Antibacterial waterproof down feather and processing method thereof

Abstract

The application relates to an antibacterial waterproof down feather and a processing method thereof, in particular to the down feather processing technology field, and the processing method of the antibacterial waterproof down feather comprises the following steps: (1) using a degreasing agent to perform degreasing treatment on the down feather; (2) performing normal-pressure plasma treatment on the down feather subjected to the degreasing treatment in the step (1); (3) mixing the down feather subjected to the normal-pressure plasma treatment in the step (2) with a bacteriostatic finishing emulsion, water and tyrosinase to perform bacteriostatic waterproof finishing, the bacteriostatic finishing emulsion is a phosphatized pea protein emulsion loaded with bacteriostatic essential oil; and (4) performing hot air drying on the down feather subjected to the bacteriostatic waterproof finishing in the step (3) to obtain the antibacterial waterproof down feather. The down feather obtained through the processing method has the advantages of persistent antibacterial property, further improved waterproof performance, good fluffiness and excellent comprehensive performance.

Description

Technical Field

[0001] The invention belongs to the technical field of down processing, and particularly relates to antibacterial and waterproof down and a processing method thereof. Background Art

[0002] Down fiber is a natural biomass material with the characteristics of light texture, fluffy and soft, and strong warmth retention. It is currently the most ideal thermal insulation material for thermal insulation performance. However, down has a high moisture regain and easily absorbs moisture from the surrounding environment. When down absorbs a large amount of water and becomes wet, its fluffy structure will be severely damaged, the thermal resistance of the down and the aggregate will be significantly reduced, the heat transfer coefficient will increase rapidly, and heat loss will be significant, affecting the normal warmth retention performance of the down. Therefore, the waterproof and water repellent properties of down should also be enhanced during processing;

[0003] Furthermore, because down inherently has an odor and is derived from animals, its antibacterial properties are relatively low, necessitating further antibacterial finishing. Existing antibacterial treatments for down often involve padding the down with an antibacterial finishing solution. This treatment method reduces the antibacterial properties of the down with increasing wash frequency, failing to effectively maintain its long-term antibacterial properties. Furthermore, the use of industrial antibacterial finishing agents can also degrade the down's performance, making it unsuitable for use. Summary of the Invention

[0004] The purpose of the present invention is to provide an antibacterial and waterproof down and a processing method thereof in order to solve the above problems.

[0005] The present invention achieves the above-mentioned purpose through the following technical solutions:

[0006] As a first aspect of the present invention, the present invention provides a method for processing antibacterial and waterproof down, comprising the following steps:

[0007] (1) Degreasing the down using a degreasing agent;

[0008] (2) subjecting the down degreased in step (1) to atmospheric pressure plasma treatment;

[0009] (3) mixing the down treated with normal pressure plasma in step (2) with an antibacterial finishing emulsion, water, and tyrosinase to perform an antibacterial and waterproof finishing, wherein the antibacterial finishing emulsion is a phosphorylated pea protein emulsion loaded with antibacterial essential oil;

[0010] (4) The antibacterial and waterproof down obtained by the antibacterial and waterproof finishing in step (3) is dried with hot air to obtain the antibacterial and waterproof down.

[0011] As a further optimization scheme of the present invention, in step (1), the specific steps of the degreasing treatment are: adding down to water and adding a degreasing agent for degreasing treatment, the mass ratio of down to water is 1:40-50, the amount of degreasing agent to water is 2-4g:1L, the degreasing temperature is 40-45°C, and the degreasing time is 30-60min.

[0012] As a further optimization scheme of the present invention, in step (2), the specific steps of the atmospheric pressure plasma treatment are: placing the down in a plasma generator, the distance between the plasma nozzle and the down is 5-10 cm, the frequency is 15-20 kHz, the moving speed is 3-5 m / min, the gas flow rate is 600-800 L / min, the voltage is 220-260 V, the duty cycle is 40-50%, and the working gas is oxygen.

[0013] As a further optimization scheme of the present invention, in step (3), the mass ratio of the antibacterial finishing emulsion, down and water is 20-40:1:30-50, the amount of tyrosinase is 0.8-1.2 g / L, the reaction temperature is 40-50°C, and the reaction time is 60-90 min.

