Preparation method of viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules
Through the preparation method of viscose fiber with mugwort essential oil/paraffinium double-layer microcapsules, the single performance and stability of phase change materials in textiles are solved, and the efficient antibacteriality and softness of the fiber are achieved, and the stability and functionality of the spinning process are improved.
Patent Information
- Application Number
- CN202510920419.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-04
- Publication Date
- 2025-08-29
- Estimated Expiration
- 2045-07-04
AI Technical Summary
When used in textiles, existing phase change materials have problems such as single performance, easy leakage, limited phase change range and poor thermal conductivity. The method of embedding functional materials into the fibers poses high cost and stability risks.
The viscose fiber preparation method of mugwort essential oil/paraffinium double-layer microcapsules is used to improve the dispersion and interface combination of microcapsules through modification enhancer and modified nanosheets. The polyurethane inner shell and polyurea shell structure are used to coat mugwort essential oil to enhance the antibacterial properties and ultraviolet shielding function of the fibers, and the microcapsules are embedded into the fibers through electrospinning.
The mechanical properties and antibacterial properties of the fiber are significantly optimized, ensuring the sustained release effect of mugwort essential oil, avoiding volatility and oxidation, and improving the stability of the spinning process and the softness and moisture absorption and breathability of the functional fibers.
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Figure CN120425475B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of viscose fiber preparation, and in particular to a method for preparing viscose fiber based on wormwood essential oil / paraffin double-layer microcapsules. Background Art
[0002] Currently, the main sources of energy include fossil fuels (coal, oil, and natural gas), nuclear energy, and renewable energy (solar energy, wind energy, hydropower, biomass energy, and geothermal energy). Fossil fuels release carbon dioxide and harmful gases during use, and most fossil fuels are becoming scarce due to human mining and exploration. To address energy shortages, reduce environmental impacts, and improve energy security, researchers are working to increase the utilization and scope of renewable and clean energy. Phase change materials, as a relatively common energy storage material, offer the advantages of non-toxicity and wide application. They are widely used in temperature regulation and energy management in buildings, solar energy systems, and electronic devices that regulate human body temperature. Because phase change materials absorb or release energy during phase changes, they can reduce energy consumption in air conditioners, heaters, and electronic temperature control devices. Phase change materials also play an important role in increasing the utilization and scope of renewable energy. Common phase change materials are mainly divided into organic phase change materials with lower phase change temperatures and inorganic phase change materials with higher phase change temperatures. Organic phase change materials mostly undergo solid-liquid phase transitions, and their temperature regulation mechanism involves absorbing or releasing heat within a certain temperature range. Therefore, organic phase change materials have the disadvantages of single performance, easy leakage, limited phase change range, and poor thermal conductivity. Microencapsulation is often used to overcome these limitations of phase change materials. Common phase change microcapsules include high-potential phase change microcapsules, multifunctional phase change microcapsules (such as antibacterial and temperature-regulating microcapsules, photothermal phase change microcapsules, and infrared phase change microcapsules), and high thermal conductivity phase change microcapsules.
[0003] As the global greenhouse effect continues to intensify, solving the problems of extreme high temperatures and bacterial growth has become imperative, and promoting energy conservation and environmental protection is crucial. Textiles are a protective layer for the human body, so various methods for preparing smart textiles have attracted widespread attention, such as combining hollow fibers with functional materials, surface finishing of fabric surfaces, and the use of surface grafting modification to prepare functional textiles. Although the application of injecting functional materials into hollow fibers and functional finishing on the surface of fabrics is common, they also have certain limitations, such as the high cost of preparing hollow fibers and the risk of degradation of surface finishing agents over time. In contrast, embedding phase change materials into fibers through electrospinning or wet spinning is a promising approach. Generally, adding microcapsules to the spinning solution has minimal effect on the chemical properties of the fiber and also ensures the softness, moisture absorption and breathability of the functional fabric.
[0004] However, integrating microcapsules into the spinning solution requires attention to factors such as the dispersibility of the microcapsules in the spinning solution and their impact on the mechanical properties of the functional fibers spun. Therefore, it is particularly important to select a dispersant that is miscible with the viscose spinning solution and can improve the adverse effects of microcapsules in the fiber. In practical applications, functional fibers with antibacterial effects and energy storage are suitable for military and outdoor fields. Viscose fibers have a sense of comfort that most chemical fibers do not have, and embedding microcapsules into the fibers can retain this advantage to a great extent. In short, the research on more comfortable and environmentally friendly multifunctional clothing has great prospects. Summary of the Invention
[0005] In view of the shortcomings of the prior art, the object of the present invention is to provide a method for preparing viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules.
