A hemp fiber antibacterial non-woven fabric and a preparation method thereof

By using ultrasonic microwave enzymatic hydrolysis and antibacterial microcapsule finishing, the problems of poor water absorption and insufficient antibacterial ability of hemp fiber were solved, and a soft and highly effective antibacterial all-hemp fiber nonwoven fabric was prepared.

CN117569003BActive Publication Date: 2025-12-30TIANZHICAO BIOPHARMACEUTICAL (HUNAN) CO LTD
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Patent Information

Application Number
CN202311473849.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-11-08
Publication Date
2025-12-30
Estimated Expiration
2043-11-08

AI Technical Summary

Technical Problem

Existing hemp fiber has poor water absorption, a hard texture, and insufficient antibacterial ability.

Method used

Cottonized hemp fiber was prepared by removing pectin and lignin from the fiber through ultrasonic microwave enzymatic hydrolysis. Hemp antibacterial microcapsules were then combined with carboxyl hemp fiber for antibacterial finishing to prepare all-hemp fiber antibacterial nonwoven fabric.

Benefits of technology

It improves the water absorption and antibacterial properties of hemp fiber, enhances the softness and antibacterial effect of nonwoven fabric, and reduces environmental damage.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a full-Hemp fiber antibacterial non-woven fabric and a preparation method thereof in the technical field of non-woven fabrics, and comprises the following components in parts by weight: cottonized Hemp fiber 35-40 parts, Hemp antibacterial microcapsules 2-5 parts, and double-carboxyl Hemp fiber 18-23 parts; the cottonized Hemp fiber is obtained by ultrasonic microwave-assisted enzymolysis of Hemp fiber; the Hemp antibacterial microcapsules are microcapsules obtained by coating gelatin-polylysine on acetic ether-extracted Hemp bast fiber and alcohol-extracted Hemp core; and the double-carboxyl Hemp fiber is obtained by reacting sodium periodate-oxidized cottonized Hemp fiber with sodium chlorite. The application realizes the removal of pectin lignin and hemicellulose by ultrasonic microwave and enzymolysis, and further realizes the softening of Hemp fiber and the improvement of water absorption performance of the Hemp fiber. Meanwhile, the Hemp antibacterial microcapsules are prepared and loaded on the carboxyl-modified fiber, so that the water absorption performance of the Hemp fiber is further improved and the antibacterial capacity is enhanced.
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Description

Technical Field

[0001] This invention belongs to the field of nonwoven fabric technology, specifically referring to a whole hemp fiber antibacterial nonwoven fabric and its preparation method. Background Technology

[0002] Hemp is a resource-rich, renewable, and environmentally friendly raw material. Hemp fiber is one of the earliest textile raw materials used by mankind. It is a natural cellulose fiber, and its unique physical structure and chemical properties have extremely high research and application value, often used in various research and development methods. Hemp fiber products have many properties such as moisture absorption, breathability, heat resistance, antibacterial properties, UV protection, radiation protection, sound absorption, and no itching sensation. Furthermore, it can degrade in the natural environment, making it a multifunctional environmentally friendly material. Hemp single fibers are very short, generally 12-25mm, with a large amount of gum attached to the surface, and the fiber species have a high content of lignin and... Hemp fibers, currently mainly degummed using chemical methods such as alkaline boiling, are then combined with cotton fibers to prepare hemp / cotton blended products. Hemp fibers have a loose structure and many pores, providing good air permeability and inhibiting the growth of anaerobic bacteria. The single fibers are tubular with a rough surface, containing numerous capillary channels connected to the lumen, as well as a large number of hydroxyl groups, enabling them to absorb and wick away moisture. Nonwoven fabric is a type of non-woven material that is formed by directly using polymer chips, short fibers, or filaments to form a web through airflow or mechanical means, followed by hydroentangling, needle punching, or hot rolling reinforcement, and finally finishing processes to create a non-woven fabric.

[0003] The existing technology currently has the following main problems: the commonly used hemp fiber has poor water absorption, a hard texture, and insufficient antibacterial ability. Summary of the Invention

[0004] To address the above issues and overcome the shortcomings of existing technologies, this invention provides an antibacterial nonwoven fabric made entirely of hemp fiber and its preparation method. To solve the problems of poor water absorption and hard texture of hemp fiber, this invention proposes a method involving ultrasonic and microwave enzymatic hydrolysis to remove pectin, lignin, and hemicellulose, thereby softening the hemp fiber and improving its water absorption. Simultaneously, hemp antibacterial microcapsules are prepared and loaded onto carboxyl-modified fibers, further enhancing the water absorption and antibacterial properties of the hemp fiber.

