Extraction process of keratin in wool and wool keratin
By using the synergistic effect of ammonium thiosulfate, 1,4-dithiothreitol and fluoro-containing silicone surfactant in wool, the extraction rate of wool keratin is improved, and the problem of low extraction rate in the prior art is solved, and efficient extraction and stability of wool keratin is achieved.
Patent Information
- Application Number
- CN202510222837.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-27
- Publication Date
- 2025-05-30
AI Technical Summary
In the prior art, the extraction rate of wool keratin is relatively low, about 80%, which is difficult to meet market demand.
A keratin extraction process in wool is adopted, including washing, degreasing, crushing, immersion in the dissolution treatment solution under the protection of inert gas, using ammonium thiosulfate and 1,4-dithiothreitol to destroy the disulfide bond in wool, and improving permeability and dispersion uniformity through fluorinated silicone surfactant, thereby improving the extraction rate of wool keratin.
Through this process, the extraction rate of wool keratin is increased to >84%, meeting market demand, and has high stability and popularization.
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Abstract
Description
Technical Field
[0001] This application relates to the technical field of wool keratin extraction. More specifically, it relates to a process for extracting keratin from wool and wool keratin. Background Art
[0002] Wool is one of the important natural protein fibers, and its main component is wool keratin. As a biopolymer material, wool keratin has good biocompatibility, degradability and other properties, and has broad application prospects in many fields such as medicine, cosmetics, and textiles. In recent years, with the progress of technology and the growth of market demand, efficiently extracting wool keratin from wool has become a research hotspot and is of great significance for promoting the development of related industries. For the methods of extracting wool keratin from wool, the industry usually adopts various means such as mechanical method, acid-base method, oxidation method, reduction method, enzymatic hydrolysis method, etc. In the prior art, the patent application with the publication number CN115215932A discloses a preparation process for effectively dissolving wool and extracting wool keratin. First, the wool is degreased and cut into pieces, then swollen with lithium bromide, and then dissolved with a reducing agent to obtain a wool keratin solution, which is purified to obtain wool keratin. However, using the above method, the extraction rate of wool keratin is about 80%, and the extraction rate of wool keratin is slightly poor and needs to be further improved. Summary of the Invention
[0003] In order to improve the extraction rate of wool keratin, this application provides a process for extracting keratin from wool and wool keratin.
[0004] In the first aspect, this application provides a process for extracting keratin from wool, adopting the following technical scheme: The process for extracting keratin from wool includes the following steps: S1. Wash, degrease, dry, and pulverize the wool to obtain wool powder; S2. Under the protection of an inert gas, immerse the wool powder in a dissolution treatment liquid, heat it to 60 - 70°C, keep it warm for 1 - 3 h, then heat it to 80 - 100°C, keep it warm for 4 - 6 h, cool it to room temperature, and perform centrifugal separation to obtain a wool keratin solution; S3. Dialyze the wool keratin solution, freeze-dry it, pulverize it, and sieve it to obtain wool keratin; Wherein, the dissolution treatment liquid is mainly made of the following raw materials in parts by weight: 100 parts of water, 4 - 6 parts of sodium thiosulfate, 9 - 11 parts of 1,4-dithiothreitol, 2 - 4 parts of alkylphenol polyoxyethylene ether, 1 - 3 parts of fluorosilicon surfactant, 0.1 - 0.3 parts of sodium dodecylsulfonate, and 0.1 - 0.3 parts of dipropylene glycol methyl ether.
[0005] The extraction process of keratin in wool of the present application, through the mutual cooperation among various steps, enables the extraction rate of wool keratin to be > 84%, has the advantage of high extraction rate, meets the market demand, and can be widely promoted and applied on a large scale.
[0006] For the dissolution treatment liquid of the present application, ammonium thiosulfate and 1,4-dithiothreitol are added to the raw material, and the synergistic effect between the two is utilized to break the disulfide bonds in wool, causing the protein to break and promoting the dissolution of wool keratin. Further, a fluorosilicon surfactant is added. The fluorosilicon surfactant contains a fluorine group, a silicon group, an ester group, an amide group, and a tertiary amine group, effectively improving the permeability and dispersion uniformity, enhancing the interaction between ammonium thiosulfate and 1,4-dithiothreitol, and increasing the extraction rate of wool keratin.
