High-fluffiness hydrophobic goose down and preparation method thereof

Abstract

The method comprises the following steps that goose down is soaked in a glutaraldehyde solution in a heat preservation mode, an enzyme preparation is added, the goose down is subjected to heat preservation and standing for enzymolysis treatment, and pretreated goose down is obtained after inactivation, cleaning and drying; 3-aminopropyltriethoxysilane is used for modifying biomass activated carbon to obtain modified biomass activated carbon, the modified biomass activated carbon adsorbs a waterborne polyurethane solution, then low-temperature baking is conducted, and the modified biomass activated carbon is ultrasonically dispersed into the pretreated down feather; raw materials are mixed to prepare membrane liquid, the membrane liquid is prepared from dopamine hydrochloride, glycerol triglycidyl ether, m-xylylenediamine, nano silicon dioxide, lithium chloride, ethyl alcohol and deionized water, and the membrane liquid forms a membrane layer on the surface of goose down through an electrostatic atomization-deposition method. The prepared goose down is high in washing resistance, high hydrophobicity and antibacterial property can still be kept after multiple times of washing, and the filling power of the goose down can be improved.

Description

Technical Field

[0001] This invention belongs to the field of wool and cashmere fabric technology, specifically relating to a high-loft, hydrophobic goose down and its preparation method. Background Technology

[0002] Goose down has a strong hygroscopic property, easily absorbing moisture in humid environments, causing fibers to stick together, clump, and lose fluffiness, significantly reducing its warmth retention. Secondly, during the washing process, the fibers of goose down products are prone to breakage, entanglement, and shrinkage, causing irreversible structural damage and seriously affecting the product's lifespan. In addition, as a protein fiber, goose down is prone to the growth of bacteria, mold, and other microorganisms during storage and use, producing odors and posing potential health risks.

[0003] To address the aforementioned problems, existing technologies primarily employ the following methods: achieving waterproofing through surface coating with a hydrophobic agent. However, traditional impregnation processes easily lead to fiber adhesion, severely affecting its fluffiness. Furthermore, the coating exhibits weak bonding with the down fibers (or down filaments), resulting in poor washability. After repeated washing, the hydrophobic properties decrease dramatically, and the weight loss rate is high. Adding organic or inorganic antibacterial agents imparts antibacterial properties, but the antibacterial components are easily dissolved during washing, leading to poor durability. Therefore, this invention provides a high-fluff, hydrophobic down and its preparation method to solve the aforementioned technical problems. Summary of the Invention

[0004] The purpose of this invention is to provide a high-loft, hydrophobic goose down and its preparation method in order to solve the above-mentioned problems.

[0005] The present invention achieves the above objectives through the following technical solutions: A method for preparing highly loft, hydrophobic goose down specifically includes the following steps: Step 1: Soak goose down in glutaraldehyde solution at a warm temperature, then add enzyme preparation, keep warm and stand for enzymatic hydrolysis, and then obtain pretreated down after inactivation, washing and drying. Step 2: Modified biomass activated carbon is obtained by modifying biomass activated carbon with 3-aminopropyltriethoxysilane. The modified biomass activated carbon is then used to adsorb aqueous polyurethane solution, baked at low temperature, and then ultrasonically dispersed into pretreated down. Step 3: Mix and prepare a membrane solution by mixing various raw materials. The raw materials for preparing the membrane solution, by weight, include 5-10 parts of dopamine hydrochloride, 4-6 parts of glycerol triglycidyl ether, 1-3 parts of m-phenylenediamine, 0.1-2 parts of nano-silica, 0.1-1 parts of lithium chloride, 8-12 parts of ethanol, and 70-80 parts of deionized water. The membrane solution is deposited on the surface of the goose down treated in Step 2 using an electrostatic atomization-deposition method to form a membrane layer. After curing, a highly fluffy hydrophobic goose down is obtained.

[0006] As a further optimization of the present invention, in step one, the mass ratio of the goose down to the 2-6wt% glutaraldehyde solution is 1:10-20; The enzyme preparation is transglutaminase and / or tyrosinase, and the dosage of the enzyme preparation is 15-45g / kg goose down.

[0007] As a further optimization of the present invention, in step one, the heat preservation soaking specifically involves adjusting the pH to 7-8 and soaking at a temperature of 50-60℃ for 50-80 minutes. The heat preservation and static setting process specifically involves maintaining a temperature of 40-50℃ for 1-3 hours.