[0005] To achieve the above objectives, the technical solution adopted by the present invention is as follows: The present invention proposes a whole hemp fiber antibacterial nonwoven fabric and its preparation method. The whole hemp fiber antibacterial nonwoven fabric comprises the following components in parts by weight: 35-40 parts of cottonized hemp fiber, 2-5 parts of hemp antibacterial microcapsules, and 18-23 parts of dicarboxylated hemp fiber; the cottonized hemp fiber is obtained by enzymatic hydrolysis of hemp fiber using ultrasound and microwave assistance; the hemp antibacterial microcapsules are microcapsules obtained from the alcohol extract of hemp bast fiber and hemp stalk core extracted with ethyl acetate coated with gelatin-polylysine; the dicarboxylated hemp fiber is obtained by reacting cottonized hemp fiber with sodium periodate after oxidation.

[0006] Preferably, the cottonized hemp fiber comprises the following components in parts by weight: 50-60 parts hemp fiber, 1.2-1.6 parts fruit enzyme, 0.6-0.8 parts laccase, and 0.5-0.7 parts hemicellulase.

[0007] Preferably, the hemp antibacterial microcapsules comprise the following components in parts by weight: 60-80 parts hemp bast fiber, 50-65 parts hemp stalk core, 5-7 parts gelatin, and 3-6 parts polylysine.

[0008] Preferably, the preparation method of the cottonized hemp fiber specifically includes the following steps:

[0009] (1) Add hemp fiber to water at a dosage of 1.2-3 g / mL and soak for 2-3 hours. Then, treat it with an ultrasonic frequency of 40-50 kHz, a microwave power of 200-300 w, and a temperature of 45-55 °C for 30 minutes. Filter and dry to obtain pretreated hemp.

[0010] (2) The pretreated hemp obtained in step (1) was added to water at an addition rate of 0.9-1.5 g / mL, followed by the addition of fruit enzyme, laccase and hemicellulase to obtain a mixture;

[0011] (3) The mixture obtained in step (1) is stirred in a water bath at 35-45℃ for 100-150 min at a speed of 30-60 rpm to obtain the enzymatic hydrolysate. The hydrolysate is then washed 3-5 times with filtered water and dried to obtain cotton-like hemp fiber.

[0012] Preferably, the preparation method of the hemp antibacterial microcapsules specifically includes the following steps:

[0013] 1. Take hemp bast fibers and hemp stalk cores, remove impurities, wash, filter, dry, and pulverize through an 80-mesh sieve to obtain a mixed powder;

[0014] 2. Add the mixed powder to anhydrous ethanol at a rate of 0.05-0.06 g / mL, heat and stir at 60-80°C at a speed of 400-500 rpm, filter and evaporate to obtain the initial extract, extract the initial extract with ethyl acetate and rotary evaporate to obtain the saturated extract.

[0015] 3. Mix gelatin and polylysine, dissolve in water at 0.02-0.03 g / mL to obtain an aqueous phase, add the extract obtained in step 2 to the aqueous phase at 0.01-0.03 g / mL, emulsify in a 40℃ constant temperature water bath at 1500 r / min for 15 min, and use glutaraldehyde with a mass concentration of 22% as a curing agent to obtain hemp antibacterial microcapsules.

[0016] Preferably, the preparation method of the dicarboxylated hemp fiber specifically includes the following steps:

[0017] S1. Add cotton-like hemp fiber to a sodium periodate solution with a mass concentration of 3-5% at an addition amount of 0.13-0.21 g / mL, and keep it at 20-35℃ for 50-80 min under light-protected conditions. Filter to obtain oxidized hemp fiber.

[0018] S2. The oxidized hemp fiber obtained in S1 was added to a glycerol solution with a mass concentration of 2.5-3.5% at an addition amount of 0.09-0.16 g / mL, stirred at 30-60 rpm for 40 min, washed three times with deionized water, and dried in an oven at 80℃ for 2 h to obtain aldehyde-modified hemp fiber.

[0019] S3. The aldehyde-modified hemp fiber obtained in S2 is added to a sodium chlorite solution with a mass concentration of 3.2-4% at an addition amount of 0.23-0.35 g / mL. The mixture is stirred at 30-50 rpm for 8-12 h, filtered, washed and dried to obtain dicarboxylated hemp fiber.

[0020] Preferably, in S1, the amount of cottonized hemp fiber added to the sodium periodate solution is 0.13-0.21 g / mL.

[0021] Preferably, in S2, the amount of oxidized hemp fiber added to the glycerol solution is 0.09-0.16 g / mL.

