Preparation method of fibers containing zanthoxylum bungeanum functional factors

Abstract

The invention belongs to the technical field of functional fibers, and particularly relates to a preparation method of fibers containing zanthoxylum bungeanum functional factors. The zanthoxylum bungeanum functional factor prepared by the method is suitable for various fiber base materials, has good dispersity, has a protection effect on a zanthoxylum bungeanum extract, prevents active components of zanthoxylum bungeanum from being lost in a high-temperature and acid-base environment, and reduces the cost and the waste of resources; through detection, the loss rate of the zanthoxylum bungeanum extract in the fiber preparation process is lower than 2%. The fiber containing the zanthoxylum bungeanum functional factor prepared by the invention has excellent antibacterial and anti-mite effects, the bacteriostasis rate to staphylococcus aureus is 97.8-99% after the fiber is washed with water for 50 times, the bacteriostasis rate to candida albicans is 98.1-99.2%, the bacteriostasis rate to escherichia coli is 97.5-98.8%, and the mite repelling rate is greater than 70%.

Description

Technical Field

[0001] The invention belongs to the technical field of functional fibers, and in particular relates to a method for preparing fibers containing Zanthoxylum bungeanum functional factors. Background Art

[0002] The progress of the times has led to an increasing demand for functional textiles. Compared with finished fabrics, textile raw materials with various functional effects - fibers and yarns - have better functional durability, so emerging functional fibers / yarns are becoming more and more popular among the public.

[0003] Natural extracts are biodegradable, safe, environmentally friendly, and have multiple functions. Therefore, they are generally added before spinning and mixed with the spinning solution before spinning. However: (1) In order to improve the storage stability of natural extracts, solid powder extracts are purchased and mixed with the spinning solution: (1) Direct mixing - poor dispersion uniformity, low bioavailability; fiber or yarn strength is affected; (2) Added after the solution is made - poor compatibility with the spinning solution, reduced functional durability, and high loss rate.

[0004] Sichuan pepper is a traditional Chinese spice and Chinese medicinal material. Modern pharmacological research has confirmed that Sichuan pepper has the effects of repelling insects, killing insects, inhibiting bacteria and preserving. The active ingredients in Sichuan pepper extract include linalool, limonene, unsaturated organic acids, etc. Studies have shown that linalool has antibacterial and insecticidal effects and can inhibit Escherichia coli; limonene has insecticidal and mite-killing functions. However, limonene contains unsaturated bonds in its structure and is not very stable. It is prone to oxidation reactions, especially under heat and light conditions. In the presence of inorganic acid (H2SO4), it reacts with water to generate α-terpineol and hydrated terpene diols, which are relatively stable under alkaline conditions. Therefore, limonene has poor stability and is easily denatured by high temperature and acidic conditions. If Sichuan pepper extract is directly added during the spinning process, the effect will be greatly reduced.

[0005] Therefore, it is urgent to develop a functional factor of Zanthoxylum bungeanum with good stability, uniform dispersion and high biological utilization rate to ensure that the role of Zanthoxylum bungeanum in the fiber is fully exerted. Summary of the invention

[0006] In order to solve the problems existing in the prior art, the present invention provides a method for preparing fiber containing Zanthoxylum bungeanum functional factors, so as to achieve the invention purpose of improving the dispersibility and utilization rate of Zanthoxylum bungeanum extract and reduce the loss of Zanthoxylum bungeanum extract during the fiber preparation process.

[0007] In order to solve the above technical problems, the present invention adopts the following technical solutions: A method for preparing fiber containing Zanthoxylum bungeanum functional factors, the preparation method comprising the following steps: S1. Modification of nanoporous silica The nanoporous silica is added to DMF and ultrasonically dispersed uniformly to obtain a suspension; KH-570 is added to DMF and stirred uniformly, and then the suspension is added, reacted at 55-70° C. for 5-10 hours, separated after centrifugation, washed with anhydrous ethanol, and dried to obtain nanoporous silica modified with a carbon-carbon double bond.

[0008] Preferably, the added amount of KH-570 is 26-34% of the mass of the nanoporous silica.