[0014] As a further optimized solution of the present invention, in step (3), the method for preparing the phosphorylated pea protein emulsion loaded with antibacterial essential oil is as follows: dissolving the phosphorylated pea protein in ethanol at room temperature, removing the precipitate by centrifugation to obtain a supernatant, adding the supernatant dropwise to distilled water to obtain a mixed solution, treating the mixed solution with ultrasound, concentrating it by rotary evaporation, and then mixing and dispersing it uniformly with the antibacterial essential oil in a volume ratio of 6-10:1 to obtain the phosphorylated pea protein emulsion loaded with antibacterial essential oil.

[0015] As a further optimized solution of the present invention, the antibacterial essential oil is one of tea tree essential oil, oregano essential oil or cinnamon essential oil.

[0016] As a second aspect of the present invention, there is also provided an antibacterial and waterproof down, which is prepared by any of the above-mentioned processing methods.

[0017] The beneficial effects of the present invention are:

[0018] (1) The present invention first degreases the down raw materials to remove excess oil on the surface of the down fibers, and then uses atmospheric pressure plasma to treat the down jacket. This not only removes bacteria and pathogens carried by the down itself and improves its antibacterial properties, but also modifies the surface of the down and promotes the grafting effect of the subsequent antibacterial finishing emulsion. At the same time, it can also promote the straightening of the down fiber molecules, increase the compression resistance of the down fiber, and further improve the fluffiness of the down fiber.

[0019] (2) The antibacterial finishing emulsion provided by the present invention is a phosphorylated pea protein down loaded with antibacterial essential oil composed of plant ingredients. Compared with industrial antibacterial finishing agents, it is less likely to cause damage to down fibers and is more environmentally friendly. In addition, the pea protein is phosphorylated to enhance its own hydrophobicity, which can promote the further improvement of the waterproof performance of the down treated with the antibacterial finishing liquid. DETAILED DESCRIPTION

[0020] The present application is described in further detail below. It is necessary to point out that the following specific implementation methods are only used to further illustrate the present application and cannot be understood as limiting the scope of protection of the present application. Technicians in this field can make some non-essential improvements and adjustments to the present application based on the above application content.

[0021] 1. Materials and Methods

[0022] The degreasing agent was dodecyl betaine (BS-12), purchased from Errek (Shandong) Chemical Group Co., Ltd.;

[0023] Pea protein, extracted by alkali dissolution and acid precipitation, 89.80 ± 0.20%), was purchased from Xi'an Qianyecao Biotechnology Co., Ltd.

[0024] Tyrosinase was purchased from Hefei Bomei Biotechnology Co., Ltd. (enzyme activity was 1100 U / mg);

[0025] Tea tree essential oil, oregano essential oil, and cinnamon essential oil were purchased from Hubei Xinyuhong Biopharmaceutical Technology Co., Ltd.;

[0026] In the following examples, any method not specified may be carried out according to conventional methods, and the materials and reagents used may be obtained through commercial channels unless otherwise specified.

[0027] 2. Specific Examples

[0028] Example 1

[0029] This embodiment provides an antibacterial and waterproof down and a processing method thereof, comprising the following steps:

[0030] (1) Add down to water and add degreasing agent for degreasing treatment. The mass ratio of down to water is 1:40, the amount of degreasing agent to water is 2g:1L, the degreasing temperature is 40℃, and the degreasing time is 30min.

[0031] (2) performing atmospheric pressure plasma treatment on the down degreased in step (1), specifically, placing the down in a plasma generator with a distance of 5 cm between the plasma nozzle and the down, a frequency of 20 kHz, a moving speed of 5 m / min, a gas flow rate of 600 L / min, a voltage of 220 V, a duty cycle of 50%, and oxygen as the working gas;

[0032] (3) Preparation of antibacterial finishing emulsion: 30g pea protein and 800mL 0.1mol / L pH 8.0 phosphate buffer, magnetic stirring for 3h. Add a certain amount of sodium tripolyphosphate, dilute to 1000mL with buffer, adjust the pH value with 1mol / L NaOH and 1mol / L HCl solution, and stabilize the reaction pH at a certain value. After reacting in a constant temperature water bath oscillator for a certain period of time, adjust the pH of the reaction solution to 4.5, magnetically stir for 30min, centrifuge, wash the precipitate 3 times, adjust the pH of the precipitated pea protein to 7.0, transfer the resulting solution to a dialysis bag, dialyze for 72h, and finally freeze-dry it, crush it, and pass it through an 80-mesh sieve;