[0006] To achieve the above object, the present invention provides the following technical solutions:
[0007] A method for preparing viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules, comprising the following preparation steps:
[0008] S1. Preparation of mugwort essential oil / paraffin double-layer microcapsules:
[0009] S11. Preparation of the oil phase: 47-50 parts of wormwood essential oil, 12-15 parts of paraffin slices, 200-250 parts of the oil phase modifier were ultrasonically treated for 10-15min at a frequency of 40kHz to obtain an oil phase;
[0010] S12 preparation of the aqueous phase: 3-6 parts of gum arabic, 4-7 parts of sodium dodecylbenzenesulfonate and 0.5-1 parts of the modified nanosheets were added to 100-120 parts of deionized water and stirred continuously until completely dissolved to obtain an aqueous phase;
[0011] S13. The aqueous phase and the oil phase were mixed and stirred at a high shear speed of 10,000 rpm / min using a homogenizer for 5-8 minutes. After ultrasonic treatment for 25-30 minutes, 2-4 drops of dibutyltin disilicate were added at 30°C while stirring at 2,500 rpm / min for 5-8 minutes. The temperature was raised to 40°C to initially form a polyurethane inner shell, and the reaction was continued with stirring at 1,800 rpm / min for 5-8 minutes.
[0012] S14. 20-25 parts of an aqueous solution of tetraethylene pentamine were added dropwise to the mixture obtained in step S13, and the temperature was raised to 50°C, the speed was adjusted to 600 rpm / min, and the polymerization reaction was carried out at 70°C for 2-3h, followed by slowly adding 5-7 parts of an aqueous solution of tetraethylene pentamine dropwise, and the reaction was continued for 40-45min to form a polyurea shell;
[0013] S15. The product obtained in step S14 was washed three times with petroleum ether and deionized water and dried in an oven at 35 ° C for 0.5-1h to obtain wormwood essential oil / paraffin double-layer microcapsules;
[0014] S2. Preparation of microcapsule spinning solution: 7-10 parts of the spinning solution and 2-4 parts of wormwood essential oil / paraffin double-layer microcapsule suspension were mixed and magnetically stirred for 40-50 min to achieve complete homogenization. 0.6-1 parts of sodium alginate were added to the spinning solution in 3-5 portions and magnetically stirred for 1-2 h to obtain a microcapsule spinning solution;
[0015] S3 spinning: The microcapsule spinning solution obtained in step S3 is pressed into a nozzle immersed in a coagulation bath by a spinning pump, and the viscose stream ejected from the spinneret decomposes and coagulates in the coagulation bath to obtain viscose fibers based on wormwood essential oil / paraffin double-layer microcapsules;
[0016] Wherein, the preparation of the oil phase modifier comprises the following steps:
[0017] S31 was added 74-80 parts of petroleum ether in 165-170 parts of isophorone diisocyanate, stirred at a speed of 400-450rpm / min for 15-20min to obtain a mixture;
[0018] S32. Add 3-5 parts of a modifier enhancer, 4-8 parts of polyethylene glycol, and 2-4 parts of triphenyl phosphate to the mixture, and ultrasonically treat for 15-20 minutes to obtain an oil phase modifier.
[0019] Preferably, the preparation of the modified nanosheets in step S12 comprises the following steps:
[0020] S21. The montmorillonite was dispersed in deionized water to form a uniform suspension, and then a 5% concentration of zinc acetate solution was added and stirred at a speed of 400-450rpm / min for 0.5-1h to obtain a precursor mixture;
[0021] S22. Sodium hydroxide solution was added to the precursor mixture to adjust the solution to alkaline, and a hydrothermal reaction was carried out at 120-150 ° C for 8-12h;
[0022] S23. The product obtained from the hydrothermal reaction in step S22 is cooled and centrifuged, washed with deionized water until neutral, and finally dried to obtain modified nanosheets.
[0023] Preferably, the preparation of the modifying enhancer in step S32 comprises the following steps:
[0024] S41. 8-10 parts of nano-silica were dispersed in 150-170 parts of anhydrous ethanol, ultrasonically treated at a frequency of 40 kHz for 20-30 min, and then 2-4 parts of γ-aminopropyltriethoxysilane were added and stirred at 50-60 ° C for 3-4h to obtain modified nano-silica;
[0025] S42. Add 3-5 parts of dicumyl peroxide and 2-4 parts of antioxidant 1010 to the modified nano-silica and stir for 0.5-1 hour to finally obtain a modified reinforcing agent.
[0026] Preferably, the coagulation bath composition is 120 g / L sulfuric acid, 15 g / L zinc sulfate and 220 g / L sodium sulfate.
[0027] Preferably, the spinning parameters in step S3 are as follows: the injection pump speed is 25 mL / h, the needle inner diameter is 0.33 mm, the needle outer diameter is 0.64 mm, and the draft ratio is 2 times.
[0028] Preferably, the tetraethylene pentamine aqueous solution in step S14 is a tetraethylene pentamine aqueous solution with a mass concentration of 7%.
[0029] Preferably, the frequency of the ultrasonic treatment in step S32 is 40 kHz and the temperature is 30°C.
[0030] Preferably, during the preparation of the modifying and reinforcing agent, the stirring speed is 450-500 rpm / min.
[0031] Preferably, in step S21, the mass ratio of montmorillonite to the zinc acetate solution with a mass concentration of 5% is 1:2-5.