[0009] Preferably, the particle size of the nanoporous silica is 100-150 nm, and the pore size is 5-15 nm.

[0010] S2. Grafting Add carbon-carbon double bond modified nanoporous silica, glycidyl methacrylate and initiator into anhydrous ethanol and stir for 20-30 minutes at a stirring rate of 300-400 r / min; heat to 60-70°C and stir for reaction for 5-7 hours, the double bonds in glycidyl methacrylate and the double bonds on the surface of nanoporous silica undergo free radical polymerization, and glycidyl methacrylate is grafted onto the nanoporous silica. After the reaction, centrifuge, filter, wash with anhydrous ethanol and ether, and dry to obtain modified nanoporous silica.

[0011] Preferably, the mass ratio of the carbon-carbon double bond modified nanoporous silica to glycidyl methacrylate is 4-6:1.05-1.45.

[0012] Preferably, the initiator is azobisisobutyronitrile, and the added amount is 1 to 2% of the mass of glycidyl methacrylate.

[0013] Preferably, the stirring reaction rate is 100-200 r / min.

[0014] S3, Load The pepper extract is added to an ethanol aqueous solution and stirred for 20 to 30 minutes to obtain a pepper extract solution, and then the modified nanoporous silica is added and stirred for 6 to 12 hours to allow the pepper extract to be fully loaded in the porous structure of the modified nanoporous silica, followed by drying to obtain the pepper functional factor.

[0015] Preferably, the mass ratio of the Zanthoxylum bungeanum extract to the ethanol aqueous solution is 1:4-7.

[0016] Preferably, the added amount of the modified nanoporous silica is 15-25% of the mass of the Zanthoxylum bungeanum extract solution.

[0017] Preferably, the mass fraction of the ethanol aqueous solution is 50-60wt%.

[0018] S4. Spinning The functional factor of Zanthoxylum bungeanum is added into the spinning solution or polymer slices before spinning and mixed evenly, and the fiber containing the functional factor of Zanthoxylum bungeanum is obtained after wet spinning or melt spinning.

[0019] Preferably, the spinning solution is viscose spinning solution or acrylic spinning solution; the polymer slices are one or more of PET slices, PA6 slices, and PA66.

[0020] Preferably, the added amount of the Zanthoxylum bungeanum functional factor is 3-5% of the effective ingredients of the spinning solution (referring to the content of methyl cellulose or polyacrylonitrile in the spinning solution) or the mass of the polymer slices.

[0021] Due to the adoption of the above technical solution, the technical effects achieved by the present invention are: 1. The fiber containing Zanthoxylum bungeanum functional factors prepared by the present invention has excellent antibacterial and anti-mite effects. After washing 50 times, the antibacterial rates of Staphylococcus aureus, Candida albicans and Escherichia coli are 97.8-99%, 98.1-99.2% and 97.5-98.8% respectively (determined according to GB / T 20944.3-2008), and the mite repellent rate is greater than 70% (determined according to the repellent method of GB / T 24253-2009 / 9.1).

[0022] 2. The pepper functional factors prepared by the present invention have good dispersibility and protect the pepper extract, thereby preventing the active ingredients of pepper from being lost in high temperature and acid-base environments, reducing costs and waste of resources; according to testing, the loss rate of pepper extract during the fiber preparation process is less than 2%.

[0023] 3. The present invention firstly uses KH-570 to modify carbon-carbon double bonds on the surface of nanoporous silica, and then grafts glycidyl methacrylate onto the nanoporous silica. During the grafting process, the double bonds in glycidyl methacrylate and the double bonds on the surface of the nanoporous silica are free radical polymerized, while the epoxy groups in glycidyl methacrylate are retained, so the functional factors of Zanthoxylum bungeanum contain epoxy groups.