[0008] As a further optimization of the present invention, in step one, before soaking the goose down in glutaraldehyde solution, the goose down is subjected to micro-etching treatment with an aqueous solution of 4-8wt% thiourea and 0.5-2wt% sodium dodecyl sulfate, with a bath ratio of 1:5-8, and stirred at 25-40 r / min for 10-15 h.

[0009] As a further optimization of the present invention, in step two, the modification treatment specifically involves preparing a 2-5 wt% 3-aminopropyltriethoxysilane solution using ethanol as a solvent, heating it to 70-80°C, adding biomass activated carbon and soaking for 30-50 minutes, centrifuging, drying and obtaining modified biomass activated carbon. The mass ratio of the biomass activated carbon to 2-5 wt% 3-aminopropyltriethoxysilane solution is 1:5-7.

[0010] As a further optimization of the present invention, in step two, the mass ratio of the modified biomass activated carbon to 12-20wt% aqueous polyurethane solution is 7-10:1; The low-temperature baking specifically refers to baking at 28-35℃ for 20-40 minutes; The mass ratio of the modified biomass activated carbon to the pretreated down is 3-7:1; The ultrasonic dispersion specifically involves a frequency of 45-60 kHz, a power of 300-500 W, a duration of 12-18 min, and a temperature of 65-80 °C.

[0011] As a further optimization of the present invention, in step three, the electrostatic atomization deposition method is used to form a 10-15 nm film layer on the goose down surface. Specifically, the rotation speed of the cage containing the goose down is 15-20 r / min, the nozzle voltage is 24-28 kV, the distance between the nozzle and the down layer is 10-15 cm, the pH of the film solution is 7.5-8.5, the flow rate of the film solution is 0.5-2 mL / min, and the atomized particle size is 25-32 µm.

[0012] As a further optimization of the present invention, in step three, the curing temperature is 65-80℃ and the time is 35-60min.

[0013] A highly fluffy, hydrophobic goose down is prepared by any of the preparation methods described above.

[0014] The beneficial effects of this invention are as follows: 1) This invention uses thiourea and sodium dodecyl sulfate aqueous solution to micro-etch goose down, soaks it in glutaraldehyde solution, and selects a specific combination of enzyme preparations to enzymatically hydrolyze the goose down to obtain pretreated goose down. Biomass activated carbon is used to modify the down and then adsorbs water-based polyurethane and ultrasonically disperses it into the pretreated goose down. Then, the membrane liquid is formed on the surface of the goose down containing water-based polyurethane and biomass activated carbon by electrostatic atomization-deposition method. This makes the goose down obtained have strong water wash resistance and can still maintain high hydrophobicity and antibacterial properties after multiple water washes, and can also improve the fluffiness of the goose down. 2) This invention uses a thiourea and sodium dodecyl sulfate aqueous solution to perform micro-etching treatment on goose down and selects a specific combination of enzyme preparations to perform enzymatic hydrolysis treatment on goose down, which can significantly improve the fluffiness of goose down and the strength and toughness of goose down fibers. Detailed Implementation

[0015] The present application will now be described in further detail. It should be noted that the following specific embodiments are only used to further illustrate the present application and should not be construed as limiting the scope of protection of the present application. Those skilled in the art can make some non-essential improvements and adjustments to the present application based on the above application content.

[0016] I. Materials 1. Goose down: Commercially available cleaned and degreased goose down, purchased from Anhui Yamei Feather and Down Co., Ltd. 2. Glutaraldehyde: Purchased from Xi'an Degu Biotechnology Co., Ltd., with a solid content of 50%. It can be mixed and diluted with water or ethanol in any way. In the following experiments, water was used to dilute it to obtain a 2-6 wt% glutaraldehyde solution. 3. Enzyme preparations: transglutaminase (purchased from Lianyungang Haiheng Biochemical Technology Co., Ltd., purity 99.99%) and / or tyrosinase (purchased from Tianmen Hengchang Chemical Co., Ltd., purity 99%). 4. 3-Aminopropyltriethoxysilane (silane coupling agent KH-550): Purchased from Shanghai Yuanye Biotechnology Co., Ltd., purity 98%; 5. Biomass activated carbon (bamboo activated carbon): purchased from Xi'an Qiyue Biotechnology Co., Ltd., with a purity of 99% and an average particle size of 0.1-0.5μm; 6. Waterborne polyurethane solution: purchased from Beijing Kemete Technology Development Co., Ltd., with a solid content of 50±2%, which can be diluted with water. In the following experiments, water was used to dilute the solution to obtain a 12-20wt% glutaraldehyde solution. 7. Thiourea: Purchased from Shandong Chongcheng Energy Technology Co., Ltd., purity 99%; 8. Sodium dodecyl sulfate: Purchased from Jinan Renyuan Chemical Co., Ltd., purity 98%; 9. Membrane solution raw materials: 5-10 parts dopamine hydrochloride (purchased from Shanghai Yuanye Biotechnology Co., Ltd., purity 98.5%), 4-6 parts glycerol triglycidyl ether (purchased from Wuhan Xinxin Jiali Biotechnology Co., Ltd., purity 99%), 1-3 parts m-phenylenediamine (purchased from Kandis Chemical (Hubei) Co., Ltd., purity 99%), 0.1-2 parts nano silica (purchased from Yumu (Ningbo) New Materials Co., Ltd., purity 99.9%), 0.1-1 parts lithium chloride (purchased from Jiangsu Changjili New Energy Technology Co., Ltd., purity 99%), 8-12 parts ethanol (purchased from Shandong Yifei Science and Trade Co., Ltd., purity 99%), 70-80 parts deionized water; sodium hydroxide is used as the pH adjuster for the membrane solution. Note: The following experiments in this invention all use preferred parameters; Unless otherwise specified, all methods used in the following examples can be performed using conventional methods. Other materials and reagents used can be obtained commercially unless otherwise specified.