[0022] Preferably, in step S3, the amount of aldehyde-modified hemp fiber added to the sodium chlorite solution is 0.23-0.35 g / mL.

[0023] This invention also provides a method for preparing an antibacterial nonwoven fabric made entirely of hemp fiber, specifically including the following steps:

[0024] Hemp antibacterial microcapsules were prepared as a 0.2-0.3 g / mL suspension and stirred evenly to obtain a finishing solution. Dicarboxylated hemp fibers and cottonized hemp fibers were used to prepare nonwoven fabric by hydroentangling and then immersed in the finishing solution. The fabric was dipped and nibbled twice, with a nibbling rate of 100%. It was then placed in a setting dryer and dried at 80°C for 3 min and at 160°C for 2 min. After cooling to room temperature, a whole hemp fiber antibacterial nonwoven fabric was obtained.

[0025] The beneficial effects of this invention are as follows: Pectin, lignin, and hemicellulose are removed from the fibers through ultrasonic microwave enzymatic hydrolysis, resulting in softer, more porous, and more absorbent cotton-like hemp fibers; using gelatin and polylysine as wall materials, hemp bast fibers and hemp stalk cores are extracted with alcohol and then with ethyl acetate to prepare hemp antibacterial microcapsules, exhibiting good antibacterial and antioxidant effects; oxidative modification of the cotton-like hemp fibers involves breaking the ortho-hydroxyl groups to obtain dialdehyde hemp fibers, which are further prepared using sodium chlorite to produce dicarboxylated hemp fibers. The fiber's water absorption is improved, and its texture is softer. Nonwoven fabric is prepared by hydroentangling cotton-like hemp fiber-dicarboxylated hemp fiber, and then functionally finished with hemp antibacterial microcapsules, which improves the antibacterial and bacteriostatic capabilities of the nonwoven fabric. At the same time, the microcapsules can be adsorbed onto the dicarboxylated hemp fiber by electrostatic interaction, increasing the nonwoven fabric's loading capacity for the extract and enhancing its antibacterial properties. By using environmentally friendly and renewable hemp fiber materials to prepare nonwoven fabric, the use of difficult-to-degrade synthetic organic macromolecules is reduced. Hemp fiber has good biodegradability, which can reduce environmental damage. Attached Figure Description

[0026] Figure 1 The results of antibacterial tests for Examples 1-3 and Comparative Examples 1-2 are shown in the figure.

[0027] Figure 2 The graph shows the results of water absorption tests for Examples 1-3 and Comparative Examples 2-3;

[0028] Figure 3 The graph shows the results of water retention rate tests for Examples 1-3 and Comparative Examples 2-3;

[0029] Figure 4 The results of the mite removal tests in Examples 1-3 and Comparative Examples 1-2 are shown in the figure.

[0030] Figure 5 This is a photograph of the antibacterial nonwoven fabric made of hemp fiber prepared in Example 1.

[0031] The accompanying drawings are provided to further illustrate the invention and form part of the specification. They are used together with the embodiments of the invention to explain the invention and do not constitute a limitation thereof. Detailed Implementation

[0032] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0033] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those familiar to those skilled in the art. Furthermore, any methods and materials similar to or equivalent to those described herein may be applied to this invention. The preferred embodiments and materials described herein are for illustrative purposes only and do not limit the scope of this application.

[0034] Unless otherwise specified, the experimental methods used in the following examples are conventional methods; unless otherwise specified, the experimental materials and test strains used in the following examples were purchased from commercial channels.

[0035] Example 1

[0036] A nonwoven fabric made entirely of hemp fiber antibacterial components comprises the following components in parts by weight: 40 parts of cottonized hemp fiber, 5 parts of hemp antibacterial microcapsules, and 23 parts of dicarboxylated hemp fiber.

[0037] The cotton-like hemp fiber comprises the following components in parts by weight: 60 parts hemp fiber, 1.6 parts fruit enzyme, 0.8 parts laccase, and 0.7 parts hemicellulase.

[0038] The hemp antibacterial microcapsules comprise the following components by weight: 80 parts hemp bast fiber, 65 parts hemp stalk core, 7 parts gelatin, and 6 parts polylysine.

[0039] The preparation method of cotton-like hemp fiber specifically includes the following steps:

[0040] (1) Add hemp fiber at a dosage of 3g / mL to water and soak for 3h. Then, treat it with an ultrasonic frequency of 50KHZ, a microwave power of 300w, and a temperature of 55℃ for 30min. Filter and dry to obtain pretreated hemp.