[0024] 4. The Zanthoxylum bungeanum functional factor prepared by the present invention is suitable for a variety of fiber substrates, especially viscose fiber and polyester. This is because the viscose spinning stock solution is alkaline. Under alkaline conditions, the epoxy groups in the Zanthoxylum bungeanum functional factor open the ring and react with the hydroxyl groups on the cellulose macromolecules for cross-linking and grafting; in a high temperature environment, the epoxy groups open the ring and react with the hydroxyl or carboxyl groups in the polyester for cross-linking and grafting, which can not only improve the mechanical properties of the fiber, but also improve the durability of the Zanthoxylum bungeanum function. The antibacterial loss rate after 100 washings is less than 5%. DETAILED DESCRIPTION

[0025] The present invention is further described below in conjunction with specific embodiments.

[0026] Embodiment 1: A method for preparing fiber containing Zanthoxylum bungeanum functional factors, the preparation method comprising the following steps: S1. Modification of nanoporous silica The nanoporous silica was added to DMF and evenly dispersed by ultrasonic to obtain a suspension; KH-570 was added to DMF and stirred evenly, and then the suspension was added, reacted at 65°C for 8 hours, separated after centrifugation, washed with anhydrous ethanol, and dried to obtain nanoporous silica modified with carbon-carbon double bonds.

[0027] The added amount of KH-570 is 30% of the mass of the nanoporous silica.

[0028] The particle size of the nanoporous silica is 120 nm and the pore size is 10 nm.

[0029] S2. Grafting Add carbon-carbon double bond modified nanoporous silica, glycidyl methacrylate and initiator into anhydrous ethanol and stir for 25 minutes at a stirring rate of 350r / min; heat to 65°C and stir for 6 hours to allow free radical polymerization of double bonds in glycidyl methacrylate and double bonds on the surface of nanoporous silica, and glycidyl methacrylate is grafted onto the nanoporous silica. After the reaction, centrifuge, filter, wash with anhydrous ethanol and ether, and dry to obtain modified nanoporous silica.

[0030] The mass ratio of the carbon-carbon double bond modified nanoporous silica to glycidyl methacrylate is 5:1.25.

[0031] The initiator is azobisisobutyronitrile, and the added amount is 1.6% of the mass of glycidyl methacrylate.

[0032] The stirring reaction rate was 150 r / min.

[0033] S3, Load The pepper extract was added to an ethanol aqueous solution and stirred for 25 minutes to obtain a pepper extract solution, and then the modified nanoporous silica was added and stirred for 10 hours to allow the pepper extract to be fully loaded in the porous structure of the modified nanoporous silica, and then dried to obtain the pepper functional factor.

[0034] The mass ratio of the Zanthoxylum bungeanum extract to the ethanol aqueous solution is 1:5.

[0035] The added amount of the modified nanoporous silica is 20% of the mass of the Zanthoxylum bungeanum extract solution.

[0036] The mass fraction of the ethanol aqueous solution is 55wt%.

[0037] S4. Spinning The functional factor of Zanthoxylum bungeanum is added into the viscose spinning stock solution and mixed evenly, and the fiber containing the functional factor of Zanthoxylum bungeanum is obtained after wet spinning.

[0038] The viscosity of the viscose spinning solution was controlled at 60 s (falling ball method), the maturity was controlled at 11 mL (10% NH4CL), and the methyl cellulose content was 7.6 wt%.

[0039] The added amount of the Zanthoxylum bungeanum functional factor is 4% of the methyl cellulose content in the viscose spinning solution.

[0040] Embodiment 2: A method for preparing fiber containing Zanthoxylum bungeanum functional factors, the preparation method comprising the following steps: S1. Modification of nanoporous silica The nanoporous silica was added to DMF and evenly dispersed by ultrasonic to obtain a suspension; KH-570 was added to DMF and stirred evenly, and then the suspension was added, reacted at 55° C. for 10 hours, separated after centrifugation, washed with anhydrous ethanol, and dried to obtain nanoporous silica modified with carbon-carbon double bonds.

[0041] The added amount of KH-570 is 26% of the mass of the nanoporous silica.

[0042] The particle size of the nanoporous silica is 100 nm and the pore size is 5 nm.