[0017] II. Methods Example 1 In this embodiment, a method for preparing highly fluffy hydrophobic goose down includes the following specific steps: (1) Preparation of pretreated down In this embodiment, the method for obtaining pretreated down is as follows: Goose down is soaked in a 3.5wt% glutaraldehyde solution (mass ratio of 1:12), the pH is adjusted to 7.2, and the solution is kept at 55°C for 65 minutes. Then, an enzyme preparation (transglutaminase, enzyme activity 8.3±0.5×10⁻⁶) is added. 5 The enzyme preparation was used at a rate of 36 g / kg of goose down. The down was kept at 45°C for 2 hours for enzymatic hydrolysis, and then inactivated, washed, and dried to obtain pretreated down.

[0018] (2) Preparation of modified biomass activated carbon and mixing with pretreated goose down ① Preparation of modified biomass activated carbon: Using ethanol as solvent, a 3.5 wt% 3-aminopropyltriethoxysilane solution was prepared. After heating to 75℃, biomass activated carbon was added and soaked for 40 min (the mass ratio of biomass activated carbon to 2 wt% 3-aminopropyltriethoxysilane solution was 1:6) to modify the biomass activated carbon. After centrifugation and drying, the modified biomass activated carbon was obtained. ② Mixing with pretreated goose down: The modified biomass activated carbon was used to adsorb 16.5wt% aqueous polyurethane solution. The mass ratio of modified biomass activated carbon to 16.5wt% aqueous polyurethane solution was 8.5:1. The mixture was baked at 30℃±1℃ for 28 min, and the dry basis dryness (dry basis dryness = dehydrated mass / initial moisture content) was 13.5%. The mixture was then ultrasonically dispersed into the pretreated down (the mass ratio of modified biomass activated carbon to pretreated down was 5:1). The ultrasonic dispersion frequency was 52KHz, the power was 380W, the time was 15 min, and the temperature was 55℃.

[0019] (3) Preparation of film layer by electrostatic atomization deposition method The raw materials for preparing the membrane solution, by weight, include 5 parts of dopamine hydrochloride, 6 parts of glycerol triglycidyl ether, 3 parts of m-phenylenediamine, 0.8 parts of nano-silica, 0.6 parts of lithium chloride, 12 parts of ethanol, and 72.6 parts of deionized water. The membrane solution is deposited on the goose down surface treated in step (2) above using an electrostatic atomization-deposition method to form a membrane layer. A mixture of various raw materials was prepared to obtain a membrane solution. An electrostatic atomization-deposition method was used to form a 12±1nm membrane layer on the surface of the goose down treated in step (2). Specifically, the rotation speed of the cage containing the goose down was 18r / min, the nozzle voltage was 25kV, the distance between the nozzle and the down layer was 12cm, the pH of the membrane solution was 8.2, the membrane solution volume was 0.8mL / min, and the atomization particle size was 28µm. After curing treatment, highly fluffy hydrophobic goose down was obtained. The curing treatment temperature was 70℃ and the time was 38min.