[0007] Optionally, the weight ratio of the wool powder to the dissolution treatment liquid is 1:(5 - 30).
[0008] By adopting the above technical solution, the weight ratio of the wool powder to the dissolution treatment liquid is optimized, facilitating the full contact between the wool powder and the dissolution treatment liquid, and contributing to the dissolution of wool keratin. In multiple embodiments, the weight ratio of the wool powder to the dissolution treatment liquid is 1:20. It can also set the weight ratio to 1:5, 1:7, 1:10, 1:13, 1:15, 1:17, 1:23, 1:25, 1:27, 1:30 according to needs, but is not limited to the listed values. Other unlisted values within this numerical range are equally applicable.
[0009] Optionally, the fluorosilicon surfactant is prepared by the following method: At a temperature of 60 - 70 °C, ethanol and ethyl acrylate are mixed, the first portion of propylenediamine is added dropwise. After the addition is complete, stirring is carried out for 18 - 22 h. Then the second portion of propylenediamine is added dropwise. After the addition is complete, stirring is carried out for 13 - 17 h. 2,2,2-trifluoroethyl acrylate and 3-allyloxypropyltrimethoxysilane are respectively added dropwise. After the addition is complete, stirring is carried out for 18 - 22 h, and then vacuum distillation is carried out to obtain the fluorosilicon surfactant.
[0010] Optionally, the weight ratio of ethyl acrylate, the first portion of propylenediamine, the second portion of propylenediamine, 2,2,2-trifluoroethyl acrylate, and 3-allyloxypropyltrimethoxysilane is 10:(1.5 - 2.5):(7 - 8):(35 - 45):(20 - 30).
[0011] By adopting the above technical solution, first, an addition reaction occurs between the carbon-carbon double bond in ethyl acrylate and the two amino groups in the first portion of propanediamine to obtain intermediate A, increasing the number of branched chains and introducing an ester group. Then, an amidation reaction occurs between the ester group in intermediate A and one amino group in the second portion of propanediamine to obtain intermediate B, extending the length of the branched chain and introducing an amino group. After that, an addition reaction occurs between the amino group in intermediate B and the carbon-carbon double bonds in 2,2,2-trifluoroethyl acrylate and 3-allyloxypropyltrimethoxysilane to obtain a fluorosilane surfactant, further increasing the number of branched chains and introducing an ester group, a fluorine group, and a silicon group. By alternately performing the addition reaction and the amidation reaction, it is convenient to control the reaction, reduce side reactions, effectively regulate the molecular structure, and ensure the stability and use effect of the preparation of the fluorosilane surfactant.
[0012] Optionally, the weight ratio of ethyl acrylate to ethanol is 1:(30 - 70). In multiple embodiments, the weight ratio of ethyl acrylate to ethanol is 1:50, and it can also set the weight ratio to 1:30, 1:35, 1:40, 1:45, 1:55, 1:60, 1:65, 1:70 according to needs, but it is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.
[0013] Optionally, the dropping time of the first portion of propanediamine is 50 - 70 min, the dropping time of the second portion of propanediamine is 50 - 70 min, the dropping time of 2,2,2-trifluoroethyl acrylate is 50 - 70 min, and the dropping time of 3-allyloxypropyltrimethoxysilane is 50 - 70 min.
[0014] By adopting the above technical solution, the dropping times of the first portion of propanediamine, the second portion of propanediamine, 2,2,2-trifluoroethyl acrylate, and 3-allyloxypropyltrimethoxysilane are optimized, facilitating the full mixing and reaction of the materials, reducing side reactions, and ensuring the stability and use effect of the preparation of the fluorosilane surfactant.