[0043] S2. Grafting Add carbon-carbon double bond modified nanoporous silica, glycidyl methacrylate and initiator into anhydrous ethanol and stir for 20 minutes at a stirring rate of 300 r / min; heat to 60°C and stir for 5 hours to react, the double bonds in glycidyl methacrylate and the double bonds on the surface of nanoporous silica undergo free radical polymerization, and glycidyl methacrylate is grafted onto the nanoporous silica. After the reaction, centrifuge, filter, wash with anhydrous ethanol and ether, and dry to obtain modified nanoporous silica.

[0044] The mass ratio of the carbon-carbon double bond modified nanoporous silica to glycidyl methacrylate is 4:1.05.

[0045] The initiator is azobisisobutyronitrile, and the added amount is 1% of the mass of glycidyl methacrylate.

[0046] The stirring reaction rate was 100 r / min.

[0047] S3, Load The pepper extract was added to an ethanol aqueous solution and stirred for 20 minutes to obtain a pepper extract solution, and then the modified nanoporous silica was added and stirred for 6 hours to allow the pepper extract to be fully loaded in the porous structure of the modified nanoporous silica, and then dried to obtain the pepper functional factor.

[0048] The mass ratio of the Zanthoxylum bungeanum extract to the ethanol aqueous solution is 1:7.

[0049] The added amount of the modified nanoporous silica is 15% of the mass of the Zanthoxylum bungeanum extract solution.

[0050] The mass fraction of the ethanol aqueous solution is 50wt%.

[0051] S4. Spinning The functional factor of Zanthoxylum bungeanum is added into the viscose spinning stock solution and mixed evenly, and the fiber containing the functional factor of Zanthoxylum bungeanum is obtained after wet spinning.

[0052] The viscosity of the viscose spinning solution was controlled at 60 s (falling ball method), the maturity was controlled at 11 mL (10% NH4CL), and the methyl cellulose content was 7.6 wt%.

[0053] The added amount of the Zanthoxylum bungeanum functional factor is 3% of the methyl cellulose content in the viscose spinning solution.

[0054] Embodiment 3: A method for preparing fiber containing Zanthoxylum bungeanum functional factors, the preparation method comprising the following steps: S1. Modification of nanoporous silica The nanoporous silica was added to DMF and evenly dispersed by ultrasonic to obtain a suspension; KH-570 was added to DMF and stirred evenly, and then the suspension was added, reacted at 70°C for 5 hours, separated after centrifugation, washed with anhydrous ethanol, and dried to obtain nanoporous silica modified with carbon-carbon double bonds.

[0055] The added amount of KH-570 is 34% of the mass of the nanoporous silica.

[0056] The particle size of the nanoporous silica is 150 nm and the pore size is 15 nm.

[0057] S2. Grafting Add carbon-carbon double bond modified nanoporous silica, glycidyl methacrylate and initiator into anhydrous ethanol and stir for 30 minutes at a stirring rate of 400 r / min; heat to 70°C and stir for 7 hours to polymerize the double bonds in glycidyl methacrylate and the double bonds on the surface of nanoporous silica, and glycidyl methacrylate is grafted onto the nanoporous silica. After the reaction, centrifuge, filter, wash with anhydrous ethanol and ether, and dry to obtain modified nanoporous silica.

[0058] The mass ratio of the carbon-carbon double bond modified nanoporous silica to glycidyl methacrylate is 6:1.45.

[0059] The initiator is azobisisobutyronitrile, and the added amount is 2% of the mass of glycidyl methacrylate.

[0060] The stirring reaction rate was 200 r / min.

[0061] S3, Load The pepper extract was added to an ethanol aqueous solution and stirred for 30 minutes to obtain a pepper extract solution, and then the modified nanoporous silica was added and stirred for 12 hours to allow the pepper extract to be fully loaded in the porous structure of the modified nanoporous silica, followed by drying to obtain the pepper functional factor.

[0062] The mass ratio of the Zanthoxylum bungeanum extract to the ethanol aqueous solution is 1:4.

[0063] The added amount of the modified nanoporous silica is 25% of the mass of the Zanthoxylum bungeanum extract solution.