[0020] Example 2 In this embodiment, a method for preparing highly fluffy hydrophobic goose down includes the following specific steps: (1) Preparation of pretreated down In this embodiment, the method for obtaining pretreated down is as follows: Goose down is soaked in a 3.5wt% glutaraldehyde solution (mass ratio of 1:12), the pH is adjusted to 7.2, and the solution is kept at 55°C for 65 minutes. Then, an enzyme preparation (transglutaminase, enzyme activity 8.3±0.5×10⁻⁶) is added. 5 The enzyme preparation was used at a rate of 36 g / kg of goose down. The down was kept at 45°C for 2 hours for enzymatic hydrolysis, and then inactivated, washed, and dried to obtain pretreated down.

[0021] (2) Preparation of modified biomass activated carbon and mixing with pretreated goose down ① Preparation of modified biomass activated carbon: Using ethanol as solvent, a 3.5 wt% 3-aminopropyltriethoxysilane solution was prepared. After heating to 75℃, biomass activated carbon was added and soaked for 40 min (the mass ratio of biomass activated carbon to 2 wt% 3-aminopropyltriethoxysilane solution was 1:6) to modify the biomass activated carbon. After centrifugation and drying, the modified biomass activated carbon was obtained. ② Mixing with pretreated goose down: The modified biomass activated carbon was used to adsorb 16.5wt% aqueous polyurethane solution. The mass ratio of modified biomass activated carbon to 16.5wt% aqueous polyurethane solution was 8.5:1. The mixture was baked at 30℃±1℃ for 28 min, and the dry basis dryness (dry basis dryness = dehydrated mass / initial moisture content) was 13.5%. The mixture was then ultrasonically dispersed into the pretreated down (the mass ratio of modified biomass activated carbon to pretreated down was 5:1). The ultrasonic dispersion frequency was 52KHz, the power was 380W, the time was 15 min, and the temperature was 55℃.

[0022] (3) Preparation of film layer by electrostatic atomization deposition method The raw materials for preparing the membrane solution, by weight, include 7 parts of dopamine hydrochloride, 5 parts of glycerol triglycidyl ether, 2 parts of m-phenylenediamine, 0.7 parts of nano-silica, 0.5 parts of lithium chloride, 10 parts of ethanol, and 74.8 parts of deionized water. The membrane solution is deposited on the goose down surface treated in step (2) above using an electrostatic atomization-deposition method to form a membrane layer. A mixture of various raw materials was prepared to obtain a membrane solution. An electrostatic atomization-deposition method was used to form a 12±1nm membrane layer on the surface of the goose down treated in step (2). Specifically, the rotation speed of the cage containing the goose down was 18r / min, the nozzle voltage was 25kV, the distance between the nozzle and the down layer was 12cm, the pH of the membrane solution was 8.2, the membrane solution volume was 0.8mL / min, and the atomization particle size was 28µm. After curing treatment, highly fluffy hydrophobic goose down was obtained. The curing treatment temperature was 70℃ and the time was 38min.

[0023] Example 3 In this embodiment, a method for preparing highly fluffy hydrophobic goose down includes the following specific steps: (1) Preparation of pretreated down In this embodiment, the method for obtaining pretreated down is as follows: Goose down is soaked in a 3.5wt% glutaraldehyde solution (mass ratio of 1:12), the pH is adjusted to 7.2, and the solution is kept at 55°C for 65 minutes. Then, an enzyme preparation (transglutaminase, enzyme activity 8.3±0.5×10⁻⁶) is added. 5The enzyme preparation was used at a rate of 36 g / kg of goose down. The down was kept at 45°C for 2 hours for enzymatic hydrolysis, and then inactivated, washed, and dried to obtain pretreated down.

[0024] (2) Preparation of modified biomass activated carbon and mixing with pretreated goose down ① Preparation of modified biomass activated carbon: Using ethanol as solvent, a 3.5 wt% 3-aminopropyltriethoxysilane solution was prepared. After heating to 75℃, biomass activated carbon was added and soaked for 40 min (the mass ratio of biomass activated carbon to 2 wt% 3-aminopropyltriethoxysilane solution was 1:6) to modify the biomass activated carbon. After centrifugation and drying, the modified biomass activated carbon was obtained. ② Mixing with pretreated goose down: The modified biomass activated carbon was used to adsorb 16.5wt% aqueous polyurethane solution. The mass ratio of modified biomass activated carbon to 16.5wt% aqueous polyurethane solution was 8.5:1. The mixture was baked at 30℃±1℃ for 28 min, and the dry basis dryness (dry basis dryness = dehydrated mass / initial moisture content) was 13.5%. The mixture was then ultrasonically dispersed into the pretreated down (the mass ratio of modified biomass activated carbon to pretreated down was 5:1). The ultrasonic dispersion frequency was 52KHz, the power was 380W, the time was 15 min, and the temperature was 55℃.