[0041] (2) The pretreated hemp obtained in step (1) was added to water at an addition rate of 1.5 g / mL, followed by the addition of fruit enzyme, laccase and hemicellulase to obtain a mixture;

[0042] (3) The mixture obtained in step (1) was stirred at 60 rpm in a 45°C water bath for 150 min to obtain the enzymatic hydrolysate. The hydrolysate was filtered, washed 5 times with water, and dried to obtain cotton-like hemp fiber.

[0043] The preparation method of hemp antibacterial microcapsules specifically includes the following steps:

[0044] 1. Take hemp bast fibers and hemp stalk cores, remove impurities, wash, filter, dry, and pulverize through an 80-mesh sieve to obtain a mixed powder;

[0045] 2. The mixed powder was added to anhydrous ethanol at a rate of 0.06 g / mL, heated and stirred at 80°C at 500 rpm, filtered and evaporated to obtain the initial extract, and the initial extract was extracted with ethyl acetate and rotary evaporated to obtain a saturated extract.

[0046] 3. Mix gelatin and polylysine, dissolve in water at 0.03 g / mL to obtain an aqueous phase, add the extract obtained in step 2 to the aqueous phase at 0.03 g / mL, emulsify in a 40°C constant temperature water bath at 1500 r / min for 15 min, and use glutaraldehyde at a mass concentration of 22% as a curing agent to obtain hemp antibacterial microcapsules.

[0047] The preparation method of dicarboxylated hemp fiber specifically includes the following steps:

[0048] S1. Cottonized hemp fiber was added to a 5% sodium periodate solution at a dosage of 0.21 g / mL. The solution was kept warm and shaken at 35°C for 80 min at 80 rpm under light-protected conditions. The solution was then filtered to obtain oxidized hemp fiber.

[0049] S2. The oxidized hemp fiber obtained in S1 was added to a 3.5% glycerol solution at an addition amount of 0.16 g / mL, stirred at 60 rpm for 40 min, washed three times with deionized water, and dried in an oven at 80 ℃ for 2 h to obtain aldehyde-modified hemp fiber.

[0050] S3. The aldehyde-modified hemp fiber obtained in S2 was added to a 4% sodium chlorite solution at an addition rate of 0.35 g / mL. The solution was stirred at 50 rpm for 12 h, filtered, washed, and dried to obtain dicarboxylated hemp fiber.

[0051] This invention also provides a method for preparing an antibacterial nonwoven fabric made entirely of hemp fiber, specifically including the following steps:

[0052] Hemp antibacterial microcapsules were prepared into a 0.3 g / mL suspension and stirred evenly to obtain a finishing solution. Dicarboxylated hemp fibers and cottonized hemp fibers were used to prepare nonwoven fabric by hydroentangling and then immersed in the finishing solution. The fabric was dipped and nibbled twice, with a nibbling rate of 100%. It was then placed in a setting dryer and dried at 80°C for 3 min and at 160°C for 2 min. After cooling to room temperature, a whole hemp fiber antibacterial nonwoven fabric was obtained.

[0053] Example 2

[0054] A nonwoven fabric made entirely of hemp fiber antibacterial components comprises the following components in parts by weight: 35 parts of cottonized hemp fiber, 2 parts of hemp antibacterial microcapsules, and 18 parts of dicarboxylated hemp fiber.

[0055] The cotton-like hemp fiber comprises the following components in parts by weight: 50 parts hemp fiber, 1.2 parts fruit enzyme, 0.6 parts laccase, and 0.5 parts hemicellulase.

[0056] The hemp antibacterial microcapsules comprise the following components by weight: 60 parts hemp bast fiber, 50 parts hemp stalk core, 5 parts gelatin, and 3 parts polylysine.

[0057] The preparation method of cotton-like hemp fiber specifically includes the following steps:

[0058] (1) Add hemp fiber at a dosage of 1.2 g / mL to water and soak for 2 hours. Then, treat it with an ultrasonic frequency of 40 kHz, a microwave power of 200 W, and a temperature of 45 °C for 25 minutes. Filter and dry to obtain pretreated hemp.

[0059] (2) The pretreated hemp obtained in step (1) was added to water at an addition rate of 0.9 g / mL, followed by the addition of fruit enzyme, laccase and hemicellulase to obtain a mixture;

[0060] (3) The mixture obtained in step (1) was stirred at 30 rpm in a 35°C water bath for 100 min to obtain the enzymatic hydrolysate. The hydrolysate was filtered, washed three times with water, and dried to obtain cotton-like hemp fiber.