[0032] Compared with the prior art, the present invention has the following beneficial effects:
[0033] 1. The present invention significantly optimizes the mechanical properties of viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules through the modified reinforcing agent, enhances the interface bonding between the microcapsules and the viscose fiber, and reduces the breakage rate during the spinning process.
[0034] 2. The present invention utilizes the aqueous phase prepared with modified nanosheets to improve the flame retardant properties of the mugwort essential oil / paraffin double-layer microcapsules, thereby enhancing the antibacterial and ultraviolet shielding functions of the viscose fiber based on the mugwort essential oil / paraffin double-layer microcapsules of the present invention.
[0035] 3. By encapsulating mugwort essential oil in double-layer microcapsules, this invention fully leverages its natural antibacterial properties. The main active ingredients of mugwort essential oil (such as eucalyptol and flavonoids) are continuously released through the microcapsule's sustained-release mechanism, significantly inhibiting the growth of common pathogens such as Escherichia coli and Staphylococcus aureus. Furthermore, the double-layer structure of the microcapsules (polyurethane inner shell and polyurea outer shell) effectively prevents volatilization and oxidation of the mugwort essential oil during the spinning process, ensuring a long-lasting antibacterial effect. BRIEF DESCRIPTION OF THE DRAWINGS
[0036] Figure 1 The present invention is a flow chart of the preparation process of viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules;
[0037] Figure 2 The infrared spectra of the mugwort essential oil / paraffin double-shell microcapsules and their core materials and shell materials of the present invention are as follows: a is the infrared spectra of the mugwort essential oil / paraffin double-shell microcapsules, mugwort essential oil and paraffin; b is the infrared spectra of the polyurethane and polyurea shell materials of the mugwort essential oil / paraffin double-shell microcapsules;
[0038] Figure 3 The particle size distribution diagram of the mugwort essential oil / paraffin double-layer microcapsules with different core-to-wall ratios of the present invention;
[0039] Figure 4 This is a scene diagram of the leakage performance experiment of the mugwort essential oil / paraffin double-layer microcapsules of the present invention;
[0040] Figure 5 The SEM images of the wormwood essential oil / paraffin double-layer microcapsules of the present invention in different environments, wherein a is a SEM image of the wormwood essential oil / paraffin double-layer microcapsules without pH treatment, b is a SEM image of the wormwood essential oil / paraffin double-layer microcapsules immersed in a hydrochloric acid solution with a concentration of 2 g / L for 24 h, c is a SEM image of the wormwood essential oil / paraffin double-layer microcapsules immersed in a sulfuric acid solution with a concentration of 2 g / L for 24 h, and d is a SEM image of the wormwood essential oil / paraffin double-layer microcapsules immersed in a sodium hydroxide solution with a concentration of 3 g / L for 24 h;
[0041] Figure 6 The thermogravimetric curves and DTG curves of the mugwort essential oil / paraffin double-layer microcapsules, mugwort essential oil, paraffin, viscose fiber and functional viscose fiber of the present invention are shown, wherein a is the thermogravimetric curve and b is the DTG curve;
[0042] Figure 7 The DSC thermograms of the mugwort essential oil / paraffin double-layer microcapsules with different core-to-wall ratios of the present invention and viscose fibers with a mugwort essential oil / paraffin double-layer microcapsule content of 1% and 3%, wherein a is the DSC thermogram of the mugwort essential oil / paraffin double-layer microcapsules with different core-to-wall ratios, and b is the DSC thermogram of the viscose fibers with a mugwort essential oil / paraffin double-layer microcapsule content of 1% and 3%;
[0043] Figure 8 The histogram shows the antibacterial effect of the mugwort essential oil / paraffin double-layer microcapsules with different core-shell ratios on Escherichia coli.
[0044] Figure 9This is a schematic diagram of the effect of the mugwort essential oil / paraffin double-layer microcapsules and functional viscose fiber on the antibacterial activity of Escherichia coli of the present invention, wherein ad is mugwort essential oil / paraffin double-layer microcapsules with core-to-wall ratios of 1:1.9, 1:1.6, 1:1.4, and 1:1, respectively, e is viscose fiber, f is functional viscose fiber with a mugwort essential oil / paraffin double-layer microcapsule content of 3%, g is functional viscose fiber with 3% mugwort essential oil / paraffin double-layer microcapsules added with sodium alginate, and h is a sterilization process diagram of functional viscose fiber. DETAILED DESCRIPTION
[0045] The present invention will be described clearly and completely below in conjunction with the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention.