[0015] In multiple embodiments, the dropping time of the first portion of propanediamine is 60 min, the dropping time of the second portion of propanediamine is 60 min, the dropping time of 2,2,2-trifluoroethyl acrylate is 60 min, and the dropping time of 3-allyloxypropyltrimethoxysilane is 60 min. According to needs, the dropping time of the first portion of propanediamine can be set to 50 min, 55 min, 65 min, or 70 min. According to needs, the dropping time of the second portion of propanediamine can also be set to 50 min, 55 min, 65 min, or 70 min. According to needs, the dropping time of 2,2,2-trifluoroethyl acrylate can also be set to 50 min, 55 min, 65 min, or 70 min. According to needs, the dropping time of 3-allyloxypropyltrimethoxysilane can also be set to 50 min, 55 min, 65 min, or 70 min. However, it is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.
[0016] In multiple embodiments, the stirring time after dropping the first portion of propanediamine is 20 h, the stirring time after dropping the second portion of propanediamine is 15 h, and the stirring time after dropping 2,2,2-trifluoroethyl acrylate and 3-allyloxypropyltrimethoxysilane is 20 h. According to needs, the stirring time after dropping the first portion of propanediamine can be set to 18 h, 18.5 h, 19 h, 19.5 h, 20.5 h, 21 h, 21.5 h, or 22 h. According to needs, the stirring time after dropping the second portion of propanediamine can also be set to 13 h, 13.5 h, 14 h, 14.5 h, 15.5 h, 16 h, 16.5 h, or 17 h. According to needs, the stirring time after dropping 2,2,2-trifluoroethyl acrylate and 3-allyloxypropyltrimethoxysilane can also be set to 18 h, 18.5 h, 19 h, 19.5 h, 20.5 h, 21 h, 21.5 h, or 22 h. However, it is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.
[0017] Optionally, the alkylphenol polyoxyethylene ether is one or more of alkylphenol polyoxyethylene ether OP-10, alkylphenol polyoxyethylene ether NP-10, and alkylphenol polyoxyethylene ether TX-10.
[0018] By adopting the above technical solution, the alkylphenol polyoxyethylene ether is optimized, which is convenient for the selection of the alkylphenol polyoxyethylene ether. Moreover, the alkylphenol polyoxyethylene ether can increase the uniformity of the dissolution treatment liquid and ensure the stability of the dissolution treatment liquid.
[0019] Optionally, the average particle size of the wool powder is 100 - 500 μm.
[0020] By adopting the above technical solution, the average particle size of the wool powder is optimized, which facilitates the dispersion of the wool powder in the dissolution treatment liquid, increases the contact area between the wool powder and the dissolution treatment liquid, improves the dissolution of wool keratin and the extraction rate of wool keratin, and ensures the stability of the extraction process. In multiple embodiments, the average particle size of the wool powder is 150 μm, and the average particle size can also be set to 100 μm, 130 μm, 180 μm, 200 μm, 230 μm, 250 μm, 280 μm, 300 μm, 330 μm, 350 μm, 380 μm, 400 μm, 430 μm, 450 μm, 480 μm, 500 μm as needed, but is not limited to the listed values, and other unlisted values within this value range are equally applicable.
[0021] Optionally, in step S1, during the degreasing treatment, sodium bicarbonate solution is used for degreasing, and the mass concentration of the sodium bicarbonate solution is 0.5 - 1.5%.
[0022] By adopting the above technical solution, the wool is degreased with sodium bicarbonate solution, effectively removing the grease impurities on the surface of the wool, facilitating the dissolution of wool keratin, and ensuring the quality of wool keratin. In multiple embodiments, the mass concentration of the sodium bicarbonate solution is 1%, and the mass concentration can also be set to 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5% as needed, but is not limited to the listed values, and other unlisted values within this value range are equally applicable.
[0023] Optionally, in step S1, during the degreasing treatment, the weight ratio of wool to sodium bicarbonate solution is 1:(10 - 30). In multiple embodiments, the weight ratio of wool to sodium bicarbonate solution is 1:20, and the weight ratio can also be set to 1:10, 1:13, 1:15, 1:18, 1:23, 1:25, 1:28, 1:30 as needed, but is not limited to the listed values, and other unlisted values within this value range are equally applicable.