[0061] The preparation method of hemp antibacterial microcapsules specifically includes the following steps:

[0062] 1. Take hemp bast fibers and hemp stalk cores, remove impurities, wash, filter, dry, and pulverize through an 80-mesh sieve to obtain a mixed powder;

[0063] 2. Add the mixed powder to anhydrous ethanol at a rate of 0.05 g / mL, heat and stir at 60°C at 400 rpm, filter and evaporate to obtain the initial extract, extract the initial extract with ethyl acetate and rotary evaporate to obtain the saturated extract.

[0064] 3. Mix gelatin and polylysine, dissolve in water at 0.02 g / mL to obtain an aqueous phase, add the extract obtained in step 2 to the aqueous phase at 0.01 g / mL, emulsify in a 40°C constant temperature water bath at 1500 r / min for 15 min, and use glutaraldehyde at a mass concentration of 22% as a curing agent to obtain hemp antibacterial microcapsules.

[0065] The preparation method of dicarboxylated hemp fiber specifically includes the following steps:

[0066] S1. Cottonized hemp fiber was added to a 3% sodium periodate solution at a dosage of 0.13 g / mL. The solution was kept warm and shaken at 20°C for 50 min at 60 rpm under dark conditions. The solution was then filtered to obtain oxidized hemp fiber.

[0067] S2. The oxidized hemp fiber obtained in S1 was added to a 2.5% glycerol solution at an addition amount of 0.09 g / mL, stirred at 30 rpm for 40 min, washed three times with deionized water, and dried in an oven at 80℃ for 2 h to obtain aldehyde-modified hemp fiber.

[0068] S3. The aldehyde-modified hemp fiber obtained in S2 was added to a sodium chlorite solution with a mass concentration of 3.2% at an addition amount of 0.23 g / mL. The mixture was stirred at 30 rpm for 8 h, filtered, washed and dried to obtain dicarboxylated hemp fiber.

[0069] This invention also provides a method for preparing an antibacterial nonwoven fabric made entirely of hemp fiber, specifically including the following steps:

[0070] Hemp antibacterial microcapsules were prepared into a 0.2 g / mL suspension and stirred evenly to obtain a finishing solution. Dicarboxylated hemp fibers and cottonized hemp fibers were used to prepare nonwoven fabric by hydroentangling and then immersed in the finishing solution. The fabric was dipped and nibbled twice, with a nibbling rate of 100%. It was then placed in a setting dryer and dried at 80°C for 3 min and at 160°C for 2 min. After cooling to room temperature, a whole hemp fiber antibacterial nonwoven fabric was obtained.

[0071] Example 3

[0072] A nonwoven fabric made entirely of hemp fiber antibacterial components comprises the following components in parts by weight: 37 parts of cottonized hemp fiber, 3 parts of hemp antibacterial microcapsules, and 20 parts of dicarboxylated hemp fiber.

[0073] The cotton-like hemp fiber comprises the following components in parts by weight: 55 parts hemp fiber, 1.4 parts fruit enzyme, 0.7 parts laccase, and 0.6 parts hemicellulase.

[0074] The hemp antibacterial microcapsules comprise the following components by weight: 70 parts hemp bast fiber, 60 parts hemp stalk core, 6 parts gelatin, and 5 parts polylysine.

[0075] The preparation method of cotton-like hemp fiber specifically includes the following steps:

[0076] (1) Add hemp fiber at a dosage of 2g / mL to water and soak for 2.5h. Then, treat it with an ultrasonic frequency of 45KHZ, a microwave power of 250w, and a temperature of 50℃ for 25-30min. Filter and dry to obtain pretreated hemp.

[0077] (2) The pretreated hemp obtained in step (1) was added to water at an addition rate of 1.2 g / mL, followed by the addition of fruit enzyme, laccase and hemicellulase to obtain a mixture;

[0078] (3) The mixture obtained in step (1) was stirred at 50 rpm in a 40°C water bath for 120 min to obtain the enzymatic hydrolysate. The hydrolysate was filtered, washed four times with water, and dried to obtain cotton-like hemp fiber.

[0079] The preparation method of hemp antibacterial microcapsules specifically includes the following steps:

[0080] 1. Take hemp bast fibers and hemp stalk cores, remove impurities, wash, filter, dry, and pulverize through an 80-mesh sieve to obtain a mixed powder;

[0081] 2. Add the mixed powder to anhydrous ethanol at a rate of 0.05 g / mL, heat and stir at 70°C at 450 rpm, filter and evaporate to obtain the initial extract, extract the initial extract with ethyl acetate and rotary evaporate to obtain the saturated extract.

[0082] 3. Mix gelatin and polylysine, dissolve in water at 0.03 g / mL to obtain an aqueous phase, add the extract obtained in step 2 to the aqueous phase at 0.02 g / mL, emulsify in a 40°C constant temperature water bath at 1500 r / min for 15 min, and use glutaraldehyde at a mass concentration of 22% as a curing agent to obtain hemp antibacterial microcapsules.

