk, eggs, etc., which are the earliest fibers to be used and are now one of the raw materials for the textile industry. Although protein fibers have excellent performance, their annual output is very limited, and the recycling of protein resources has become a hot topic in research. Animal protein molecular chains are connected by hydrogen bonds and covalent bonds, and the highly ordered structure makes animal protein exhibit excellent performance. In addition, protein has the advantages of excellent biodegradability, high permeability and good biocompatibility.
[0003] However, the existing animal protein fibers produced using animal protein still have poor mechanical properties, the fibers are easy to break, have low strength, and have poor toughness. Therefore, it is necessary to obtain an animal protein fiber with excellent mechanical properties produced using animal protein to broaden the application of animal protein fibers in textile products such as cashmere. Summary of the invention
[0004] The present invention provides a method for producing animal protein fiber and cashmere by utilizing animal protein, which solves the problem of poor mechanical properties of animal protein fiber produced by utilizing animal protein in the related art.
[0005] The technical solution of the present invention is as follows: The present invention provides a method for producing animal protein fiber using animal protein, comprising the following steps: S1, dissolving cashmere protein to obtain a cashmere protein solution; S2, mixing the milk protein with the acidic aqueous solution for the first time, filtering the filter residue and mixing it with the alkaline aqueous solution for the second time to obtain a milk protein solution; S3. After mixing the cashmere protein solution and the milk protein solution for the third time, adding an initiator and a cross-linking agent and mixing for the fourth time to obtain a spinning solution, spinning, and obtaining animal protein fibers.
[0006] As a further technical solution, in step S1, the solvent during dissolution includes sodium hydroxide solution; The dissolving temperature is 70-80°C and the dissolving time is 90-100 minutes.
[0007] As a further technical solution, in step S2, the pH value of the acidic aqueous solution is 4-4.5, and the pH value of the alkaline aqueous solution is 9-9.5; The temperature during the first mixing is 30-40°C and the time is 40-60 minutes; The temperature of the second mixing is 45-50°C and the time is 60-70 minutes; The time for the third mixing is 120 to 160 minutes; The fourth mixing time is 50 to 90 minutes.
[0008] As a further technical solution, the mass ratio of the milk protein to the acidic aqueous solution is 1:8-12; During the first mixing, an impurity-removing and anti-coagulant is also added, and the mass ratio of the milk protein to the impurity-removing and anti-coagulant is 100:0.5-0.8; The impurity-removing anticoagulant comprises the following components in parts by weight: 1-2 parts of polyacrylamide and 1-1.5 parts of diethylene glycol monomethyl ether.
[0009] As a further technical solution, the mass ratio of the cashmere protein solution to the milk protein solution is 6:1-3.
[0010] As a further technical solution, the components of the cross-linking agent include one or more of glutaraldehyde, dextran, and glyoxal; the initiator includes ammonium persulfate; the mass of the cross-linking agent is 1% to 1.5% of the mass of the cashmere protein; the mass of the initiator is 0.01% to 0.03% of the mass of the cashmere protein; A modifier is also added during the fourth mixing, and the mass of the modifier is 1% to 2% of the mass of the cashmere protein; The modifier comprises hydroxypropyl chitosan and ethylene-vinyl alcohol copolymer in a mass ratio of 5:1-3.
[0011] In the present invention, hydroxypropyl chitosan and ethylene-vinyl alcohol copolymer are added as modifiers to a mixture of a cashmere protein solution and a milk protein solution to synergistically prepare animal protein fibers, thereby further improving the mechanical properties of the animal protein fibers.
[0012] As a further technical solution, the melt index of the ethylene-vinyl alcohol copolymer at 210° C. and 2.16 kg is 3.2-4.0 g / 10 min.
[0013] As a further technical solution, the modifier includes hydroxypropyl chitosan, ethylene-vinyl alcohol copolymer, and N-tert-octylacrylamide in a mass ratio of 5:3:1-3.