[0024] Optionally, in step S3, during the dialysis treatment, the cut-off molecular weight for dialysis is 1000 - 5000 D, the dialysis time is 2 - 3 days, and during the dialysis process, deionized water is changed every 4 - 8 h.
[0025] By adopting the above technical solution, small molecule impurities can be effectively removed, the target wool keratin component can be retained, the dialysis environment can be kept stable, and the purity and quality of wool keratin can be ensured. In multiple embodiments, the cut-off molecular weight for dialysis is 3500D, the dialysis time is 3 days, and during the dialysis process, deionized water is changed every 8 hours. The cut-off molecular weight can be set to 1000D, 1500D, 2000D, 2500D, 3000D, 4000D, 4500D, 5000D as needed, the dialysis time can be set to 2 days, 2.5 days as needed, and the time for changing deionized water can also be set to 4 hours, 4.5 hours, 5 hours, 5.5 hours, 6 hours, 6.5 hours, 7 hours, 7.5 hours as needed, but it is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.
[0026] In a second aspect, the present application provides a wool keratin, adopting the following technical solution: The wool keratin is obtained by the method of the extraction process of keratin in the wool described above.
[0027] In summary, the present application has at least the following beneficial effects: In the extraction process of keratin in the wool of the present application, ammonium thiosulfate and 1,4-dithiothreitol are added to the raw materials of the dissolution treatment solution, and the synergistic effect between the two is utilized to break the disulfide bonds in the wool, causing the protein to break, and promoting the dissolution of wool keratin. A fluorosilicon surfactant is also added to the raw materials, effectively improving the permeability and dispersion uniformity, increasing the extraction rate of wool keratin, making the extraction rate of wool keratin > 84%, having the advantage of high extraction rate, and can be widely promoted and applied on a large scale. Specific embodiments
[0028] To make the present application easier to understand, the following will further illustrate the present application in detail with reference to embodiments. These embodiments are only illustrative and are not limited to the application scope of the present application. The raw materials or components used in the present application can be obtained through commercial channels or conventional methods without special instructions.
[0029] Preparation examples Preparation example 1 A fluorosilicon surfactant is prepared by the following method: At a stirring rate of 400 r / min and a temperature of 65 °C, 10 kg of ethyl acrylate was added to 500 kg of ethanol and stirred for 2 min. Then, 1.9 kg of the first portion of propanediamine was added dropwise over 60 min. After the addition was complete, stirring was continued for 20 h. Subsequently, 7.4 kg of the second portion of propanediamine was added dropwise over 60 min. After the addition was complete, stirring was continued for 15 h. Then, 40.7 kg of 2,2,2-trifluoroethyl acrylate and 23.4 kg of 3-allyloxypropyltrimethoxysilane were added dropwise, each over 60 min. After the addition was complete, stirring was continued for 20 h. Thereafter, ethanol was removed by vacuum distillation to obtain the fluorosilane surfactant.
[0030] Preparation Example 2 A fluorosilane surfactant, which is different from that in Preparation Example 1 in that the addition amounts of the first portion of ethylenediamine, the second portion of ethylenediamine, 2,2,2-trifluoroethyl acrylate, and 3-allyloxypropyltrimethoxysilane are different, and the addition amount of the first portion of ethylenediamine is 1.5 kg, the addition amount of the second portion of ethylenediamine is 8 kg, the addition amount of 2,2,2-trifluoroethyl acrylate is 35 kg, and the addition amount of 3-allyloxypropyltrimethoxysilane is 30 kg.
[0031] Preparation Example 3 A fluorosilane surfactant, which is different from that in Preparation Example 1 in that the addition amounts of the first portion of ethylenediamine, the second portion of ethylenediamine, 2,2,2-trifluoroethyl acrylate, and 3-allyloxypropyltrimethoxysilane are different, and the addition amount of the first portion of ethylenediamine is 2.5 kg, the addition amount of the second portion of ethylenediamine is 7 kg, the addition amount of 2,2,2-trifluoroethyl acrylate is 45 kg, and the addition amount of 3-allyloxypropyltrimethoxysilane is 20 kg. Example
[0032] Table 1 Dosages of raw materials for the dissolution treatment liquid (unit: kg) Example 1 A process for extracting keratin from wool, comprising the following steps: S0. Prepare a dissolution treatment liquid, and the raw materials and their ratios of the dissolution treatment liquid are shown in Table 1.