[0033] Then, 20 g of phosphorylated pea protein was dissolved in 400 ml of 85% ethanol by volume at room temperature, and the precipitate was removed by centrifugation at 5000 g for 10 min to obtain a supernatant. The supernatant was added dropwise to 1200 ml of distilled water to obtain a mixed solution. The mixed solution was treated with ultrasound (500 W) for 10 min and then concentrated by rotary evaporation until the total volume was reduced to 600 ml. The mixed solution was then mixed and uniformly dispersed with antibacterial essential oil in a volume ratio of 6:1 to obtain a phosphorylated pea protein emulsion loaded with antibacterial essential oil, wherein the antibacterial essential oil was oregano essential oil.

[0034] (4) mixing the down treated with normal pressure plasma in step (2) with an antibacterial finishing emulsion, water, and tyrosinase for antibacterial and waterproof finishing, wherein the antibacterial finishing emulsion is a phosphorylated pea protein emulsion loaded with antibacterial essential oil, the mass ratio of the antibacterial finishing emulsion, down, and water is 40:1:50, the amount of tyrosinase is 1.2 g / L, the reaction temperature is 50° C., and the reaction time is 60 min;

[0035] (5) The down treated in step (4) is dried with hot air at a wind speed of 3 m / s and a drying temperature of 50°C.

[0036] Example 2

[0037] This embodiment provides a method for processing antibacterial and waterproof down, comprising the following steps:

[0038] (1) Degreasing treatment is the same as in Example 1;

[0039] (2) performing atmospheric pressure plasma treatment on the down degreased in step (1), specifically, placing the down in a plasma generator with a distance of 10 cm between the plasma nozzle and the down, a frequency of 15 kHz, a moving speed of 3 m / min, a gas flow rate of 800 L / min, a voltage of 260 V, a duty cycle of 40%, and oxygen as the working gas;

[0040] (3) Preparation method of antibacterial finishing emulsion The same as in Example 1 except that tea tree essential oil is selected as the antibacterial essential oil and the volume ratio of the mixed liquid to the tea tree essential oil is 10:1;

[0041] (4) mixing the down treated with atmospheric pressure plasma in step (2) with an antibacterial finishing emulsion, water, and tyrosinase for antibacterial and waterproof finishing, wherein the antibacterial finishing emulsion is a phosphorylated pea protein emulsion loaded with antibacterial essential oil, the mass ratio of the antibacterial finishing emulsion, down, and water is 20:1:30, the amount of tyrosinase is 0.8 g / L, the reaction temperature is 40° C., and the reaction time is 90 min;

[0042] (5) The hot air drying step is the same as in Example 1.

[0043] Example 3

[0044] This embodiment provides a method for processing antibacterial and waterproof down, comprising the following steps:

[0045] (1) Degreasing treatment is the same as in Example 1;

[0046] (2) Atmospheric pressure plasma treatment is the same as in Example 1;

[0047] (3) Preparation of antibacterial finishing emulsion: The antibacterial essential oil is cinnamon essential oil, and the volume ratio of the mixed liquid to tea tree essential oil is 8:1. Other aspects are the same as in Example 1.

[0048] (4) mixing the down treated with normal pressure plasma in step (2) with an antibacterial finishing emulsion, water, and tyrosinase for antibacterial and waterproof finishing, wherein the antibacterial finishing emulsion is a phosphorylated pea protein emulsion loaded with antibacterial essential oil, the mass ratio of the antibacterial finishing emulsion, down, and water is 30:1:40, the amount of tyrosinase is 1 g / L, the reaction temperature is 45° C., and the reaction time is 75 min;

[0049] (5) The hot air drying step is the same as in Example 1.

[0050] Comparative Example 1

[0051] This comparative example provides a method for processing antibacterial and waterproof down. Except for not performing step (2), the remaining steps are the same as those in Example 1.