[0014] In the present invention, the modifiers of 5:3:1-3 hydroxypropyl chitosan, ethylene-vinyl alcohol copolymer and N-tert-octylacrylamide are added to a mixture of cashmere protein solution and milk protein solution to prepare animal protein fiber, thereby further improving the mechanical properties of the animal protein fiber.
[0015] As a further technical solution, the diameter of the animal protein fiber is 15~20μm.
[0016] The present invention also provides a method for producing cashmere by utilizing animal protein, wherein the cashmere is prepared by using the animal protein fiber as the raw material of the cashmere.
[0017] The working principle and beneficial effects of the present invention are: In the present invention, animal protein is used to produce animal protein fiber, and a blend of cashmere protein and milk protein is spun to prepare the animal protein fiber, thereby significantly improving the mechanical properties of the animal protein fiber. DETAILED DESCRIPTION
[0018] 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.
[0019] In the following examples and comparative examples, the weight average molecular weight of polyacrylamide is 6 million.
[0020] Example 1 The method for producing animal protein fiber using animal protein comprises the following steps: S1, mixing cashmere protein and sodium hydroxide solution at 70° C. for 100 minutes to obtain a cashmere protein solution; S2, at 30 ° C, milk protein, impurity removal anticoagulant, pH 4 hydrochloric acid aqueous solution are mixed for 60 min, the filter residue is filtered and mixed with a sodium hydroxide solution with a pH value of 9 at 50 ° C for 60 min to obtain a milk protein solution; wherein the mass ratio of milk protein to hydrochloric acid aqueous solution is 1:8, the mass ratio of milk protein to impurity removal anticoagulant is 100:0.5, and the impurity removal anticoagulant comprises the following components in parts by weight: 1 part of polyacrylamide and 1 part of diethylene glycol monomethyl ether; S3. After mixing the cashmere protein solution and the milk protein solution at a mass ratio of 6:1 for 120 minutes, add ammonium persulfate and glyoxal and mix for 50 minutes to obtain a spinning solution, and spin to obtain animal protein fibers with a diameter of 15 μm; the mass of glyoxal is 1% of the mass of cashmere protein; the mass of ammonium persulfate is 0.01% of the mass of cashmere protein.
[0021] Example 2 The method for producing animal protein fiber using animal protein comprises the following steps: S1, mixing cashmere protein and sodium hydroxide solution at 80° C. for 90 minutes to obtain a cashmere protein solution; S2, at 40 ° C, milk protein, impurity removal anticoagulant, pH 4.5 hydrochloric acid aqueous solution was mixed for 40 min, the filter residue was filtered and mixed with a sodium hydroxide solution with a pH of 9.5 at 45 ° C for 70 min to obtain a milk protein solution; wherein the mass ratio of milk protein to hydrochloric acid aqueous solution is 1:12, the mass ratio of milk protein to impurity removal anticoagulant is 100:0.8, and the impurity removal anticoagulant includes the following components in parts by weight: 2 parts of polyacrylamide and 1.5 parts of diethylene glycol monomethyl ether; S3. After mixing the cashmere protein solution and the milk protein solution at a mass ratio of 6:3 for 160 minutes, ammonium persulfate and glyoxal are added and mixed for 90 minutes to obtain a spinning solution, and spinning is performed to obtain animal protein fibers with a diameter of 20 μm; the mass of glyoxal is 1% of the mass of the cashmere protein; the mass of ammonium persulfate is 0.02% of the mass of the cashmere protein.
[0022] Example 3 The method for producing animal protein fiber using animal protein comprises the following steps: S1, mixing cashmere protein and sodium hydroxide solution at 75° C. for 100 minutes to obtain a cashmere protein solution; S2, at 40 ° C, milk protein, impurity removal anticoagulant, pH 4 hydrochloric acid aqueous solution are mixed for 60 min, the filter residue is filtered and mixed with a sodium hydroxide solution with a pH value of 9.5 at 50 ° C for 70 min to obtain a milk protein solution; wherein the mass ratio of milk protein to hydrochloric acid aqueous solution is 1:10, the mass ratio of milk protein to impurity removal anticoagulant is 100:0.6, and the impurity removal anticoagulant comprises the following components in parts by weight: 2 parts of polyacrylamide and 1.5 parts of diethylene glycol monomethyl ether; S3. After mixing the cashmere protein solution and the milk protein solution at a mass ratio of 3:1 for 120 minutes, add ammonium persulfate and glyoxal and mix for 60 minutes to obtain a spinning solution, and spin to obtain animal protein fibers with a diameter of 15 μm; the mass of glyoxal is 1% of the mass of cashmere protein; the mass of ammonium persulfate is 0.03% of the mass of cashmere protein.