[0025] (3) Preparation of film layer by electrostatic atomization deposition method The raw materials for preparing the membrane solution, by weight, include 10 parts of dopamine hydrochloride, 4 parts of glycerol triglycidyl ether, 1 part of m-phenylenediamine, 0.4 parts of nano-silica, 0.8 parts of lithium chloride, 8 parts of ethanol, and 75.8 parts of deionized water. The membrane solution is deposited on the goose down surface treated in step (2) above using an electrostatic atomization-deposition method to form a membrane layer. A mixture of various raw materials was prepared to obtain a membrane solution. An electrostatic atomization-deposition method was used to form a 12±1nm membrane layer on the surface of the goose down treated in step (2). Specifically, the rotation speed of the cage containing the goose down was 18r / min, the nozzle voltage was 25kV, the distance between the nozzle and the down layer was 12cm, the pH of the membrane solution was 8.2, the membrane solution volume was 0.8mL / min, and the atomization particle size was 28µm. After curing treatment, highly fluffy hydrophobic goose down was obtained. The curing treatment temperature was 70℃ and the time was 38min.

[0026] Example 4 In this embodiment, a method for preparing high-loft hydrophobic goose down is based on Example 2, with adjustments made to the preparation of pretreated down in step (1). The adjusted method is as follows: In this embodiment, the method for obtaining pretreated down is as follows: Goose down is micro-etched using a 6.5wt% thiourea and 1.2wt% sodium dodecyl sulfate aqueous solution at a bath ratio of 1:6, stirred at 32 r / min for 12 h, rinsed twice with water, dehydrated, dried, and then soaked in a 3.5wt% glutaraldehyde solution (mass ratio of the two is 1:12), the pH is adjusted to 7.2, and the solution is kept at 55℃ for 65 min. Then, an enzyme preparation (transglutaminase, enzyme activity 8.3±0.5×10⁻⁶) is added. 5 The enzyme preparation was used at a rate of 36 g / kg of goose down. The down was kept at 45°C for 2 hours for enzymatic hydrolysis, and then inactivated, washed, and dried to obtain pretreated down. Everything else is consistent with Example 2.

[0027] Example 5 In this embodiment, a method for preparing high-loft hydrophobic goose down is based on Example 4, with adjustments made to the preparation of pretreated down in step (1). The adjusted method is as follows: In this embodiment, the method for obtaining pretreated down is as follows: Goose down is micro-etched using a 6.5wt% thiourea and 1.2wt% sodium dodecyl sulfate aqueous solution at a bath ratio of 1:6, stirred at 32 r / min for 12 h, rinsed twice with water, dehydrated, and dried. Then, it is soaked in a 3.5wt% glutaraldehyde solution (mass ratio of the two is 1:12), the pH is adjusted to 7.2, and it is kept at 55℃ for 65 min. Finally, an enzyme preparation (glutaminase and tyrosinase at a mass ratio of 1:1, with each enzyme activity of 8.3 ± 0.5 × 10⁻⁶) is added. 5 The enzyme preparation was used at a rate of 36 g / kg of goose down. The down was kept at 45°C for 2 hours for enzymatic hydrolysis, and then inactivated, washed, and dried to obtain pretreated down. Everything else is the same as in Example 4.

[0028] Example 6 In this embodiment, a method for preparing high-loft hydrophobic goose down is based on Example 4, with adjustments made to the preparation of pretreated down in step (1). The adjusted method is as follows: In this embodiment, the method for obtaining pretreated down is as follows: Goose down is micro-etched using a 6.5wt% thiourea and 1.2wt% sodium dodecyl sulfate aqueous solution at a bath ratio of 1:6, stirred at 32 r / min for 12 h, rinsed twice with water, dehydrated, dried, and then soaked in a 3.5wt% glutaraldehyde solution (mass ratio of the two is 1:12). The pH is adjusted to 7.2, and the solution is kept at 55℃ for 65 min. Then, an enzyme preparation (tyrosinase, enzyme activity 8.3±0.5×10⁻⁶) is added. 5The enzyme preparation was used at a rate of 36 g / kg of goose down. The down was kept at 45°C for 2 hours for enzymatic hydrolysis, and then inactivated, washed, and dried to obtain pretreated down. Everything else is the same as in Example 4.