[0064] The mass fraction of the ethanol aqueous solution is 60wt%.

[0065] S4. Spinning The functional factor of Zanthoxylum bungeanum is added into the viscose spinning stock solution and mixed evenly, and the fiber containing the functional factor of Zanthoxylum bungeanum is obtained after wet spinning.

[0066] The viscosity of the viscose spinning solution was controlled at 60 s (falling ball method), the maturity was controlled at 11 mL (10% NH4CL), and the methyl cellulose content was 7.6 wt%.

[0067] The added amount of the Zanthoxylum bungeanum functional factor is 5% of the methyl cellulose content in the viscose spinning solution.

[0068] Embodiment 4: A method for preparing fiber containing Zanthoxylum bungeanum functional factors, the preparation method comprising the following steps: S1. Modification of nanoporous silica The nanoporous silica was added to DMF and evenly dispersed by ultrasonic to obtain a suspension; KH-570 was added to DMF and stirred evenly, and then the suspension was added, reacted at 65°C for 8 hours, separated after centrifugation, washed with anhydrous ethanol, and dried to obtain nanoporous silica modified with carbon-carbon double bonds.

[0069] The added amount of KH-570 is 30% of the mass of the nanoporous silica.

[0070] The particle size of the nanoporous silica is 120 nm and the pore size is 10 nm.

[0071] S2. Grafting Add carbon-carbon double bond modified nanoporous silica, glycidyl methacrylate and initiator into anhydrous ethanol and stir for 25 minutes at a stirring rate of 350r / min; heat to 65°C and stir for 6 hours to allow free radical polymerization of double bonds in glycidyl methacrylate and double bonds on the surface of nanoporous silica, and glycidyl methacrylate is grafted onto the nanoporous silica. After the reaction, centrifuge, filter, wash with anhydrous ethanol and ether, and dry to obtain modified nanoporous silica.

[0072] The mass ratio of the carbon-carbon double bond modified nanoporous silica to glycidyl methacrylate is 5:1.25.

[0073] The initiator is azobisisobutyronitrile, and the added amount is 1.6% of the mass of glycidyl methacrylate.

[0074] The stirring reaction rate was 150 r / min.

[0075] S3, Load The pepper extract was added to an ethanol aqueous solution and stirred for 25 minutes to obtain a pepper extract solution, and then the modified nanoporous silica was added and stirred for 10 hours to allow the pepper extract to be fully loaded in the porous structure of the modified nanoporous silica, and then dried to obtain the pepper functional factor.

[0076] The mass ratio of the Zanthoxylum bungeanum extract to the ethanol aqueous solution is 1:5.

[0077] The added amount of the modified nanoporous silica is 20% of the mass of the Zanthoxylum bungeanum extract solution.

[0078] The mass fraction of the ethanol aqueous solution is 55wt%.

[0079] S4. Spinning The functional factors of Zanthoxylum bungeanum are added into PET slices and mixed evenly, and the fibers containing the functional factors of Zanthoxylum bungeanum are obtained after melt spinning.

[0080] The process parameters of the melt spinning are: the temperature of zone 1 is 295°C, the temperature of zone 2 is 300°C, the temperature of zone 3 is 310°C, and the temperature of zone 4 is 300°C.

[0081] The added amount of the Zanthoxylum bungeanum functional factor is 4% of the mass of the PET slices.

[0082] Embodiment 5: A method for preparing fiber containing Zanthoxylum bungeanum functional factors, the preparation method comprising the following steps: S1. Modification of nanoporous silica The nanoporous silica was added to DMF and evenly dispersed by ultrasonic to obtain a suspension; KH-570 was added to DMF and stirred evenly, and then the suspension was added, reacted at 55° C. for 10 hours, separated after centrifugation, washed with anhydrous ethanol, and dried to obtain nanoporous silica modified with carbon-carbon double bonds.

[0083] The added amount of KH-570 is 26% of the mass of the nanoporous silica.

[0084] The particle size of the nanoporous silica is 100 nm and the pore size is 5 nm.