[0033] Among them, the alkylphenol polyoxyethylene ether is alkylphenol polyoxyethylene ether OP-10; the fluorosilane surfactant is prepared by the method of Preparation Example 1.
[0034] The dissolution treatment liquid is prepared by the following method: while the stirring rate is 400 r / min, add alkylphenol polyoxyethylene ether, fluorosilicon surfactant, sodium dodecyl sulfonate, and dipropylene glycol methyl ether into water, stir for 2 min, then add sodium thiosulfate and 1,4-dithiothreitol, and stir for 2 min to obtain the dissolution treatment liquid.
[0035] S1. Wash the wool, degrease it, dry it, and crush it to obtain wool powder, and the average particle size of the wool powder is 150 μm.
[0036] Among them, the wool is the wool of Han sheep, and the degreasing is carried out by the following method: immerse the washed wool in a sodium bicarbonate solution with a mass concentration of 1%, soak for 4 h, take it out, and wash with water to complete degreasing.
[0037] Moreover, the weight ratio of the wool to the sodium bicarbonate solution is 1:20.
[0038] S2. Under nitrogen protection, immerse the wool powder in the dissolution treatment liquid, heat up to 65 °C, keep warm for 2 h, then heat up to 90 °C, keep warm for 5 h, cool down to 25 °C, and perform centrifugal separation to obtain a wool keratin solution.
[0039] Among them, the weight ratio of the wool powder to the dissolution treatment liquid is 1:20.
[0040] S3. Dialyze the wool keratin solution, freeze-dry it, crush it, and pass it through a 100-mesh sieve to obtain wool keratin.
[0041] Among them, the dialysis is carried out by the following method: put the wool keratin solution into a dialysis bag with a cut-off molecular weight of 3500 D and dialyze it in deionized water for 3 days. During the dialysis process, change the deionized water every 8 h.
[0042] Example 2 A process for extracting keratin from wool, the difference from Example 1 is that in step S0, the raw material ratio of the dissolution treatment liquid is different, and the raw material ratio of the dissolution treatment liquid is shown in Table 1.
[0043] Example 3 A process for extracting keratin from wool, the difference from Example 1 is that in step S0, the raw material ratio of the dissolution treatment liquid is different, and the raw material ratio of the dissolution treatment liquid is shown in Table 1.
[0044] Example 4 A process for extracting keratin from wool, the difference from Example 1 is that in step S0, among the raw materials of the dissolution treatment liquid, the source of the fluorosilicon surfactant is different, and the fluorosilicon surfactant is prepared by the method of Preparation Example 2.
[0045] Example 5 An extraction process of keratin in wool, the difference from Example 1 is that in step S0, among the raw materials of the dissolution treatment liquid, the source of the fluorosilicone surfactant is different, and the fluorosilicone surfactant is obtained by the method of Preparation Example 3.
[0046] Comparative Example Comparative Example 1 An extraction process of keratin in wool, the difference from Example 1 is that in step S0, among the raw materials of the dissolution treatment liquid, an equal amount of sodium thiosulfate is used to replace 1,4-dithiothreitol.
[0047] Comparative Example 2 An extraction process of keratin in wool, the difference from Example 1 is that in step S0, among the raw materials of the dissolution treatment liquid, an equal amount of 1,4-dithiothreitol is used to replace sodium thiosulfate.
[0048] Comparative Example 3 An extraction process of keratin in wool, the difference from Example 1 is that in step S0, among the raw materials of the dissolution treatment liquid, an equal amount of fluorosurfactant FS-3100 is used to replace the fluorosilicone surfactant.
[0049] Comparative Example 4 An extraction process of keratin in wool, the difference from Example 1 is that in step S0, among the raw materials of the dissolution treatment liquid, an equal amount of 3-allyloxypropyltrimethoxysilane is used to replace the fluorosilicone surfactant.