[0083] The preparation method of dicarboxylated hemp fiber specifically includes the following steps:

[0084] S1. Cottonized hemp fiber was added to a 4% sodium periodate solution at a dosage of 0.17 g / mL. The solution was kept warm and shaken at 30°C for 70 min at 70 rpm under light-protected conditions. The oxidized hemp fiber was then obtained by filtration.

[0085] S2. The oxidized hemp fiber obtained in S1 was added to a 3% glycerol solution at an addition amount of 0.12 g / mL, stirred at 50 rpm for 40 min, washed three times with deionized water, and dried in an oven at 80 ℃ for 2 h to obtain aldehyde-modified hemp fiber.

[0086] S3. The aldehyde-modified hemp fiber obtained in S2 was added to a 3.5% sodium chlorite solution at a dosage of 0.3 g / mL, stirred at 40 rpm for 10 h, filtered, washed and dried to obtain dicarboxylated hemp fiber.

[0087] This invention also provides a method for preparing an antibacterial nonwoven fabric made entirely of hemp fiber, specifically including the following steps:

[0088] Hemp antibacterial microcapsules were prepared into a 0.25 g / mL suspension and stirred evenly to obtain a finishing solution. Dicarboxylated hemp fibers and cottonized hemp fibers were used to prepare nonwoven fabric by hydroentangling and then immersed in the finishing solution. The fabric was dipped and nibbled twice, with a nibbling rate of 100%. It was then placed in a setting dryer and dried at 80°C for 3 min and at 160°C for 2 min. After cooling to room temperature, a whole hemp fiber antibacterial nonwoven fabric was obtained.

[0089] Comparative Example 1

[0090] This comparative example provides a nonwoven fabric that differs from Example 1 only in that it does not contain hemp antibacterial microcapsules in its composition; the other components and their contents are the same as in Example 1.

[0091] Comparative Example 2

[0092] This comparative example provides a nonwoven fabric that differs from Example 1 only in that it does not contain dicarboxylated hemp fiber in its composition; the other components and their contents are the same as in Example 1.

[0093] Comparative Example 3

[0094] This comparative example provides a nonwoven fabric that differs from Example 1 only in that the hemp in the components is not cottonized, and the cottonized hemp fibers are replaced with uncottonized hemp fibers. It also does not contain hemp antibacterial microcapsules. The remaining components and component contents are the same as in Example 1.

[0095] Comparative Example 4

[0096] This comparative example provides a nonwoven fabric that differs from Example 1 only in that the hemp in the components is cottonized and there are no hemp antibacterial microcapsules. The other components and their contents are the same as in Example 1.

[0097] Experimental Example

[0098] 1. Antibacterial test

[0099] Rectangles with a width of 0.5 cm and a length of 2 cm, cut from Examples 1-3 and Comparative Examples 1-2, were used as the experimental group. Rectangles with a width of 0.5 cm and a length of 2 cm, cut from Comparative Example 4, were used as the control group. The concentration was 2 × 10⁻⁶. 8 12 mL each of CFU / mL *E. coli* and *Staphylococcus aureus* suspensions were added to the control and experimental groups, and the mixtures were thoroughly mixed for 5 min. Then, 1 mL of each suspension was added to a 5 mL PBS buffer solution in a test tube for dilution. Agar medium was added to sterile dishes, and the mixtures were incubated at 37°C for 24 h. Plate counts were performed, and the inhibition rate was calculated using the following formula:

[0100] Antibacterial rate = (number of colonies in control group - number of colonies in experimental group) / number of colonies in control group × 100%.

[0101] Figure 1The figures show the results of antibacterial tests for Examples 1-3 and Comparative Examples 1-2. As shown, Examples 1-3 showed inhibition rates of 99.9%, 100%, and 100% against *Escherichia coli*, and 99.8%, 100%, and 99.6% against *Staphylococcus aureus*, respectively. Comparative Examples 1-2 showed inhibition rates of 63.1% and 72.5% against *Escherichia coli*, and 64.2% and 69.3% against *Staphylococcus aureus*, respectively. The inhibition rates of Examples 1-3 against *Escherichia coli* and *Staphylococcus aureus* are significantly higher. The antibacterial effect was significantly higher than that of Comparative Example 1, indicating that the use of hemp antibacterial microcapsules enhanced the antibacterial effect. The antibacterial rates of Escherichia coli and Staphylococcus aureus in Examples 1-3 were significantly higher than those in Comparative Example 2, indicating that the use of dicarboxylated hemp fiber enhanced the antibacterial effect. The alcohol extracts of hemp bast fiber and hemp stalk core, after extraction with ethyl acetate, showed good antibacterial effects. The microcapsule wall material contained polylysine carrying a large number of amino groups, which could bind to the surface of dicarboxylated hemp fiber containing a large number of carboxyl groups, thereby increasing the microcapsule loading rate and enhancing the antibacterial effect.