[0046] See also Figure 1-9 , the present invention provides a technical solution:
[0047] Example 1
[0048] A method for preparing viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules:
[0049] S1. Preparation of mugwort essential oil / paraffin double-layer microcapsules:
[0050] S11. Preparation of the oil phase: 47 g of wormwood essential oil, 12 g of paraffin slices, and 200 mL of an oil phase modifier were ultrasonically treated for 10 min at a frequency of 40 kHz to obtain an oil phase;
[0051] S12. Preparation of the aqueous phase: 3 g of gum arabic, 4 g of sodium dodecylbenzenesulfonate and 0.5 g of the modified nanosheets were added to 100 mL of deionized water and stirred continuously until completely dissolved to obtain an aqueous phase;
[0052] S13. The aqueous phase and the oil phase were mixed and stirred at 10,000 rpm / min using a homogenizer for 5 minutes. After ultrasonic treatment for 25 minutes, 2 drops of dibutyltin dilaurate were added at 30°C while stirring at 2,500 rpm / min for 5 minutes. The temperature was raised to 40°C to initially form a polyurethane inner shell. The reaction was then stirred at 1,800 rpm / min for 5 minutes.
[0053] S14. 20 mL of a 7% aqueous solution of tetraethylene pentamine was added dropwise to the mixture obtained in step S13, and the temperature was raised to 50 ° C, the speed was adjusted to 600 rpm / min, and the polymerization reaction was carried out at 70 ° C for 2 h, and then 5 mL of a 7% aqueous solution of tetraethylene pentamine was slowly added dropwise, and the reaction was continued for 40 min to form a polyurea shell;
[0054] S15. The product obtained in step S14 was washed three times with petroleum ether and deionized water and dried in an oven at 35 ° C for 0.5 h to obtain wormwood essential oil / paraffin double-layer microcapsules;
[0055] S2. Preparation of microcapsule spinning solution: 7 mL of spinning solution and 2 g of wormwood essential oil / paraffin bilayer microcapsule suspension were mixed and magnetically stirred for 40 min to achieve complete homogenization. 0.6 g of sodium alginate was added to the spinning solution in three portions and magnetically stirred for 1 h to obtain a microcapsule spinning solution;
[0056] S3. The microcapsule spinning solution obtained in step S3 is pressed into a nozzle immersed in a coagulation bath through a spinning pump. The viscose stream ejected from the spinneret decomposes and coagulates in the coagulation bath, ultimately obtaining viscose fibers based on wormwood essential oil / paraffin double-layer microcapsules;
[0057] The preparation of the modified nanosheets comprises the following steps:
[0058] S21. The montmorillonite was dispersed in deionized water to form a uniform suspension, and then a 5% zinc acetate solution (2 times the amount of montmorillonite) was added and stirred at 400 rpm / min for 0.5 h to obtain a precursor mixture;
[0059] S22. Sodium hydroxide solution was added to the precursor mixture to adjust the solution to alkaline, and a hydrothermal reaction was carried out at 120 ° C for 8 h;
[0060] S23. The product obtained by the hydrothermal reaction in step S122 is cooled, centrifuged, washed with deionized water until neutral, and dried to obtain modified nanosheets;
[0061] The preparation of the oil phase modifier comprises the following steps:
[0062] S31 was added 74g of petroleum ether to 165g of isophorone diisocyanate and stirred at a speed of 400rpm / min for 15min to obtain a mixture;
[0063] S32. 3 g of a modifier enhancer, 4 g of polyethylene glycol, and 2 g of triphenyl phosphate were added to the mixture and sonicated (40 kHz, 30°C) for 15 min to obtain an oil phase modifier.
[0064] The preparation of the modified reinforcing agent comprises the following steps:
[0065] S41. 8 g of nano-silica was dispersed in 150 mL of anhydrous ethanol, ultrasonicated at a frequency of 40 kHz for 20 min, and then 2 g of γ-aminopropyltriethoxysilane was added. The mixture was stirred at 450 rpm / min for 3 h at 50 ° C to obtain modified nano-silica;
[0066] S42. Add 3 g of dicumyl peroxide and 2 g of antioxidant 1010 to the modified nano-silica, and stir at a speed of 450 rpm / min for 0.5 h to finally obtain a modified reinforcing agent.
[0067] Example 2
[0068] A method for preparing viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules:
[0069] S1. Preparation of mugwort essential oil / paraffin double-layer microcapsules:
[0070] S11. Preparation of the oil phase: 50 g of wormwood essential oil, 15 g of paraffin slices, 250 mL of an oil phase modifier were ultrasonically treated for 15 min at a frequency of 40 kHz to obtain an oil phase;
[0071] S12. Preparation of the aqueous phase: 6 g of gum arabic, 7 g of sodium dodecylbenzenesulfonate and 1 g of modified nanosheets were added to 120 mL of deionized water and stirred continuously until completely dissolved to obtain an aqueous phase;
[0072] S13. The aqueous phase and the oil phase were mixed and stirred at 10,000 rpm / min using a homogenizer for 8 minutes. After ultrasonic treatment for 30 minutes, 4 drops of dibutyltin dilaurate were added at 30°C while stirring at 2,500 rpm / min for 8 minutes. The temperature was raised to 40°C to initially form a polyurethane inner shell, and the reaction was continued with stirring at 1,800 rpm / min for 8 minutes.