[0050] Comparative Example 5 An extraction process of keratin in wool, the difference from Example 1 is that in step S0, in the preparation method of the fluorosilicone surfactant among the raw materials of the dissolution treatment liquid, an equal amount of 2,2,2-trifluoroethyl acrylate is used to replace 3-allyloxypropyltrimethoxysilane.
[0051] Comparative Example 6 An extraction process of keratin in wool, the difference from Example 1 is that in step S0, in the preparation method of the fluorosilicone surfactant among the raw materials of the dissolution treatment liquid, an equal amount of 3-allyloxypropyltrimethoxysilane is used to replace 2,2,2-trifluoroethyl acrylate.
[0052] Performance Detection Respectively take the wool keratin obtained in step S3 of Examples 1-5 and Comparative Examples 1-6, and detect the extraction rate of the wool keratin. The detection results are shown in Table 2.
[0053] Table 2 Detection Results As can be seen from Table 2, the extraction process of keratin in wool of the present application has a higher extraction rate of wool keratin. The extraction rate of wool keratin is 84.6 - 88.5%, showing the advantage of high extraction rate, meeting the market demand, and can be widely promoted and applied on a large scale.
[0054] Compare Comparative Examples 1 - 2 with Example 1. Sodium thiosulfate is added to the raw material of the dissolution treatment solution in the extraction process of Comparative Example 1; 1,4 - dithiothreitol is added to the raw material of the dissolution treatment solution in the extraction process of Comparative Example 2; sodium thiosulfate and 1,4 - dithiothreitol are added to the raw material of the dissolution treatment solution in the extraction process of Example 1. It can be seen from this that compared with using sodium thiosulfate alone or 1,4 - dithiothreitol alone, using sodium thiosulfate and 1,4 - dithiothreitol simultaneously and utilizing the synergistic effect between the two can improve the extraction rate of wool keratin.
[0055] Compare Comparative Examples 3 - 4 with Example 1. A fluorosurfactant FS - 3100 is added to the raw material of the dissolution treatment solution in the extraction process of Comparative Example 3; 3 - allyloxypropyltrimethoxysilane is added to the raw material of the dissolution treatment solution in the extraction process of Comparative Example 4; a fluorosilicone surfactant is added to the raw material of the dissolution treatment solution in the extraction process of Example 1. It can be seen from this that adding a fluorosilicone surfactant to the raw material of the dissolution treatment solution can also improve the extraction rate of wool keratin. This may be because the fluorosilicone surfactant can effectively enhance the permeability and dispersion uniformity, which is beneficial to the dissolution of wool keratin and improve the extraction rate of wool keratin.
[0056] Compare Comparative Examples 5 - 6 with Example 1. The fluorosilicone surfactant in the raw material of the dissolution treatment solution in the extraction process of Comparative Example 5 is prepared by using ethyl acrylate, propylenediamine, and 2,2,2 - trifluoroethyl acrylate; the fluorosilicone surfactant in the raw material of the dissolution treatment solution in the extraction process of Comparative Example 6 is prepared by using ethyl acrylate, propylenediamine, and 3 - allyloxypropyltrimethoxysilane; the fluorosilicone surfactant in the raw material of the dissolution treatment solution in the extraction process of Example 1 is prepared by using ethyl acrylate, propylenediamine, 2,2,2 - trifluoroethyl acrylate, and 3 - allyloxypropyltrimethoxysilane. It can be seen from this that in the preparation method of the fluorosilicone surfactant, by the reaction of ethyl acrylate and propylenediamine to increase the number of branched chains, and then grafting 2,2,2 - trifluoroethyl acrylate and 3 - allyloxypropyltrimethoxysilane simultaneously to obtain the fluorosilicone surfactant, the fluorosilicone surfactant contains fluorine groups, silicon groups, ester groups, amide groups, and tertiary amine groups, which improves the use effect of the fluorosilicone surfactant and increases the extraction rate of wool keratin.
