Preparation method of quinoa protein finishing agent for treating cellulosic fibers
Quinoa protein powder is prepared through enzymatic lysis and drying processes, and double purification and modification treatment is carried out, which solves the problem of poor binding of quinoa protein liquid with regenerated cellulose fibers in the prior art, and realizes the preparation of high-purity and high-active quinoa protein liquid, which is suitable for the application of composite fibers.
Patent Information
- Application Number
- CN202411558828.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-04
- Publication Date
- 2025-03-07
AI Technical Summary
The prior art lacks effective methods for extracting and modifying quinoa protein liquids so that they can be well combined with regenerated cellulose fibers for the preparation of green and environmentally friendly healthy textiles.
Quinoa protein powder was prepared by enzymatic lysis and drying, and dissolved with ethanol, further dissolved at controlled temperature using potassium hydroxide solution, followed by double purification. Then, polyvinylpyrrolidone and glycidyl methacrylate were used for modification treatment to enhance the stability and binding strength of the quinoa protein solution.
It realizes the preparation of high-purity and high-activity quinoa protein solution, which can be combined with cellulose fibers, enhances the mechanical properties and additional functionality of the fibers, and is suitable for green and environmentally friendly healthy textiles.
Smart Images
Figure CN119571616A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of quinoa protein finishing agent preparation, in particular to a method for preparing a quinoa protein finishing agent that can be used for treating cellulose fibers. Background Art
[0002] Quinoa is a plant of the genus Chenopodiaceae. It is cold-resistant, drought-resistant, and salt-resistant. It is a crop that prefers cool and high altitudes. It requires almost no fertilizers or pesticides throughout the process and has natural pollution-free characteristics. Quinoa seeds are mainly white, black, red and other colors, among which white tastes the best and has the highest nutritional value. Quinoa is high in protein and contains a rich variety of amino acids. In addition to the 9 essential amino acids for humans, it also contains many non-essential amino acids, especially lysine, which is not found in most crops. The main components of quinoa protein are albumin and globulin, and the role of disulfide bonds makes their molecular structure more stable. In addition, quinoa is rich in mineral elements and a variety of vitamins required for normal human metabolism. It does not contain cholesterol and gluten, and its sugar content, fat content and calories are all at a low level.
[0003] Raw cellulose fiber is a fiber extracted and remade from cellulose raw materials by chemical methods. Cellulose is a natural high molecular polymer widely found in plants, mainly derived from the cell walls of plants such as cotton, wood, and hemp, mainly including viscose fiber and lyocell fiber. Regenerated cellulose fiber is widely used in textiles and clothing, medical and health care, paper manufacturing, and industrial filtration materials due to its excellent physical and chemical properties, such as good hygroscopicity, softness, breathability, and biodegradability. The presence of active hydroxyl groups on cellulose molecules allows each link in the production of regenerated cellulose fibers to be grafted and copolymerized with many other molecules for combined modification.
[0004] Quinoa protein can be effectively extracted to prepare composite regenerated cellulose fiber raw materials, which can be used to prepare green, environmentally friendly and healthy textiles. However, there is currently no relatively mature technology for this, and there is also a lack of reports on the extraction and modification methods of quinoa protein liquid that can be well combined with regenerated cellulose fibers.
[0005] Therefore, in view of this, the existing structure and defects are studied and improved, and a preparation method of a quinoa protein finishing agent that can be used to treat cellulose fibers is proposed. Summary of the invention
[0006] In view of the deficiencies in the prior art, the present invention provides a method for preparing a quinoa protein finishing agent that can be used to treat cellulose fibers, thereby solving the problems raised in the above-mentioned background technology.
[0007] To achieve the above objectives, the present invention is implemented by the following technical scheme: a preparation method of a quinoa protein finishing agent that can be used to treat cellulose fibers, the preparation method comprising the following steps: Preparation of quinoa protein liquid: washing the quinoa raw material, removing impurities, and adding an appropriate amount of deionized water to prepare a quinoa dispersion slurry; adding an appropriate amount of alkaline protease to the quinoa dispersion slurry, and performing preliminary enzymolysis under appropriate pH and temperature conditions to cleave the protein in the quinoa; Modification of quinoa protein liquid: polyvinyl pyrrolidone and glycidyl methacrylate were used to modify the quinoa protein liquid; Modification of cellulose fibers: including pretreatment and immersion in modified quinoa protein solution for chemical cross-linking reaction.
[0008] Furthermore, the amount of vinyl pyrrolidone added is 1-20% of the quinoa protein liquid, and the amount of glycidyl methacrylate added is 5-15% of the weight of the quinoa protein liquid.