[0085] S2. Grafting Add carbon-carbon double bond modified nanoporous silica, glycidyl methacrylate and initiator into anhydrous ethanol and stir for 20 minutes at a stirring rate of 300 r / min; heat to 60°C and stir for 5 hours to react, the double bonds in glycidyl methacrylate and the double bonds on the surface of nanoporous silica undergo free radical polymerization, and glycidyl methacrylate is grafted onto the nanoporous silica. After the reaction, centrifuge, filter, wash with anhydrous ethanol and ether, and dry to obtain modified nanoporous silica.

[0086] The mass ratio of the carbon-carbon double bond modified nanoporous silica to glycidyl methacrylate is 4:1.05.

[0087] The initiator is azobisisobutyronitrile, and the added amount is 1% of the mass of glycidyl methacrylate.

[0088] The stirring reaction rate was 100 r / min.

[0089] S3, Load The pepper extract was added to an ethanol aqueous solution and stirred for 20 minutes to obtain a pepper extract solution, and then the modified nanoporous silica was added and stirred for 6 hours to allow the pepper extract to be fully loaded in the porous structure of the modified nanoporous silica, and then dried to obtain the pepper functional factor.

[0090] The mass ratio of the Zanthoxylum bungeanum extract to the ethanol aqueous solution is 1:7.

[0091] The added amount of the modified nanoporous silica is 15% of the mass of the Zanthoxylum bungeanum extract solution.

[0092] The mass fraction of the ethanol aqueous solution is 50wt%.

[0093] S4. Spinning The functional factors of Zanthoxylum bungeanum are added into PET slices and mixed evenly, and the fibers containing the functional factors of Zanthoxylum bungeanum are obtained after melt spinning.

[0094] The process parameters of the melt spinning are: the temperature of zone 1 is 295°C, the temperature of zone 2 is 300°C, the temperature of zone 3 is 310°C, and the temperature of zone 4 is 300°C.

[0095] The added amount of the Zanthoxylum bungeanum functional factor is 3% of the mass of the PET slices.

[0096] Embodiment 6: A method for preparing fiber containing Zanthoxylum bungeanum functional factors, the preparation method comprising the following steps: S1. Modification of nanoporous silica The nanoporous silica was added to DMF and evenly dispersed by ultrasonic to obtain a suspension; KH-570 was added to DMF and stirred evenly, and then the suspension was added, reacted at 70°C for 5 hours, separated after centrifugation, washed with anhydrous ethanol, and dried to obtain nanoporous silica modified with carbon-carbon double bonds.

[0097] The added amount of KH-570 is 34% of the mass of the nanoporous silica.

[0098] The particle size of the nanoporous silica is 150 nm and the pore size is 15 nm.

[0099] S2. Grafting Add carbon-carbon double bond modified nanoporous silica, glycidyl methacrylate and initiator into anhydrous ethanol and stir for 30 minutes at a stirring rate of 400 r / min; heat to 70°C and stir for 7 hours to polymerize the double bonds in glycidyl methacrylate and the double bonds on the surface of nanoporous silica, and glycidyl methacrylate is grafted onto the nanoporous silica. After the reaction, centrifuge, filter, wash with anhydrous ethanol and ether, and dry to obtain modified nanoporous silica.

[0100] The mass ratio of the carbon-carbon double bond modified nanoporous silica to glycidyl methacrylate is 6:1.45.

[0101] The initiator is azobisisobutyronitrile, and the added amount is 2% of the mass of glycidyl methacrylate.

[0102] The stirring reaction rate was 200 r / min.

[0103] S3, Load The pepper extract was added to an ethanol aqueous solution and stirred for 30 minutes to obtain a pepper extract solution, and then the modified nanoporous silica was added and stirred for 12 hours to allow the pepper extract to be fully loaded in the porous structure of the modified nanoporous silica, followed by drying to obtain the pepper functional factor.

[0104] The mass ratio of the Zanthoxylum bungeanum extract to the ethanol aqueous solution is 1:4.

[0105] The added amount of the modified nanoporous silica is 25% of the mass of the Zanthoxylum bungeanum extract solution.