[0052] Comparative Example 2

[0053] This comparative example provides a method for processing antibacterial and waterproof down. In step (3), the pea protein is not phosphorylated in the preparation of the antibacterial finishing emulsion. 20 g of pea protein is dissolved in 400 ml of 85% ethanol by volume at room temperature, centrifuged at 5000 g for 10 min to remove the precipitate, and a supernatant is obtained. The supernatant is added dropwise to 1200 ml of distilled water to obtain a mixed solution. The mixed solution is subjected to ultrasonic treatment (500 W) for 10 min and then concentrated by rotary evaporation until the total volume is reduced to 600 ml. The mixed solution is then mixed and uniformly dispersed with an antibacterial essential oil in a volume ratio of 6:1 to obtain a phosphorylated pea protein emulsion loaded with an antibacterial essential oil, wherein the antibacterial essential oil is oregano essential oil. The remaining steps are the same as those in Example 1.

[0054] Comparative Example 3

[0055] This comparative example provides a method for processing antibacterial and waterproof down. In step (3), in the preparation of the antibacterial finishing emulsion, soybean alcohol-soluble protein is used instead of phosphorylated pea protein. 20 g of soybean alcohol-soluble protein is dissolved in 400 ml of 85% ethanol by volume at room temperature, and the supernatant is removed by centrifugation at 5000 g for 10 min to obtain a supernatant. The supernatant is added dropwise to 1200 ml of distilled water to obtain a mixed solution. The mixed solution is subjected to ultrasonic treatment (500 W) for 10 min and then concentrated by rotary evaporation until the total volume is reduced to 600 ml. The mixed solution is then mixed and uniformly dispersed with an antibacterial essential oil in a volume ratio of 6:1 to obtain a phosphorylated pea protein emulsion loaded with an antibacterial essential oil, wherein the antibacterial essential oil is oregano essential oil. The remaining steps are the same as those in Example 1.

[0056] Comparative Example 4

[0057] This comparative example provides a method for processing antibacterial and waterproof down. The method comprises the following steps: except that in step (4), the down treated with atmospheric pressure plasma in step (2) is mixed with an antibacterial finishing emulsion and water for antibacterial and waterproof finishing. The antibacterial finishing emulsion is a phosphorylated pea protein emulsion loaded with an antibacterial essential oil. The mass ratio of the antibacterial finishing emulsion, down, and water is 40:1:50. The reaction temperature is 50° C., and the reaction time is 60 minutes. The remaining steps are the same as those in Example 1.

[0058] Comparative Example 5

[0059] This comparative example provides a method for processing antibacterial and waterproof down, except that in step (2), the degreased down is oxidized using an oxidant, the degreased down is added to water and an oxidant (hydrogen peroxide) is added, the mass ratio of down to water is 1:30, the amount ratio of oxidant to water is 1g:1L, the oxidation temperature is 30°C, and the oxidation time is 40min.

[0060] Comparative Example 6

[0061] This comparative example provides a method for processing antibacterial and waterproof down. Except for step (4), in which the down treated with atmospheric pressure plasma in step (2) is mixed with a commercially available down antibacterial finishing agent AGS-YR001 and water for antibacterial and waterproof finishing, the mass ratio of the down antibacterial finishing agent, down, and water is 40:1:50, and the remaining steps are the same as those in Example 1.

[0062] Verification test

[0063] 1. Antibacterial properties of down obtained by processing in Examples 1-3 and Comparative Examples 1-6 were tested:

[0064] (1) Determination of antibacterial properties: According to GB / T 20944.2-2007 "Evaluation of antibacterial properties of textiles Part 2: Absorption method", the test bacteria are Escherichia coli 8099 (Gram-negative bacteria) and Staphylococcus aureus ATCC6538. According to the standard, each fabric sample was cut into 20mm×20mm size, and the antibacterial test was carried out after 0 and 50 washings. The down washing method is: 1g down is immersed in 500mL distilled water, shaken and washed at 40℃, and washed every 15 minutes.

[0065] The results are shown in Table 1.

[0066] Table 1. Down performance test results

[0067]

[0068] As can be seen from Table 1, the down treated by the processing methods disclosed in Examples 1-3 has better antibacterial properties than the down obtained by the other comparative examples.