[0009] Furthermore, the reaction temperature of the initial enzymatic hydrolysis of quinoa protein is 45-65°C, and the reaction time is 1h-10h. The reaction temperature of the quinoa protein liquid polyvinyl pyrrolidone and glycidyl methacrylate (GMA) is 60-80°C, and the reaction time is 1h-6h. The pH value of the secondary enzymatic hydrolysis is 6.0-7.5, the temperature is 50-70°C, and the reaction time is 2-6 hours.
[0010] Furthermore, an appropriate amount of amylase and digestive enzyme are added to the quinoa dispersion slurry that has undergone preliminary enzymatic hydrolysis, and secondary enzymatic hydrolysis is continued under controlled conditions to further decompose starch and sugars and improve the protein extraction rate; unreacted carbohydrates and insoluble matter in the enzymatic hydrolysis process are removed by filtration or centrifugation to obtain a relatively pure quinoa protein slurry; the quinoa protein slurry is dried, which can be spray drying, freeze drying or other suitable drying techniques, to finally obtain quinoa protein powder.
[0011] Furthermore, the added amounts of amylase and digestive enzyme are 0.5-2.0% and 0.1-0.5% of the weight of the quinoa dispersion, respectively.
[0012] Furthermore, in the modification treatment of the cellulose fibers, the chemical crosslinking reaction conditions are pH 3.5-5.5 and 60°C-120°C, and maintained for 1-2 hours.
[0013] Furthermore, the quinoa is pretreated before enzymatic hydrolysis, and the pretreatment method is: first swelling with hot water, then removing water and mixing and grinding with ethanol-type volatile alcohol to obtain the quinoa dispersion slurry.
[0014] Furthermore, the quinoa dispersed slurry is first adjusted to alkaline pH with alkali solution, and then alkaline protease is added for hydrolysis to obtain quinoa protein primary slurry, and then acid is used to adjust the pH of the quinoa protein primary slurry to neutral, and then amylase and digestive enzyme are added to obtain the quinoa protein slurry. The quinoa modified finishing agent is suitable for cellulose fibers including viscose fibers or lyocell fibers.
[0015] Furthermore, quinoa protein powder is dissolved in a solvent and an alkali solution and purified multiple times to obtain the quinoa protein liquid, and the purification includes centrifugation and filter pressing.
[0016] Further, quinoa protein powder and ethanol are mixed at a ratio of 1:1.5-10, dissolved in an alkali solution at a temperature of 45-80°C for full dissolution, the dissolved protein solution is centrifuged, and then filtered twice with a plate and frame filter to obtain a quinoa protein solution. The drying technology used in the drying step is spray drying, the air inlet temperature is controlled at 150-200°C, the air outlet temperature is controlled at 80-100°C, and the heat setting condition in the post-treatment is maintained at 120°C for 30 minutes The present invention provides a method for preparing a quinoa protein finishing agent that can be used to treat cellulose fibers, which has the following beneficial effects: 1. The preparation method of the quinoa protein finishing agent for treating cellulose fiber comprises mixing the quinoa protein powder obtained by enzymatic hydrolysis and drying process with an appropriate amount of ethanol to promote its dissolution. Using potassium hydroxide solution as a solvent, the quinoa protein powder is further dissolved under precisely controlled temperature conditions to ensure the full dissolution of the protein and the retention of biological activity. The obtained quinoa protein solution is subjected to two purification processes, the first purification may involve physical methods such as filtration or centrifugation, and the second purification may use more sophisticated membrane filtration or chromatography technology to remove impurities and improve the purity of the protein solution. After double purification, a quinoa protein solution with a higher purity is obtained, and the quinoa protein content is 5-60%.
[0017] 2. The preparation method of the quinoa protein finishing agent for treating cellulose fibers comprises modifying the purified quinoa protein liquid, first using polyvinyl pyrrolidone (PVP) as a dispersant to improve the uniformity of the dispersion of the quinoa protein liquid in the fiber. Subsequently, glycidyl methacrylate (GMA) is used for cross-linking modification to enhance the stability of the quinoa protein liquid and its binding force with the cellulose fiber. After the above steps, the quinoa protein liquid finally obtained not only has high purity, but also has better functionality through modification, and is suitable for composite application with regenerated cellulose fiber. BRIEF DESCRIPTION OF THE DRAWINGS
[0018] Figure 1 This is a table showing the protein content of samples obtained in different embodiments of the present invention. DETAILED DESCRIPTION
[0019] The following embodiments of the present invention are described in further detail in conjunction with the accompanying drawings and examples. The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention. Example 1
[0020] A method for preparing quinoa protein comprises the following steps: Quinoa pretreatment: rinse the quinoa with pure water continuously, drain the water, soak it in hot water for 4 hours, dry it in an oven, add ethanol, stir evenly, and grind it in a grinder. The ratio of quinoa to ethanol is 1:6. Enzymolysis: adjust the pH to 9.0 with potassium hydroxide, add 5% alkaline protease to the quinoa protein slurry for hydrolysis, keep warm at 35°C for 3 hours, and preliminarily obtain the primary quinoa protein slurry, then adjust the pH to 7.0 with dilute acetic acid, add 5% amylase and digestive enzyme, the mass ratio of amylase to digestive enzyme is 1:1, keep warm at 35°C, fully react for 2 hours, and spray dry the obtained protein solution to obtain high-purity quinoa protein powder; Cross-linking modification: Mix quinoa protein powder and ethanol in a ratio of 1:6, and use a 1% potassium hydroxide solution to fully dissolve it. The specific dissolution temperature curve is: first increase the temperature from room temperature to 55°C at 2°C / min, keep it warm for 1 hour, then increase the temperature to 75°C at 5°C / min, keep it warm for 0.5 hour, filter the dissolved protein liquid using a centrifuge at a speed of 4000 rpm for 4 minutes, and then use a plate and frame filter for secondary filtration.