[0106] The mass fraction of the ethanol aqueous solution is 60wt%.

[0107] S4. Spinning The functional factors of Zanthoxylum bungeanum are added into PET slices and mixed evenly, and the fibers containing the functional factors of Zanthoxylum bungeanum are obtained after melt spinning.

[0108] The process parameters of the melt spinning are: the temperature of zone 1 is 295°C, the temperature of zone 2 is 300°C, the temperature of zone 3 is 310°C, and the temperature of zone 4 is 300°C.

[0109] The added amount of the Zanthoxylum bungeanum functional factor is 5% of the mass of the PET slices.

[0110] Comparative Example 1 Representative Example 1 was selected, the functional factor of Zanthoxylum bungeanum was removed, and an equal amount of Zanthoxylum bungeanum extract was directly added to the viscose spinning solution. The rest was consistent with Example 1, as Comparative Example 1.

[0111] Comparative Example 2 Representative Example 4 was selected, the functional factor of Zanthoxylum bungeanum was removed, and an equal amount of Zanthoxylum bungeanum extract was directly added to the PET slices. The rest was consistent with Example 1, as Comparative Example 1.

[0112] Comparative Example 3 Representative Example 1 was selected, the modified nanoporous silica was removed, and unmodified nanoporous silica was used in the loading step. The rest was consistent with Example 1, as Comparative Example 3.

[0113] Comparative Example 4 Representative Example 4 was selected as Comparative Example 3, in which the modified nanoporous silica was removed and unmodified nanoporous silica was used in the loading step, while the rest was consistent with Example 1.

[0114] The properties of the fibers prepared in Examples 1-6 and Comparative Examples 1-4 were tested, as shown in Tables 1 and 2.

[0115] Table 1 (based on viscose fiber) Test items Dry strength (cN / dtex) Wet strength (cN / dtex) Loss rate of active ingredients of Zanthoxylum bungeanum during fiber preparation (%) Antibacterial loss rate after 100 washes (%) Example 1 2.93 2.05 1.06 3.68 Example 2 2.71 1.92 1.35 3.76 Example 3 2.85 1.97 1.24 3.71 Comparative Example 1 1.95 1.02 32 48 Comparative Example 3 2.06 1.13 1.43 21 Table 2 (using polyester substrate) Test items Breaking strength (cN / dtex) Loss rate of active ingredients of Zanthoxylum bungeanum during fiber preparation (%) Antibacterial loss rate after 100 washes (%) Example 4 4.75 1.56 3.23 Example 5 4.23 1.77 3.52 Example 6 4.59 1.64 3.45 Comparative Example 2 3.06 43 45 Comparative Example 4 3.17 1.82 20 It can be seen from Tables 1 and 2 that the fibers using the Zanthoxylum functional factor have better mechanical properties and functional durability, while the strength of the control fiber is poor. This is because the dispersibility of the Zanthoxylum functional factor and nano-silica in the spinning solution and PET chips is poor, while the Zanthoxylum functional factor contains methyl groups on its surface, so it has better dispersibility; and the viscose spinning solution is alkaline. Under alkaline conditions, the epoxy groups in the Zanthoxylum functional factor open the ring and react with the hydroxyl groups on the cellulose macromolecules for cross-linking and grafting; in a high temperature environment, the epoxy groups open the ring and react with the hydroxyl or carboxyl groups in the polyester for cross-linking and grafting, further improving the mechanical properties and functional water-washing resistance of the fiber.

[0116] Nano-silicon dioxide itself has a certain adsorption and protection effect on the active ingredients of Zanthoxylum bungeanum, so the active ingredient loss rate and water washing antibacterial loss rate of Comparative Examples 3 and 4 are better than those of Comparative Examples 1 and 2.

[0117] The fiber containing Zanthoxylum bungeanum functional factors prepared by using Examples 1-6 not only has good mechanical properties, but also has excellent antibacterial and anti-mite effects. After washing 50 times, the antibacterial rates of Staphylococcus aureus, Candida albicans, and Escherichia coli are 97.8% to 99%, 98.1% to 99.2%, and 97.5% to 98.8% (determined in accordance with GB / T 20944.3-2008), and the mite repellent rate is greater than 70% (determined in accordance with the repellent method of GB / T 24253-2009 / 9.1).