[0069] Comparative Example 1 was not subjected to normal pressure plasma treatment compared to Example 1. From the antibacterial results, Comparative Example 1 is inferior to Example 1. The reason is that normal pressure plasma treatment can further remove bacteria and molds carried by the down itself while modifying the surface of the down to produce free radicals, so that active centers are formed on the surface of the down, which is helpful for the subsequent grafting effect of the antibacterial finishing emulsion with antibacterial effect. The present application subsequently tests the grafting amount of the down obtained in Comparative Example 1 and Example 1, and uses the weight gain to evaluate the grafting rate on the antibacterial finishing emulsion down. The greater the weight gain, the higher the grafting rate. The down obtained in Example 1 and the down treated in steps (1)-(2) of Example 1 were dried at 65°C for 30 minutes, and weighed after cooling. The down obtained in Comparative Example 1 and the down treated in step (1) of Comparative Example 1 were dried at 65°C for 30 minutes, respectively;

[0070] The calculation formula is as follows: Wherein, m1 is the dry weight of down after processing in steps (1)-(2), g; m2 is the dry weight of down finally obtained, g,

[0071] Since comparative example 1 was not subjected to plasma treatment, m1 of comparative example 1 is the dry weight of the down after treatment in step (1). After testing, the weight gain of the down in comparative example 1 was 13.43 mg / g, while that in embodiment 1 was 20.21 mg / g.

[0072] Compared with Example 1, Comparative Example 4 does not use tyrosinase. Tyrosinase promotes the cross-linking of the phosphorylated pea protein emulsion loaded with antibacterial essential oil and the fiber molecules, which helps to improve the grafting effect of the phosphorylated pea protein emulsion loaded with antibacterial essential oil on the surface of the down jacket fiber. From the antibacterial results, Comparative Example 4 is inferior to Example 1. Subsequently, Comparative Example 4 was also tested for down weight gain, and the result was 11.68 mg / g.

[0073] Comparative Example 5 uses oxidation treatment instead of the atmospheric pressure plasma treatment in Example 1. Both are methods for modifying the surface of down. From the results, the effect of atmospheric pressure plasma treatment in improving the antibacterial properties of down is better than that of oxidant treatment.

[0074] 2. The down processed in Examples 1-3 and Comparative Examples 1-6 was subjected to fill power measurement. A 20g sample was taken from each group and dried at 70°C. After 45 minutes, the sample was manually shaken and placed in a pre-treatment chamber to fully fluff the sample. The sample was then allowed to stand for 24 hours at 20°C and 65% relative humidity. Accurately weigh 18g of the sample from the pre-treatment chamber and gently transfer it to a national standard fill power meter. Gently stir the sample with a glass rod. Cover the sample with an aluminum pressure plate, gently press the plate against the sample, and allow it to fall naturally. After the plate stops falling, let it rest for 1 minute. The scale marks on both sides of the fill power meter wall were recorded. The test was repeated five times, and the average value was taken. The results are shown in Table 2.

[0075] Table 2. Down performance test results

[0076]

[0077]

[0078] It can be seen from Table 2 that the down processed by the processing methods disclosed in Examples 1-3 has better fluffiness than that processed by other comparative examples.

[0079] Compared to Example 1, which did not undergo atmospheric pressure plasma treatment, the down of Comparative Example 1 had a lower fluffiness than Example 1. This is because atmospheric pressure plasma treatment can straighten down fiber molecules, increasing the down fiber's resistance to compression, and thus improving the fluffiness of the down to a certain extent. Comparative Example 5 achieved a similar effect in improving the fluffiness of down as Example 1. The oxidant treatment of down can destroy the cell membrane composed of sterols and trisphosphates on the surface of the down fiber. When the oxidant penetrates further into the protein structure, it breaks the disulfide bonds between some of the down fibers, weakening the original intermolecular attraction and straightening the originally curved molecular chains in the protein structure, thereby improving the fluffiness of the down.

[0080] Compared with Example 1, in which tyrosinase was not used, the down fluffiness of Comparative Example 4 was lower than that of Example 1. The reason is that tyrosinase can catalyze the enzymatic cross-linking reaction between down protein fibers, thereby increasing the degree of cross-linking between fiber molecules and promoting the improvement of the compression resistance of the down fibers.