[0102] 2. Water absorption and water retention rate test

[0103] Examples 1-3 and Comparative Examples 2-3 were cut into rectangles with a width of 0.5 cm and a length of 2 cm. The rectangles, each measuring 2 × 2 cm, were placed in a vacuum drying oven and dried at 25 °C for 1 h. The initial weight was measured. Then, the samples were soaked in deionized water for 24 h until saturation, and the saturated weight was measured. The samples were then placed in a centrifuge and centrifuged at 1200 rpm for 15 min. The weight after centrifugation was measured.

[0104] Calculate the water absorption rate using the following formula:

[0105] Water absorption rate = (saturated weight - initial weight) / initial weight × 100%;

[0106] Calculate the water retention rate using the following formula:

[0107] Water retention rate = (weight after centrifugation - initial weight) / initial weight × 100%.

[0108] Figure 2 The figures show the results of water absorption rate tests for Examples 1-3 and Comparative Examples 2-3. As shown, the water absorption rates for Examples 1-3 and Comparative Examples 1-3 are 743.5%, 740.7%, 742.1%, 603.9%, and 411.5%, respectively. Figure 3The results of water retention rate tests for Examples 1-3 and Comparative Examples 2-3 are shown in the figure. As shown, the water retention rates of Examples 1-3 and Comparative Examples 2-3 are 54.3%, 43.5%, 46.6%, 31.9%, and 21.1%, respectively. As shown, the water absorption and water retention rates of Examples 1-3 are higher than those of Comparative Examples 2-3, indicating that the use of dicarboxylated hemp fiber and cottonized hemp fiber enhances the water retention and absorption effect. Carboxyl groups can combine with water molecules, so dicarboxylated hemp fiber has good water retention and absorption capacity. Cottonized hemp fiber removes fructose, lignin, and hemicellulose, and its porous structure can better absorb water.

[0109] 4. Mite removal test

[0110] Using Examples 1-3 and Comparative Examples 1-2 as samples, and Comparative Example 3 as a control, the samples were placed at the bottom of the culture dishes. A 10mm thick sponge with approximately 200mm edges was placed in a covered container, and saturated saline solution was poured in to just cover the sponge. Three samples and three control samples were placed in each of the six culture dishes. 0.05g of mite feed was evenly distributed on the samples. 150 surviving mites were placed in each of the six culture dishes. The six culture dishes were placed on the sponge in the container, with a distance of more than 10mm between the culture dishes (as per GB / T24253-2009, 9.2 Inhibition Method). The container was covered and placed in a constant temperature and humidity incubator at 25℃ and 75% relative humidity. After 7 days of culture, the number of surviving adult mites and nymphs was observed and recorded as the survival rate. The inhibition rate was calculated using the following formula:

[0111] Inhibition rate = (average number of surviving mites in three control samples - average number of surviving mites in three test samples) / average number of surviving mites in three control samples × 100%.

[0112] Figure 4 The results of the mite-removal tests for Examples 1-3 and Comparative Examples 1-2 are shown in the figure. As shown, the mite inhibition rates of Examples 1-3 and Comparative Examples 1-2 were 62.3%, 63.8%, 63.0%, 24.6%, and 43.3%, respectively. The mite inhibition rate of Examples 1-3 was significantly higher than that of Comparative Examples 1-2, indicating that the use of hemp antibacterial microcapsules and dicarboxylated hemp fibers enhanced the mite-removal effect. The alcohol extracts of hemp bast fibers and hemp stalk cores, after extraction with ethyl acetate, have good antibacterial effects. The microcapsule wall material contains polylysine carrying a large number of amino groups, which can bind to the surface of dicarboxylated hemp fibers containing a large number of carboxyl groups, increasing the microcapsule loading rate and enhancing the mite-removal effect. The inhibition rate of Examples 1-3 was greater than 60%. Therefore, according to GB / T24253-2009, the samples have an anti-mite effect.

[0113] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

[0114] The present invention and its embodiments have been described above. This description is not restrictive, and the accompanying drawings are only one embodiment of the present invention. The actual application is not limited to this. In conclusion, if those skilled in the art are inspired by this description and design similar methods and embodiments without departing from the spirit of the present invention, they should all fall within the protection scope of the present invention.