[0023] Example 4 The difference between this embodiment and embodiment 3 is that step S3 of the method for producing animal protein fibers using animal protein is: after mixing the cashmere protein solution and the milk protein solution at a mass ratio of 3:1, adding a modifier, ammonium persulfate, and glyoxal to mix, to obtain a spinning solution, spinning, and obtaining animal protein fibers with a diameter of 15 μm; The mass of the modifier is 1.5% of the mass of the cashmere protein, and the modifier is hydroxypropyl chitosan.
[0024] Example 5 The only difference between this embodiment and embodiment 4 is that the modifier is ethylene-vinyl alcohol copolymer, and the melt index of ethylene-vinyl alcohol copolymer at 210° C. and 2.16 kg is 3.2 g / 10 min.
[0025] Example 6 The only difference between this embodiment and embodiment 4 is that the modifier is N-tert-octyl acrylamide.
[0026] Example 7 The only difference between this embodiment and embodiment 4 is that the modifier is hydroxypropyl chitosan and ethylene-vinyl alcohol copolymer in a mass ratio of 5:1, and the melt index of the ethylene-vinyl alcohol copolymer at 210° C. and 2.16 kg is 3.2 g / 10 min.
[0027] Example 8 The only difference between this embodiment and embodiment 4 is that the modifier is hydroxypropyl chitosan and ethylene-vinyl alcohol copolymer in a mass ratio of 5:3, and the melt index of the ethylene-vinyl alcohol copolymer at 210° C. and 2.16 kg is 3.2 g / 10 min.
[0028] Example 9 The only difference between this embodiment and embodiment 8 is that the modifier is hydroxypropyl chitosan, ethylene-vinyl alcohol copolymer, and N-tert-octylacrylamide in a mass ratio of 5:3:1.
[0029] Example 10 The only difference between this embodiment and embodiment 8 is that the modifier is hydroxypropyl chitosan, ethylene-vinyl alcohol copolymer, and N-tert-octylacrylamide in a mass ratio of 5:3:3.
[0030] Embodiment 11 The difference between this embodiment and embodiment 10 is that the modifier is hydroxypropyl chitosan, ethylene-vinyl alcohol copolymer, and N-tert-octylacrylamide in a mass ratio of 5:3:3; The melt index of the ethylene-vinyl alcohol copolymer at 210° C. and 2.16 kg was 4.0 g / 10 min.
[0031] Comparative Example 1 The method for producing animal protein fiber using animal protein comprises the following steps: S1, mixing cashmere protein and sodium hydroxide solution at 75° C. for 100 minutes to obtain a cashmere protein solution; S2. Mix the cashmere protein solution, ammonium persulfate and glyoxal for 180 minutes to obtain a spinning solution, and spin to obtain animal protein fibers with a diameter of 15 μm; the mass of glyoxal is 1% of the mass of the cashmere protein; the mass of ammonium persulfate is 0.03% of the mass of the cashmere protein.
[0032] The mechanical properties of the animal protein fibers prepared in Examples 1 to 11 and Comparative Example 1 were tested respectively: the breaking strength (dry breaking strength) and breaking elongation were tested according to the standard GB / T 14337-2022 "Test method for tensile properties of chemical staple fibers"; The results are shown in Table 1 below.
[0033] Table 1 Mechanical properties test results
[0034] Compared with Comparative Example 1, the breaking strength and breaking elongation of the animal protein fibers prepared in Examples 1 to 11 are higher, indicating that the mechanical properties of the animal protein fibers are significantly improved by using animal protein to produce animal protein fibers and spinning a blend of cashmere protein and milk protein to prepare animal protein fibers.