[0081] 3. The down obtained by processing in Examples 1-3 and Comparative Examples 1-6 was subjected to hydrophobicity testing. The surface contact angle of the down was measured using a contact angle tester. Ten samples were tested in each group, and the average results were taken. The results are shown in Table 3.

[0082] Table 3. Down performance test results

[0083]

[0084] As can be seen from Table 2, the water repellency of the down processed using the processing methods disclosed in Examples 1-3 is better than that of the other comparative examples. Compared with Example 1, the pea protein used in Comparative Example 2 was not phosphorylated, and the water repellency of the down processed was inferior to that of Example 1. This is because the surface hydrophobicity of the pea protein obtained through phosphorylation is enhanced. When the antibacterial finishing emulsion is subsequently grafted onto the down surface, the hydrophobicity of the pea protein surface can be used to relatively increase the water repellency of the down surface. Comparative Example 4 differs from Example 1 in that it does not use old protease. As shown in the above tests, the grafting effect of the antibacterial finishing emulsion is not as good as that of Example 1, resulting in relatively poorer surface water repellency. Comparative Example 5 uses an oxidant treatment instead of the atmospheric pressure plasma treatment of Example 1. The oxidant treatment mainly improves the fluffiness of the down, but its effect on promoting water repellency is not as good as that of Example 1.

[0085] The above-described embodiments merely illustrate several implementations of the present invention. While the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that a person skilled in the art would be able to make numerous variations and improvements without departing from the spirit of the present invention, and all such variations and improvements fall within the scope of protection of the present invention.

Claims

1. A method for processing antibacterial and waterproof down, characterized by: The following steps are involved: (1) Degreasing the down using a degreasing agent; (2) treating the down degreased in step (1) with atmospheric pressure plasma; (3) The down treated with normal pressure plasma in step (2) is mixed with an antibacterial finishing emulsion, water, and tyrosinase for antibacterial and waterproof finishing, wherein the antibacterial finishing emulsion is a phosphorylated pea protein emulsion loaded with antibacterial essential oil. The preparation method of the phosphorylated pea protein emulsion loaded with antibacterial essential oil is as follows: dissolving the phosphorylated pea protein in ethanol at room temperature, removing the precipitate by centrifugation to obtain a supernatant, adding the supernatant dropwise to distilled water to obtain a mixed solution, treating the mixed solution with ultrasound, concentrating it by rotary evaporation, and then uniformly mixing and dispersing it with the antibacterial essential oil in a volume ratio of 6-10:1 to obtain the phosphorylated pea protein emulsion loaded with antibacterial essential oil; (4) The antibacterial and waterproof down obtained by the antibacterial and waterproof finishing in step (3) is dried with hot air to obtain the antibacterial and waterproof down.

2. The method for processing antibacterial and waterproof down according to claim 1, characterized in that: In step (1), the specific steps of the degreasing treatment are: adding down to water and adding a degreasing agent for degreasing treatment, the mass ratio of down to water is 1:40-50, the amount of degreasing agent to water is 2-4g:1L, the degreasing temperature is 40-45°C, and the degreasing time is 30-60min.

3. The method for processing antibacterial and waterproof down according to claim 1, characterized in that: In step (2), the specific steps of the atmospheric pressure plasma treatment are: placing the down in a plasma generator, the distance between the plasma nozzle and the down is 5-10 cm, the frequency is 15-20 kHz, the moving speed is 3-5 m / min, the gas flow rate is 600-800 L / min, the voltage is 220-260 V, the duty cycle is 40-50%, and the working gas is oxygen.

4. The method for processing antibacterial and waterproof down according to claim 1, characterized in that: In step (3), the mass ratio of the antibacterial finishing emulsion, down and water is 20-40:1:30-50, the amount of tyrosinase used is 0.8-1.2 g / L, the reaction temperature is 40-50° C., and the reaction time is 60-90 min.

5. The method for processing antibacterial and waterproof down according to claim 1, characterized in that: The antibacterial essential oil is one of tea tree essential oil, oregano essential oil or cinnamon essential oil. 6.An antibacterial and waterproof down, characterized by: The invention is prepared by the processing method according to any one of claims 1 to 5.

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