[0021] The temperature of the filtered filtrate, i.e., the quinoa protein liquid, was raised to 55°C, 4% polyvinyl pyrrolidone was added, stirred evenly, and reacted for 1.5 hours; the temperature was then raised to 75°C, 4% glycidyl methacrylate was added, stirred evenly, and reacted for 1.5 hours. The protein content of the quinoa protein liquid obtained after stirring evenly was 20%. Example 2
[0022] A method for preparing quinoa protein comprises the following steps: Quinoa pretreatment: rinse the quinoa with pure water continuously, drain the water, soak it in hot water for 6 hours, dry it in an oven, add ethanol, stir it evenly, and grind it in a grinder. The ratio of quinoa to ethanol is 1:4. Enzymolysis: adjust the pH to 10.0 with sodium hydroxide, add 6% alkaline protease to the quinoa protein slurry for hydrolysis, keep warm at 40°C for 4 hours, and preliminarily obtain the primary quinoa protein slurry. Then adjust the pH to 6.8 with dilute acetic acid, add 6% amylase and digestive enzyme, the mass ratio of amylase and digestive enzyme is 1:1, keep warm at 40°C, fully react for 3 hours, and spray dry the obtained protein solution to obtain high-purity quinoa protein powder.
[0023] Cross-linking modification: Mix quinoa protein powder and ethanol in a ratio of 1:4, and fully dissolve it in a 2% sodium hydroxide solution. The specific dissolution temperature curve is: first increase the temperature from room temperature to 65°C at 2°C / min, keep it warm for 2 hours, then increase the temperature to 85°C at 5°C / min, keep it warm for 1 hour, filter the dissolved protein liquid using a centrifuge at a speed of 5000 rpm for 5 minutes, and then use a plate and frame filter for secondary filtration.
[0024] The temperature of the filtered filtrate, i.e., the quinoa protein liquid, was raised to 60°C, 5% polyvinyl pyrrolidone was added, stirred evenly, and reacted for 2 hours; the temperature was then raised to 80°C, 8% glycidyl methacrylate was added, stirred evenly, and reacted for 2 hours. The protein content of the quinoa protein liquid obtained after stirring evenly was 30%.
[0025] Comparative Example 1 The difference between this embodiment and embodiment 1 is that the added amount of polyvinyl pyrrolidone is 5% of the quinoa protein liquid, and the added amount of glycidyl methacrylate is 5% of the quinoa protein liquid.
[0026] Comparative Example 2 The difference between this embodiment and embodiment 1 is that the added amount of polyvinyl pyrrolidone is 8% of the quinoa protein liquid, and the added amount is 8% of the quinoa protein liquid.
[0027] Comparative Example 3 The difference between this embodiment and embodiment 1 is that polyvinyl pyrrolidone and glycidyl methacrylate are not added to the quinoa protein liquid after enzymatic hydrolysis for modification.
[0028] Comparative Example 4 The difference between this embodiment and embodiment 1 is that glycidyl methacrylate is not added to the quinoa protein liquid after the primary modification for secondary cross-linking modification.
[0029] The protein content of the above examples and comparative examples was tested, and the test results obtained are as follows: Figure 1 As shown: From the instruction manual Figure 1 It can be seen that after the quinoa protein liquid is modified, its protein content is significantly increased.
[0030] Through the above embodiments, the present invention provides a method for preparing quinoa protein, which can efficiently prepare a quinoa protein liquid with high purity and high activity by accurately controlling the enzymatic hydrolysis conditions, dissolution and cross-linking modification steps. The obtained quinoa protein liquid can be used for compounding with cellulose fibers to enhance the mechanical properties and additional functionality of the fibers, and has broad application prospects.