[0073] S14. 25 mL of a 7% aqueous solution of tetraethylene pentamine was added dropwise to the mixture obtained in step S13, and the temperature was raised to 50 ° C, the speed was adjusted to 600 rpm / min, and the polymerization reaction was carried out at 70 ° C for 3 h, and then 7 mL of a 7% aqueous solution of tetraethylene pentamine was slowly added dropwise, and the reaction was continued for 45 min to form a polyurea shell;
[0074] S15. The product obtained in step S14 was washed three times with petroleum ether and deionized water and dried in an oven at 35 ° C for 1 h to obtain wormwood essential oil / paraffin double-layer microcapsules;
[0075] S2. Preparation of microcapsule spinning solution: 10 mL of the spinning solution and 4 g of the mugwort essential oil / paraffin double-layer microcapsule suspension were mixed and magnetically stirred for 50 min to achieve complete homogenization. 1 g of sodium alginate was added to the spinning solution in 5 portions and magnetically stirred for 2 h to obtain a microcapsule spinning solution;
[0076] S3. The microcapsule spinning solution obtained in step S3 is pressed into a nozzle immersed in a coagulation bath through a spinning pump. The viscose stream ejected from the spinneret decomposes and coagulates in the coagulation bath, ultimately obtaining viscose fibers based on wormwood essential oil / paraffin double-layer microcapsules;
[0077] The preparation of the modified nanosheets comprises the following steps:
[0078] S21. The montmorillonite was dispersed in deionized water to form a uniform suspension, and then a 5% zinc acetate solution (5 times the amount of montmorillonite) was added and stirred at 450 rpm / min for 1 h to obtain a precursor mixture;
[0079] S22. Sodium hydroxide solution was added to the precursor mixture to adjust the solution to alkaline, and a hydrothermal reaction was carried out at 150 ° C for 12 h;
[0080] S23. The product obtained by the hydrothermal reaction in step S122 is cooled, centrifuged, washed with deionized water until neutral, and dried to obtain modified nanosheets;
[0081] The preparation of the oil phase modifier comprises the following steps:
[0082] S31 was added 80g of petroleum ether in 170g of isophorone diisocyanate and stirred at a speed of 450rpm / min for 20min to obtain a mixture;
[0083] S32. 5 g of a modifier enhancer, 8 g of polyethylene glycol, and 4 g of triphenyl phosphate were added to the mixture and sonicated (40 kHz, 30°C) for 20 min to obtain an oil phase modifier.
[0084] The preparation of the modified reinforcing agent comprises the following steps:
[0085] S41. 10 g of nano-silica was dispersed in 170 mL of anhydrous ethanol, ultrasonicated at a frequency of 40 kHz for 30 min, and then 4 g of γ-aminopropyltriethoxysilane was added. The mixture was stirred at 500 rpm / min for 4 h at 60 ° C to obtain modified nano-silica;
[0086] S42. Add 5 g of dicumyl peroxide and 4 g of antioxidant 1010 to the modified nano-silica, and stir at a speed of 500 rpm / min for 1 hour to finally obtain a modified reinforcing agent.
[0087] Example 3
[0088] A method for preparing viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules:
[0089] S1. Preparation of mugwort essential oil / paraffin double-layer microcapsules:
[0090] S11. Preparation of the oil phase: 48 g of wormwood essential oil, 13 g of paraffin slices, 220 mL of an oil phase modifier were ultrasonically treated for 11 min at a frequency of 40 kHz to obtain an oil phase;
[0091] S12. Preparation of the aqueous phase: 4 g of gum arabic, 5 g of sodium dodecylbenzenesulfonate and 0.6 g of modified nanosheets were added to 110 mL of deionized water and stirred continuously until completely dissolved to obtain an aqueous phase;
[0092] S13. The aqueous phase and the oil phase were mixed and stirred at 10,000 rpm / min using a homogenizer for 6 minutes. After ultrasonic treatment for 26 minutes, 3 drops of dibutyltin dilaurate were added at 30°C while stirring at 2,500 rpm / min for 6 minutes. The temperature was raised to 40°C to initially form a polyurethane inner shell, and the reaction was continued with stirring at 1,800 rpm / min for 6 minutes.