Claims

1. A full hemp fiber antibacterial nonwoven fabric, characterized by: The cottonized hemp fiber comprises the following components in parts by weight: 35-40 parts of cottonized hemp fiber, 2-5 parts of hemp antibacterial microcapsule, and 18-23 parts of double-carboxyl hemp fiber; the cottonized hemp fiber is obtained by ultrasonic microwave-assisted enzymatic hydrolysis of hemp fiber; the hemp antibacterial microcapsule is a microcapsule obtained by coating gelatin-polylysine on the alcohol extract of hemp bast fiber and hemp core; the double-carboxyl hemp fiber is obtained by reacting the cottonized hemp fiber with sodium chlorite after sodium periodate oxidation; The cottonized hemp fiber comprises the following components in parts by weight: 50-60 parts of hemp fiber, 1.2-1.6 parts of pectinase, 0.6-0.8 parts of laccase, and 0.5-0.7 parts of hemicellulase; The preparation method of the cottonized hemp fiber specifically comprises the following steps: (1) hemp fiber is added to water at an addition amount of 1.2-3 g / mL and soaked for 2-3 h, and then treated at an ultrasonic frequency of 40-50 KHZ, a microwave power of 200-300 W, and a temperature of 45-55 ℃ for 30 min, filtered and dried to obtain pretreated hemp; (2) the pretreated hemp obtained in step (1) is added to water at an addition amount of 0.9-1.5 g / mL, and then pectinase, laccase and hemicellulase are added to obtain a mixture; (3) the mixture obtained in step (2) is stirred in a 30-60 rpm water bath at 35-45 ℃ for 100-150 min to obtain an enzymatic hydrolysate, which is filtered, washed with water for 3-5 times, and dried to obtain cottonized hemp fiber; The hemp antibacterial microcapsule comprises the following components in parts by weight: 60-80 parts of hemp bast fiber, 50-65 parts of hemp core, 5-7 parts of gelatin, and 3-6 parts of polylysine; The preparation method of the hemp antibacterial microcapsule specifically comprises the following steps: I. The hemp bast fiber and hemp core are taken, impurities are removed, washed, filtered, dried, and pulverized through an 80-mesh sieve to obtain a mixed powder; II. The mixed powder is added to anhydrous ethanol at an addition amount of 0.05-0.06 g / mL, and stirred at a speed of 400-500 rpm at 60-80 ℃, filtered and evaporated to obtain a primary extract, and the primary extract is extracted with ethyl acetate and rotary evaporated to obtain a saturated extract; III. Gelatin and polylysine are mixed, dissolved in water at 0.02-0.03 g / mL to obtain an aqueous phase, the extract obtained in step II is added to the aqueous phase at an addition amount of 0.01-0.03 g / mL, and emulsified at 40 ℃ constant temperature water bath and 1500 r / min for 15 min, and a 22% glutaraldehyde solution is used as a curing agent to obtain hemp antibacterial microcapsules; The preparation method of the double-carboxyl hemp fiber specifically comprises the following steps: S1. The cottonized hemp fiber is added to a 3-5% sodium periodate solution at an addition amount of 0.13-0.21 g / mL, and oscillated at a speed of 60-80 rpm at 20-35 ℃ under light-proof conditions for 50-80 min, and filtered to obtain oxidized hemp fiber; S2, the oxidized hemp fibers obtained in S1 were added to a glycerol solution with a mass concentration of 2.5-3.5% at an addition amount of 0.09-0.16 g / mL, stirred at 30-60 rpm for 40 min, washed with deionized water for 3 times, and dried in an oven at 80°C for 2 h to obtain aldehyde-modified hemp fibers; S3, the aldehyde-modified hemp fibers obtained in S2 were added to a sodium chlorite solution with a mass concentration of 3.2-4% at an addition amount of 0.23-0.35 g / mL, stirred at 30-50 rpm for 8-12 h, filtered, washed and dried to obtain double-carboxylated hemp fibers.

2. A method of producing the full hemp fiber antibacterial nonwoven fabric according to claim 1, characterized by: Specifically comprising the following steps: The hemp antibacterial microcapsules were configured into a suspension of 0.2-0.3 g / mL, stirred uniformly to obtain a finishing liquid, the double-carboxylated hemp fibers and the cottonized hemp fibers were prepared into non-woven fabrics by the spunlace method, and were immersed into the finishing liquid, double-dipped and double-rolled with a roll liquid rate of 100%, placed in a setting dryer, baked at 80°C for 3 min, baked at 160°C for 2 min, and cooled to room temperature to obtain a full-hemp fiber antibacterial non-woven fabric.

Citation Information

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