[0057] It should be noted that the above-described embodiments are only used to explain the present application and do not constitute any limitation to the present application. The present application has been described by referring to typical embodiments, but it should be understood that the words used therein are descriptive and explanatory words rather than limiting words. Modifications can be made to the present application within the scope of the claims of the present application as provided, and the present application can be revised without departing from the scope and spirit of the present application. Although the present application described therein relates to specific methods, materials and embodiments, it does not mean that the present application is limited to the specific examples disclosed therein. On the contrary, the present application can be extended to all other methods and applications with the same function.
Claims
1. A process for extracting keratin from wool, characterized in that: The steps include: S1, washing, degreasing, drying and crushing the wool to obtain wool powder; S2. Under the protection of inert gas, immerse the wool powder in the dissolving treatment solution, heat it to 60-70°C, keep it warm for 1-3 hours, heat it to 80-100°C, keep it warm for 4-6 hours, cool it to room temperature, centrifuge it, and obtain the wool keratin solution; S3, dialyzing the wool keratin solution, freeze-drying, crushing, and sieving to obtain wool keratin; The dissolving treatment liquid is mainly made of the following raw materials in parts by weight: 100 parts of water, 4-6 parts of sodium thiosulfate, 9-11 parts of 1,4-dithiothreitol, 2-4 parts of alkylphenol polyoxyethylene ether, 1-3 parts of fluorinated silicon surfactant, 0.1-0.3 parts of sodium dodecyl sulfate, and 0.1-0.3 parts of dipropylene glycol methyl ether.
2. The process for extracting keratin from wool according to claim 1, characterized in that: The weight ratio of the wool powder to the dissolving treatment liquid is 1:(5-30).
3. The process for extracting keratin from wool according to claim 1, characterized in that: The fluorine-containing silicon surfactant is prepared by the following method: At a temperature of 60-70°C, ethanol and ethyl acrylate are mixed, and the first portion of propylene diamine is added dropwise. After the addition is completed, stirring is carried out for 18-22 hours. The second portion of propylene diamine is added dropwise. After the addition is completed, stirring is carried out for 13-17 hours. 2,2,2-trifluoroethyl acrylate and 3-allyloxypropyl trimethoxysilane are added dropwise respectively. After the addition is completed, stirring is carried out for 18-22 hours. Reduced pressure distillation is carried out to obtain a fluorine-containing silicon surfactant.
4. The process for extracting keratin from wool according to claim 3, characterized in that: The weight ratio of the ethyl acrylate, the first part of propylene diamine, the second part of propylene diamine, 2,2,2-trifluoroethyl acrylate, and 3-allyloxypropyl trimethoxysilane is 10:(1.5-2.5):(7-8):(35-45):(20-30).
5. The process for extracting keratin from wool according to claim 3, characterized in that: The first portion of propylene diamine is added for 50-70 min, the second portion of propylene diamine is added for 50-70 min, the 2,2,2-trifluoroethyl acrylate is added for 50-70 min, and the 3-allyloxypropyl trimethoxysilane is added for 50-70 min.
6. The process for extracting keratin from wool according to claim 1, characterized in that: The alkylphenol polyoxyethylene ether is one or more of alkylphenol polyoxyethylene ether OP-10, alkylphenol polyoxyethylene ether NP-10 and alkylphenol polyoxyethylene ether TX-10.
7. The process for extracting keratin from wool according to claim 1, characterized in that: The average particle size of the wool powder is 100-500 μm.
8. The process for extracting keratin from wool according to claim 1, characterized in that: In step S1, during the degreasing treatment, a sodium bicarbonate solution is used for degreasing, and the mass concentration of the sodium bicarbonate solution is 0.5-1.5%.
9. The process for extracting keratin from wool according to claim 1, characterized in that: In step S3, during the dialysis treatment, the molecular weight cutoff of the dialysis is 1000-5000D, the dialysis time is 2-3 days, and during the dialysis process, the deionized water is replaced every 4-8 hours.
10. Wool keratin, characterized in that: The method is obtained by using the extraction process of keratin in wool as described in any one of claims 1 to 9.
Citation Information
Patent Citations
Preparation process for effectively dissolving wool and extracting wool keratin
CN115215932A