[0093] S14. 21 mL of a 7% aqueous solution of tetraethylene pentamine was added dropwise to the mixture obtained in step S13, and the temperature was raised to 50°C, the speed was adjusted to 600 rpm / min, and the polymerization reaction was carried out at 70°C for 2.5 h, followed by the slow addition of 6 mL of a 7% aqueous solution of tetraethylene pentamine, and the reaction was continued for 41 min to form a polyurea shell;
[0094] S15. The product obtained in step S14 was washed three times with petroleum ether and deionized water and dried in an oven at 35 ° C for 0.6 h to obtain wormwood essential oil / paraffin double-layer microcapsules;
[0095] S2. Preparation of microcapsule spinning solution: 8 mL of spinning solution and 3 g of wormwood essential oil / paraffin double-layer microcapsule suspension were mixed and magnetically stirred for 42 min to achieve complete homogenization. 0.8 g of sodium alginate was added to the spinning solution in four portions and magnetically stirred for 1.2 h to obtain a microcapsule spinning solution;
[0096] S3. The microcapsule spinning solution obtained in step S3 is pressed into a nozzle immersed in a coagulation bath through a spinning pump. The viscose stream ejected from the spinneret decomposes and coagulates in the coagulation bath, ultimately obtaining viscose fibers based on wormwood essential oil / paraffin double-layer microcapsules;
[0097] The preparation of the modified nanosheets comprises the following steps:
[0098] S21. The montmorillonite was dispersed in deionized water to form a uniform suspension, and then a 5% zinc acetate solution was added (the amount added was 3 times that of the montmorillonite), and stirred at a speed of 420 rpm / min for 0.6h to obtain a precursor mixture;
[0099] S22. Sodium hydroxide solution was added to the precursor mixture to adjust the solution to alkaline, and a hydrothermal reaction was carried out at 130 ° C for 9 h;
[0100] S23. The product obtained by the hydrothermal reaction in step S122 is cooled, centrifuged, washed with deionized water until neutral, and dried to obtain modified nanosheets;
[0101] The preparation of the oil phase modifier comprises the following steps:
[0102] S31 was added 75g of petroleum ether to 166g of isophorone diisocyanate and stirred at a speed of 420rpm / min for 16min to obtain a mixture;
[0103] S32. 4 g of a modifier enhancer, 5 g of polyethylene glycol, and 3 g of triphenyl phosphate were added to the mixture and sonicated (40 kHz, 30°C) for 16 min to obtain an oil phase modifier.
[0104] The preparation of the modified reinforcing agent comprises the following steps:
[0105] S41. 9 g of nano-silica was dispersed in 155 mL of anhydrous ethanol and ultrasonically treated at a frequency of 40 kHz for 22 min. 3 g of γ-aminopropyltriethoxysilane was added and stirred at 460 rpm / min at 52 ° C for 3.2 h to obtain modified nano-silica.
[0106] S42. Add 4 g of dicumyl peroxide and 3 g of antioxidant 1010 to the modified nano-silica, and stir at a speed of 460 rpm / min for 0.7 h to finally obtain a modified reinforcing agent.
[0107] Example 4
[0108] A method for preparing viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules:
[0109] S1. Preparation of mugwort essential oil / paraffin double-layer microcapsules:
[0110] S11. Preparation of the oil phase: 49 g of wormwood essential oil, 14 g of paraffin slices, and 240 mL of an oil phase modifier were ultrasonically treated for 14 min at a frequency of 40 kHz to obtain an oil phase;
[0111] S12. Preparation of the aqueous phase: 5 g of gum arabic, 6 g of sodium dodecylbenzenesulfonate and 0.8 g of modified nanosheets were added to 115 mL of deionized water and stirred continuously until completely dissolved to obtain an aqueous phase;
[0112] S13. The aqueous phase and the oil phase were mixed and stirred at 10,000 rpm / min using a homogenizer for 7 minutes. After ultrasonic treatment for 28 minutes, 3 drops of dibutyltin dilaurate were added at 30°C while stirring at 2,500 rpm / min for 7 minutes. The temperature was raised to 40°C to initially form a polyurethane inner shell. The reaction was then stirred at 1,800 rpm / min for 7 minutes to form a polyurea outer shell.
[0113] S14. 24 mL of a 7% aqueous solution of tetraethylene pentamine was added dropwise to the mixture obtained in step S13, and the temperature was raised to 50 ° C, the speed was adjusted to 600 rpm / min, and the polymerization reaction was carried out at 70 ° C for 2.8 h, and then 6 mL of a 7% aqueous solution of tetraethylene pentamine was slowly added dropwise, and the reaction was continued for 44 min;
[0114] S15. The product obtained in step S14 was washed three times with petroleum ether and deionized water and dried in an oven at 35 ° C for 0.8 h to obtain wormwood essential oil / paraffin double-layer microcapsules;
[0115] S2. Preparation of microcapsule spinning solution: 9 mL of spinning solution and 3.5 g of wormwood essential oil / paraffin double-layer microcapsule suspension were mixed and magnetically stirred for 48 min to achieve complete homogenization. 0.8 g of sodium alginate was added to the spinning solution in four portions and magnetically stirred for 1.6 h to obtain a microcapsule spinning solution;
[0116] S3. The microcapsule spinning solution obtained in step S3 is pressed into a nozzle immersed in a coagulation bath through a spinning pump. The viscose stream ejected from the spinneret decomposes and coagulates in the coagulation bath, ultimately obtaining viscose fibers based on wormwood essential oil / paraffin double-layer microcapsules;
[0117] The preparation of the modified nanosheets comprises the following steps:
[0118] S21. The montmorillonite was dispersed in deionized water to form a uniform suspension, and then a 5% zinc acetate solution was added (the amount added was 4 times that of the montmorillonite), and stirred at 440 rpm / min for 0.8h to obtain a precursor mixture;
[0119] S22. Sodium hydroxide solution was added to the precursor mixture to adjust the solution to alkaline, and a hydrothermal reaction was carried out at 140 ° C for 11 h;
[0120] S23. The product obtained by the hydrothermal reaction in step S122 is cooled, centrifuged, washed with deionized water until neutral, and dried to obtain modified nanosheets;
[0121] The preparation of the oil phase modifier comprises the following steps:
[0122] S31 was added 78g of petroleum ether to 165g of isophorone diisocyanate and stirred at a speed of 440rpm / min for 18min to obtain a mixture;
[0123] S32. 4 g of a modifier enhancer, 7 g of polyethylene glycol, and 3.5 g of triphenyl phosphate were added to the mixture and sonicated (40 kHz, 30°C) for 18 min to obtain an oil phase modifier.