[0031] The embodiments of the present invention are given for the purpose of illustration and description, and are not intended to be exhaustive or to limit the invention to the disclosed forms. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiments are selected and described in order to better illustrate the principles and practical applications of the present invention and to enable those of ordinary skill in the art to understand the present invention and thereby design various embodiments with various modifications suitable for specific uses.
Claims
1. A method for preparing a quinoa protein finishing agent for treating cellulose fibers, characterized in that: The preparation method comprises the following steps: Preparation of quinoa protein liquid: washing the quinoa raw material, removing impurities, and adding an appropriate amount of deionized water to prepare a quinoa dispersion slurry; adding an appropriate amount of alkaline protease to the quinoa dispersion slurry, and performing preliminary enzymolysis under appropriate pH and temperature conditions to cleave the protein in the quinoa; Modification of quinoa protein liquid: polyvinyl pyrrolidone and glycidyl methacrylate were used to modify the quinoa protein liquid; Modification of cellulose fibers: including pretreatment and immersion in modified quinoa protein solution for chemical cross-linking reaction.
2. The method for preparing a quinoa protein finishing agent for treating cellulose fibers according to claim 1, characterized in that: The added amount of polyvinyl pyrrolidone is 1-20% of the quinoa protein liquid, and the added amount of glycidyl methacrylate is 5-15% of the weight of the quinoa protein liquid.
3. The method for preparing a quinoa protein finishing agent for treating cellulose fibers according to claim 2, characterized in that: The reaction temperature of the initial enzymatic hydrolysis of quinoa protein is 45-65°C, and the reaction time is 1h-10h. The reaction temperature of the quinoa protein liquid polyvinyl pyrrolidone and glycidyl methacrylate (GMA) is 60-80°C, and the reaction time is 1h-6h. The pH value of the secondary enzymatic hydrolysis is 6.0-7.5, the temperature is 50-70°C, and the reaction time is 2-6 hours.
4. The method for preparing a quinoa protein finishing agent for treating cellulose fibers according to claim 1, characterized in that: The quinoa dispersion slurry that has undergone preliminary enzymatic hydrolysis is then added with an appropriate amount of amylase and digestive enzyme, and secondary enzymatic hydrolysis is continued under controlled conditions to further decompose starch and sugars and improve the protein extraction rate; unreacted carbohydrates and insoluble matter in the enzymatic hydrolysis process are removed by filtration or centrifugation to obtain a relatively pure quinoa protein slurry; the quinoa protein slurry is dried, which can be spray drying, freeze drying or other suitable drying techniques, to finally obtain quinoa protein powder.
5. The method for preparing a quinoa protein finishing agent for treating cellulose fibers according to claim 1, characterized in that: The added amounts of amylase and digestive enzyme are 0.5-2.0% and 0.1-0.5% of the weight of the quinoa dispersion slurry, respectively.
6. The method for preparing a quinoa protein finishing agent for treating cellulose fibers according to claim 1, characterized in that: In the modification treatment of cellulose fibers, the conditions for the chemical crosslinking reaction are pH 3.5-5.5 and 60°C-120°C, and maintained for 1-2 hours.
7. The method for preparing a quinoa protein finishing agent for treating cellulose fibers according to claim 1, characterized in that: The quinoa is pretreated before enzymolysis, and the pretreatment method is: firstly swell with hot water, then remove the water and mix and grind with ethanol-type volatile alcohol to obtain the quinoa dispersion slurry.
8. The method for preparing a quinoa protein finishing agent for treating cellulose fibers according to claim 7, characterized in that: The quinoa dispersion slurry is firstly prepared by adjusting the pH value to alkaline with alkali solution, and then adding alkaline protease to hydrolyze to obtain a quinoa protein primary slurry. Then, the pH value of the quinoa protein primary slurry is adjusted to neutral with acid, and then amylase and digestive enzyme are added to obtain the quinoa protein slurry. The quinoa modified finishing agent is suitable for cellulose fibers including viscose fibers or lyocell fibers.
9. The method for preparing a quinoa protein finishing agent for treating cellulose fibers according to claim 1, characterized in that: The quinoa protein powder is dissolved in a solvent and an alkali solution and is purified multiple times to obtain the quinoa protein liquid, wherein the purification includes centrifugation and filter pressing.
10. The method for preparing a quinoa protein finishing agent for treating cellulose fibers according to claim 1, characterized in that: Quinoa protein powder and ethanol are mixed at a ratio of 1:1.5-10, dissolved in an alkaline solution at a temperature of 45-80°C for full dissolution, the dissolved protein solution is centrifugally filtered, and then filtered twice with a plate and frame filter to obtain a quinoa protein solution. The drying technology used in the drying step is spray drying, the inlet air temperature is controlled at 150-200°C, the outlet air temperature is controlled at 80-100°C, and the heat setting condition in the post-treatment is maintained at 120°C for 30 minutes.