[0029] Comparative Example 1 In this comparative example, a method for preparing high-loft hydrophobic goose down was based on Example 5, with adjustments made to the preparation of pretreated down in step (1). The adjusted method is as follows: In this comparative example, the pretreated down was obtained by micro-etching the goose down with a 6.5wt% thiourea and 1.2wt% sodium dodecyl sulfate aqueous solution at a bath ratio of 1:6, stirring at 32 rpm for 12 h, rinsing twice with water, dehydrating, drying, and then soaking in a 3.5wt% glutaraldehyde solution (mass ratio of the two solutions: 1:12), adjusting the pH to 7.2, and incubating at 55℃ for 65 min. Then, an enzyme preparation (laccase, enzyme activity 8.3±0.5×10⁻⁶) was added. 5 The enzyme preparation was used at a rate of 36 g / kg of goose down. The down was kept at 45°C for 2 hours for enzymatic hydrolysis, and then inactivated, washed, and dried to obtain pretreated down. Everything else is consistent with Example 5.

[0030] Comparative Example 2 In this comparative example, a method for preparing high-loft hydrophobic goose down was based on Example 5, with adjustments made to the preparation of pretreated down in step (1). The adjusted method is as follows: In this comparative example, the method for obtaining pretreated down was as follows: goose down was micro-etched with an aqueous solution of 6.5wt% thiourea and 1.2wt% sodium dodecyl sulfate at a bath ratio of 1:6, stirred at 32 r / min for 12 h, rinsed twice with water, dehydrated and dried, then soaked in a 3.5wt% glutaraldehyde solution (mass ratio of the two is 1:12), the pH was adjusted to 7.2, and the solution was kept at 55℃ for 65 min. After rinsing and drying, the pretreated down was obtained. Everything else is consistent with Example 5.

[0031] Comparative Example 3 In this comparative example, a method for preparing highly fluffy hydrophobic goose down is based on Example 5, but the preparation of pre-treated down in step (1) is omitted; Everything else is consistent with Example 5.

[0032] Comparative Example 4 In this comparative example, a method for preparing highly fluffy hydrophobic goose down was based on Example 5, with adjustments made to step (2) regarding the preparation of modified biomass activated carbon and its mixing with pretreated goose down. Step (2) was adjusted as follows: Mixed with pretreated goose down: 16.5wt% aqueous polyurethane solution was adsorbed using biomass activated carbon. The mass ratio of biomass activated carbon to 16.5wt% aqueous polyurethane solution was 8.5:1. The mixture was baked at 30℃±1℃ for 28 min, and the dry basis dryness (dry basis dryness = dehydrated mass / initial moisture content) was 13.5%. The mixture was then ultrasonically dispersed into the pretreated down (the mass ratio of biomass activated carbon to pretreated down was 5:1). The ultrasonic dispersion frequency was 52KHz, the power was 380W, the time was 15 min, and the temperature was 55℃. Everything else is consistent with Example 5.

[0033] Comparative Example 5 In this comparative example, a method for preparing highly fluffy hydrophobic goose down was based on Example 5, with adjustments made to step (2) regarding the preparation of modified biomass activated carbon and its mixing with pretreated goose down. Step (2) was adjusted as follows: Preparation of modified biomass activated carbon: Using ethanol as solvent, a 3.5 wt% 3-aminopropyltriethoxysilane solution was prepared. After heating to 75℃, biomass activated carbon was added and soaked for 40 min (the mass ratio of biomass activated carbon to 2 wt% 3-aminopropyltriethoxysilane solution was 1:6) to modify the biomass activated carbon. After centrifugation and drying, the modified biomass activated carbon was obtained. Mixing with pretreated goose down: Modified biomass activated carbon is ultrasonically dispersed into pretreated down (the mass ratio of modified biomass activated carbon to pretreated down is 5:1). The ultrasonic dispersion frequency is 52KHz, the power is 380W, the time is 15min, and the temperature is 55℃. Everything else is consistent with Example 5.

[0034] Comparative Example 6 In this comparative example, a method for preparing highly fluffy hydrophobic goose down was based on Example 5, with adjustments made to step (3) of preparing the film using the electrostatic atomization deposition method. Step (3) was adjusted as follows: The raw materials for preparing the membrane solution, by weight, include 5 parts dopamine, 6 parts glycerol triglycidyl ether, 3 parts m-phenylenediamine, 0.8 parts nano silica, 0.6 parts lithium chloride, 12 parts ethanol, and 72.6 parts deionized water. The membrane solution is deposited on the goose down surface treated in step (2) above using an electrostatic atomization-deposition method to form a membrane layer. A mixture of various raw materials was prepared to obtain a membrane solution. An electrostatic atomization-deposition method was used to form a 12±1nm membrane layer on the surface of the goose down treated in step (2). Specifically, the rotation speed of the cage containing the goose down was 18r / min, the nozzle voltage was 25kV, the distance between the nozzle and the down layer was 12cm, the pH of the membrane solution was 8.2, the membrane solution flow rate was 0.8mL / min, and the atomization particle size was 28µm. After curing treatment, highly fluffy hydrophobic goose down was obtained. The curing treatment temperature was 70℃ and the time was 38min. Everything else is consistent with Example 5.