[0124] The preparation of the modified reinforcing agent comprises the following steps:
[0125] S41. 9 g of nano-silica was dispersed in 165 g of anhydrous ethanol, ultrasonicated at a frequency of 40 kHz for 28 min, and then 3 g of γ-aminopropyltriethoxysilane was added. The mixture was stirred at a speed of 480 rpm / min at 58 ° C for 3.8 h to obtain modified nano-silica;
[0126] S42. Add 4.5 g of dicumyl peroxide and 3.5 g of antioxidant 1010 to the modified nano-silica, and stir at a speed of 480 pm / min for 0.8 h to finally obtain a modified reinforcing agent.
[0127] Performance testing:
[0128] By controlling the preparation process parameters of Examples 1-4 of the present invention, the core-to-wall ratios of the mugwort essential oil / paraffin double-layer microcapsules obtained were 1:1.9, 1:1.6, 1:1.4 and 1:1, respectively, corresponding to Examples 1-4.
[0129] 1. Infrared spectroscopy analysis of mugwort essential oil / paraffin double-layer microcapsules
[0130] The synthesis reaction mechanism of mugwort essential oil / paraffin double-shell microcapsules was explored, and the infrared spectra of the microcapsules and their two core materials (mugwort essential oil and sliced paraffin) and double-shell materials (polyurea and polyurethane) were analyzed. Figure 2 As shown, Figure 2 a is the infrared spectrum of mugwort essential oil / paraffin double-shell microcapsules, mugwort essential oil and paraffin, Figure 2 b is the infrared spectrum of polyurethane and polyurea, the shell materials of mugwort essential oil / paraffin double-shell microcapsules. Figure 2 a and Figure 2 As shown in b, the spectra of microcapsules and paraffin are both at 1471 cm −1There is a characteristic band at 1646-1543 cm-1, indicating the bending vibration in the CH plane. In addition, the carbonylation peak is at 1646-1543 cm-1. -1 range, while the stretching vibration peak of -NH appears at 3279cm -1 , -CH peak falls at 3000-2800cm -1 The range is consistent with the formation process of polyurethane and polyurea. It is worth noting that the same absorption peak is observed in the spectrum of microcapsules. As expected, the infrared spectrum of wormwood essential oil has a peak at 1725 cm −1 and 1263cm −1 There are two characteristic peaks at 1725cm −1 The peak at 1263 cm corresponds to the acyl group, while the peak at 1263 cm −1 The peaks correspond to the stretching rotation patterns of CO and COC, which are characteristic of triterpenes and eucalyptol compounds, the main components of wormwood essential oil. It is worth noting that the microcapsules also have a peak at 1725 cm -1 and 1263cm -1 The results show the same absorption peak at , which confirms that the shell material of the wormwood essential oil / paraffin double-layer microcapsules includes polyurethane and polyurea, while the core material includes paraffin and wormwood essential oil.
[0131] 2. Particle size analysis and acid and alkali resistance test of mugwort essential oil / paraffin double-shell microcapsules
[0132] The particle size of microcapsules with core-to-wall ratios of 1:1.9, 1:1.6, 1:1.4 and 1:1 was analyzed. Figure 3 The average particle sizes of the wormwood oil / paraffin double-shell microcapsules were found to be 526.8 nm, 586.2 nm, 388.1 nm, and 618.0 nm, respectively, with increasing core material content. The average diameter initially increased, then decreased, and finally increased again with increasing core material content. This variation suggests that the degree of core material encapsulation in the wormwood oil / paraffin double-shell microcapsules affects their overall size. Optimal encapsulation is key to controlling the size of wormwood oil / paraffin double-shell microcapsules. Too little core material results in a thicker shell and a larger average particle size, while too much core material impedes complete shell coverage and results in a wider particle size distribution. A core-to-wall ratio of 1:1.4 results in the smallest particle size and the narrowest particle size range. During integration with the spinning solution, the smaller particle size enhances dispersant adsorption per unit surface area and increases electrostatic repulsion and steric hindrance between the wormwood oil / paraffin double-shell microcapsules. Therefore, selecting mugwort essential oil / paraffin double-shell microcapsules with small size and narrow distribution is beneficial to improving the dispersion stability in viscose spinning solution.