[0118] Unless otherwise specified, the ratios and percentages described in the present invention are all weight ratios and weight percentages; and the raw materials are all commercially available.

[0119] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention is described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for preparing fiber containing Zanthoxylum bungeanum functional factors, characterized in that: The preparation method comprises modification, grafting, loading and spinning of nanoporous silica.

2. The method for preparing a fiber containing Zanthoxylum bungeanum functional factors according to claim 1, characterized in that: The modification of the nanoporous silica is as follows: adding the nanoporous silica to DMF and uniformly dispersing it by ultrasonication to obtain a suspension; adding KH-570 to the DMF and stirring evenly, then adding the suspension, reacting at 55-70° C. for 5-10 hours, separating after centrifugation, washing with anhydrous ethanol, and drying to obtain the nanoporous silica modified with carbon-carbon double bonds.

3. The method for preparing a fiber containing Zanthoxylum bungeanum functional factors according to claim 2, characterized in that: The amount of KH-570 added is 26-34% of the mass of the nanoporous silica; The particle size of the nanoporous silica is 100-150 nm, and the pore size is 5-15 nm.

4. The method for preparing a fiber containing Zanthoxylum bungeanum functional factors according to claim 1, characterized in that: The grafting comprises the following steps: adding carbon-carbon double bond modified nanoporous silica, glycidyl methacrylate and an initiator into anhydrous ethanol and stirring for 20 to 30 minutes at a stirring rate of 300 to 400 r / min; heating to 60 to 70° C. and stirring for reaction for 5 to 7 hours; centrifuging, filtering, washing with anhydrous ethanol and ether, and drying after the reaction is completed to obtain the modified nanoporous silica.

5. The method for preparing a fiber containing Zanthoxylum bungeanum functional factors according to claim 4, characterized in that: The mass ratio of the carbon-carbon double bond modified nanoporous silica to glycidyl methacrylate is 4-6:1.05-1.

45.

6. The method for preparing a fiber containing Zanthoxylum bungeanum functional factors according to claim 4, characterized in that: The initiator is azobisisobutyronitrile, and the amount added is 1-2% of the mass of glycidyl methacrylate; The stirring reaction rate is 100-200 r / min.

7. The method for preparing a fiber containing Zanthoxylum bungeanum functional factors according to claim 1, characterized in that: The loading method comprises adding the Zanthoxylum bungeanum extract to an ethanol aqueous solution and stirring for 20 to 30 minutes to obtain a Zanthoxylum bungeanum extract solution, then adding the modified nanoporous silica and stirring for 6 to 12 hours to allow the Zanthoxylum bungeanum extract to be fully loaded in the porous structure of the modified nanoporous silica, and then drying to obtain the Zanthoxylum bungeanum functional factor.

8. The method for preparing a fiber containing Zanthoxylum bungeanum functional factors according to claim 7, characterized in that: The mass ratio of the Zanthoxylum bungeanum extract to the ethanol aqueous solution is 1:4-7; The amount of modified nanoporous silica added is 15-25% of the mass of the pepper extract solution; The mass fraction of the ethanol aqueous solution is 50-60wt%.

9. The method for preparing a fiber containing Zanthoxylum bungeanum functional factors according to claim 1, characterized in that: The spinning process comprises adding the Zanthoxylum bungeanum functional factor into the spinning solution or polymer slices by a method of adding before spinning and mixing them evenly, and obtaining the fiber containing the Zanthoxylum bungeanum functional factor by wet spinning or melt spinning.

10. The method for preparing fiber containing Zanthoxylum bungeanum functional factors according to claim 9, characterized in that: The spinning solution is viscose spinning solution or acrylic spinning solution; the polymer slices are one or more of PET slices, PA6 slices, and PA66; The added amount of the Zanthoxylum bungeanum functional factor is 3-5% of the effective components of the spinning solution or the mass of the polymer slices.