[0035] Blank Group 1 Commercially available cleaned and degreased goose down was used as the blank group.

[0036] III. Performance Testing (1) Looseness test Method for obtaining goose down samples washed 45 times: Using 100% pure cotton fabric with a diameter of 12 inches, cut two pieces of fabric with a diameter of 12 inches. Sew the two circular pieces of fabric together to form a pillowcase, leaving a small opening for filling with down. Weigh 100g of goose down and fill the circular pillowcase through the small opening. Finally, sew the pillowcase closed to form a small circular pillow. According to the down washing method in IDFB—2017, the washing machine and dryer were operated according to the requirements of AATCC 135 standard. The single washing program was as follows: washing time 20min at 20℃±2℃, spin-drying time 7min, and drying time 28min at 40±2℃. The single washing program was repeated 45 times to obtain goose down samples washed 45 times.

[0037] The weight loss rate of the goose down samples washed 45 times in Examples 1-6, Comparative Examples 1-6, and the blank group was calculated using the following formula: Weight loss rate = [(Weight of unwashed goose down sample - Weight of goose down sample washed 45 times) / Weight of unwashed goose down sample] × 100%; Loft performance test: The loft performance of unwashed goose down samples and goose down samples washed 45 times were tested according to the experimental methods of GB / T 10288-2016 Test Methods for Down and Feathers. The down was rated according to the loft evaluation standards for down products specified in the latest national standard GB / T 45266-2025 Guidelines for Quality Grading of Consumer Products (Down Products). The loft evaluation standards for down are shown in Table 1. Table 1 Evaluation Criteria for Down Loft ; Table 2 shows the loft test data of unwashed goose down samples and goose down samples washed 45 times in water from Examples 1-6, Comparative Examples 1-6, and the blank group: Table 2. Test data on the loft performance of goose down ; Experimental Conclusion: Based on the experimental data in Table 2, it can be seen that the goose down in Examples 1-6 all have high loft and low weight loss rate after washing, indicating that the goose down fibers (or down filaments) have good toughness and are not easy to break. Compared with commercially available washed and degreased goose down, they all have varying degrees of improvement. Among them, the effects of Examples 4 and 5 are more prominent. This shows that micro-etching treatment of goose down with thiourea and sodium dodecyl sulfate aqueous solution and enzymatic hydrolysis treatment of goose down with a specific combination of enzyme preparations can significantly improve the loft of goose down and enhance the toughness of goose down fibers, making goose down resistant to washing and durable.

[0038] (2) Hydrophobicity test Hydrophobicity test: The surface contact angles of unwashed goose down samples and goose down samples washed 45 times in water from Examples 1-6, Comparative Examples 1-6, and the blank group were tested using a contact angle meter. Ten samples were tested in each group, and the average value of the results was recorded in Table 3 below, as shown in the details below: Table 3 Test data on the waterproof and moisture-proof properties of goose down ; Experimental conclusions: Based on the analysis in Table 3, it is known that the pretreatment steps for goose down (including micro-etching treatment of goose down with thiourea and sodium dodecyl sulfate aqueous solution, and enzymatic hydrolysis treatment of goose down with a specific combination of enzyme preparations) are prerequisites for the subsequent ultrasonic dispersion and adsorption of modified biomass activated carbon containing aqueous polyurethane solution. This enhances the adhesion and durability of activated carbon particles to goose down fibers. Furthermore, the preparation of a membrane layer with dopamine hydrochloride as the main component on goose down with modified biomass activated carbon (containing aqueous polyurethane solution) exhibits strong water wash resistance, and the goose down retains high hydrophobicity even after multiple water washes.