[0035] Compared with Examples 3 to 5, the breaking strength and breaking elongation of the animal protein fibers prepared in Examples 7 to 8 are higher, indicating that the addition of hydroxypropyl chitosan and ethylene-vinyl alcohol copolymer as modifiers to the mixture of cashmere protein solution and milk protein solution to synergistically prepare animal protein fibers further improves the mechanical properties of the animal protein fibers.
[0036] Compared with Examples 7 to 8, the animal protein fibers prepared in Examples 9 to 11 have higher breaking strength and breaking elongation, indicating that the mechanical properties of the animal protein fibers are further improved by adding a modifier of 5:3:1 to 3 of hydroxypropyl chitosan, ethylene-vinyl alcohol copolymer, and N-tert-octylacrylamide to a mixture of cashmere protein solution and milk protein solution to prepare the animal protein fibers.
[0037] 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 animal protein fiber using animal protein, characterized in that: The following steps are involved: S1, dissolving cashmere protein to obtain a cashmere protein solution; S2, mixing the milk protein with the acidic aqueous solution for the first time, filtering the filter residue and mixing it with the alkaline aqueous solution for the second time to obtain a milk protein solution; S3. After mixing the cashmere protein solution and the milk protein solution for the third time, adding an initiator and a cross-linking agent and mixing for the fourth time to obtain a spinning solution, spinning, and obtaining animal protein fibers.
2. The method for producing animal protein fiber using animal protein according to claim 1, characterized in that: In step S1, the solvent used for dissolving includes sodium hydroxide solution; The dissolving temperature is 70-80°C and the dissolving time is 90-100 minutes.
3. The method for producing animal protein fiber using animal protein according to claim 1, characterized in that: In step S2, the pH value of the acidic aqueous solution is 4-4.5, and the pH value of the alkaline aqueous solution is 9-9.5; The temperature during the first mixing is 30-40°C and the time is 40-60 minutes; The temperature of the second mixing is 45-50°C and the time is 60-70 minutes; The time for the third mixing is 120 to 160 minutes; The fourth mixing time is 50 to 90 minutes.
4. The method for producing animal protein fiber using animal protein according to claim 1, characterized in that: The mass ratio of the milk protein to the acidic aqueous solution is 1:8-12; During the first mixing, an impurity-removing and anti-coagulant is also added, and the mass ratio of the milk protein to the impurity-removing and anti-coagulant is 100:0.5-0.8; The impurity-removing anticoagulant comprises the following components in parts by weight: 1-2 parts of polyacrylamide and 1-1.5 parts of diethylene glycol monomethyl ether.
5. The method for producing animal protein fiber using animal protein according to claim 1, characterized in that: The mass ratio of the cashmere protein solution to the milk protein solution is 6:1-3.
6. The method for producing animal protein fiber using animal protein according to claim 1, characterized in that: The components of the cross-linking agent include one or more of glutaraldehyde, dextran, and glyoxal; A modifier is also added during the fourth mixing, and the mass of the modifier is 1% to 2% of the mass of the cashmere protein; The modifier comprises hydroxypropyl chitosan and ethylene-vinyl alcohol copolymer in a mass ratio of 5:1-3.
7. The method for producing animal protein fiber using animal protein according to claim 6, characterized in that: The ethylene-vinyl alcohol copolymer has a melt index of 3.2-4.0 g / 10 min at 210° C. and 2.16 kg.
8. The method for producing animal protein fiber using animal protein according to claim 6, characterized in that: The modifier comprises hydroxypropyl chitosan, ethylene-vinyl alcohol copolymer and N-tert-octyl acrylamide in a mass ratio of 5:3:1-3.
9. The method for producing animal protein fiber using animal protein according to claim 1, characterized in that: The diameter of the animal protein fiber is 15-20 μm.
10. A method for producing cashmere using animal protein, characterized in that: Cashmere is prepared by using the animal protein fiber described in any one of claims 1 to 9 as the raw material of cashmere.