[0039] (3) Antibacterial performance test Antimicrobial performance testing: The antimicrobial performance of unwashed goose down samples and goose down samples washed 45 times were tested according to the experimental methods in GB / T20944.2-2007 "Evaluation of antimicrobial properties of textiles - Part 2: Absorption method". The test bacteria used were Gram-negative bacteria (Klebsiella pneumoniae ATCC4352). The antimicrobial tests were conducted according to the standard specifications, and the test results are recorded in Table 4 below. Table 4. Test data on the antibacterial properties of goose down ; Experimental conclusion: As shown in Table 4, the material prepared by the method of the present invention has both high fluffiness and strong hydrophobicity, and can also maintain a long-lasting antibacterial effect. This indicates that the film structure formed on the surface of the goose down has strong stability and is not easy to fall off.

[0040] The above embodiments merely illustrate several implementation methods of the present invention, and their descriptions are relatively specific and detailed, but they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention.

Claims

1. A process for the production of a high loft hydrophobic goose down, characterized in that: Specifically comprising the following steps: Step one: soak the goose down in a glutaraldehyde solution, then add enzyme preparation, incubate and stand for enzymatic hydrolysis, then inactivate, wash, dry, and obtain the pretreated down; Step two: modify the biomass activated carbon with 3-aminopropyl triethoxysilane to obtain modified biomass activated carbon, adsorb the aqueous polyurethane solution with the modified biomass activated carbon, low-temperature baking, and then disperse into the pretreated down through ultrasonic; Step three: mix a plurality of raw materials to obtain a film solution, the preparation raw materials of the film solution, by weight, include dopamine hydrochloride 5-10 parts, glycerol triglycidyl ether 4-6 parts, m-xylylenediamine 1-3 parts, nano silicon dioxide 0.1-2 parts, lithium chloride 0.1-1 part, ethanol 8-12 parts, and deionized water 70-80 parts, form a film layer on the surface of the goose down treated in step two by electrostatic atomization-deposition method, and obtain high-loft hydrophobic goose down after solidification treatment.

2. A process for the production of a high loft hydrophobic goose down according to claim 1, characterized in that: In step one, the mass ratio of the goose down to 2-6wt% glutaraldehyde solution is 1:10-20; The enzyme preparation is glutamine transaminase and / or tyrosinase, and the dosage of the enzyme preparation is 15-45g / kg goose down.

3. A process for making a high loft hydrophobic goose down according to claim 1, characterized in that: In step one, the incubation and soaking is specifically adjusting the pH to 7-8, and incubating and soaking at 50-60℃ for 50-80min; The incubation and standing is specifically incubating and standing at 40-50℃ for 1-3h.

4. The method of claim 1, wherein the high loft hydrophobic goose down is prepared by the steps of: In step one, before soaking the goose down in the glutaraldehyde solution, the goose down is also subjected to micro-etching treatment with 4-8wt% thiourea and 0.5-2wt% sodium dodecyl sulfate aqueous solution, the bath ratio is 1:5-8, and the stirring speed is 25-40r / min for 10-15h.

5. The method for preparing high-loft hydrophobic goose down according to claim 1, characterized in that: In step two, the modification treatment is specifically preparing a 2-5wt% 3-aminopropyl triethoxysilane solution with ethanol as the solvent, soaking the biomass activated carbon in the solution after heating to 70-80℃ for 30-50min, and obtaining the modified biomass activated carbon after centrifugation and drying; The mass ratio of the biomass activated carbon to the 2-5wt% 3-aminopropyl triethoxysilane solution is 1:5-7.

6. A process for making a high loft hydrophobic goose down according to claim 1, characterized in that: In step two, the mass ratio of the modified biomass activated carbon to 12-20wt% aqueous polyurethane solution is 7-10:1; The low-temperature baking is specifically baking at 28-35℃ for 20-40min; The mass ratio of the modified biomass activated carbon to the pretreated down is 3-7:1; The ultrasonic dispersion is specifically at a frequency of 45-60KHz, a power of 300-500W, a time of 12-18min, and a temperature of 65-80℃.

7. A process for making a high loft hydrophobic goose down according to claim 1, characterized in that: In step three, the electrostatic atomization deposition method is used to form a 10-15nm film layer on the surface of the goose down, which is specifically that the rotating speed of the cage containing the goose down is 15-20r / min, the voltage of the spray head is 24-28kV, the distance between the spray head and the down layer is 10-15cm, the pH of the film solution is 7.5-8.5, the flow rate of the film solution is 0.5-2mL / min, and the atomization particle size is 25-32µm.

8. A process for making a high loft hydrophobic goose down according to claim 1, characterized in that: In step three, the temperature of the solidification treatment is 65-80°C, and the time is 35-60 min.

9. A high loft hydrophobic goose down characterized in that: The method is prepared by any one of claims 1-8.