[0133] To further verify that the microcapsule shell material completely encapsulates the core material, a double-layer microcapsule of wormwood essential oil / paraffin wax with a core-to-wall ratio of 1:1.4 and sliced paraffin wax were placed on filter paper and heated at 65 °C for 15 minutes. During this process, the paraffin wax melted and permeated through the filter paper. At this time, a few drops of red dye were added to the two filter papers that had been exposed to different materials. Figure 4 As shown, the filter paper soaked in paraffin remained colorless, indicating that the dye was unable to penetrate the filter paper due to being isolated by the paraffin. In contrast, the filter paper exposed to the mugwort essential oil / paraffin bilayer microcapsules was completely dyed red by the dye. This result shows that the bilayer shell of the microcapsules effectively prevents leakage of the core material.
[0134] During the viscose spinning process, the solution containing microcapsules will undergo bidirectional diffusion in the coagulation bath. The components in the coagulation bath (sulfuric acid, zinc sulfate and sodium sulfate) diffuse into the viscose stream, and the sodium hydroxide in the viscose stream and the water produced by the neutralization reaction diffuse into the coagulation bath. The bidirectional diffusion process will make the microcapsules have good corrosion resistance. Figure 5 As shown in Figure 1, the stretching, pickling, and desulfurization stages of the coagulation bath in viscose spinning were simulated. Hydrochloric acid (2 g / L), sulfuric acid (2 g / L), and 10 mL of hydrochloric acid solutions were prepared for each phase. Three microcapsules (2 g each) were immersed in these solutions for 24 hours. Microcapsules immersed in the hydrochloric acid solution developed slight surface irregularities, but the microcapsule shell remained intact (attached). Figure 5 b). However, immersion in sulfuric acid solution damaged the shell of the microcapsules (attached Figure 5 c), which indicates that the acid resistance of polyurea is not good, but no leakage of the core material was observed. In sodium hydroxide solution, the microcapsule shell was very smooth and showed no signs of corrosion (attached Figure 5 d), indicating that polyurea has better tolerance to alkaline conditions than acidic conditions. In summary, the mugwort essential oil / paraffin double-layer microcapsules exhibit good stability in the acidic and alkaline environment of viscose, and the double-layer shell material of the microcapsules can prevent leakage of the core material.
[0135] 3. Thermal performance analysis of mugwort essential oil / paraffin double-layer microcapsules
[0136] In order to explore the thermal volatilization of wormwood essential oil after microencapsulation, the thermal stability of wormwood essential oil / paraffin microcapsules and their core materials was further studied. Figure 6As shown in the figure, as the temperature increases, wormwood essential oil begins to lose weight at 100°C, paraffin begins to lose weight at 150°C, and wormwood essential oil / paraffin double-layer multifunctional microcapsules begin to lose weight at 200°C. This weight loss temperature pattern indicates that the shell material of the wormwood essential oil / paraffin double-layer microcapsules effectively hinders the volatilization of the core material. The weight loss of wormwood essential oil / paraffin double-layer microcapsules at 200°C may be due to the fact that the shell layer (polyurea outer shell and polyurethane inner shell) begins to degrade at this temperature, causing paraffin and wormwood essential oil to begin to volatilize. This observation shows that the wormwood essential oil / paraffin double-layer microcapsules have the ability to withstand temperatures as high as 200°C. In order to analyze the effect of additives on the thermal stability of viscose fiber, thermogravimetric analysis was performed on viscose fiber and functional fibers with added sodium carboxymethyl cellulose and sodium alginate, respectively (see attached figure). Figure 6 a) Viscose and functional viscose fibers have the ability to withstand temperatures up to 200°C. The thermal decomposition curve of functional viscose fibers remains largely consistent with that of viscose fibers up to 200°C, indicating that the microcapsule suspension and additives do not significantly affect the thermal stability of regenerated cellulose fibers.
[0137] In order to test the core-to-wall ratio with the best phase change performance, the thermal response of these microcapsules at different core-to-shell ratios was analyzed using differential scanning calorimetry (DSC). Figure 7 Two distinct peaks were revealed in the endothermic and exothermic curves of the mugwort essential oil / paraffin bilayer microcapsules, attributed to the phase transition ability of the core material (paraffin). The phase transition peak observed between 25°C and 35°C was caused by the solid-solid phase transition of the paraffin, resulting in a less pronounced peak. However, the transition between 35°C and 50°C, originating from the solid-liquid phase transition of the paraffin, manifested as a more prominent peak. Notably, the phase transition peak was essentially absent at core-to-wall ratios of 1:1 and 1:1.9, indicating that a significant amount of paraffin was unencapsulated. This suggests that excessively large or small core-to-shell ratios can adversely affect microcapsule formation and phase transition properties. The phase transition curves of the microcapsules differed slightly at core-to-wall ratios of 1:1.4 and 1:1.6, with the former exhibiting a sharper peak. Furthermore, increasing the paraffin content resulted in subtle changes in the phase transition temperature of the microcapsules, but the overall trends remained largely consistent. The crystallization enthalpy (ΔHc) and melting enthalpy (ΔHm) of mugwort essential oil / paraffin double-layer microcapsules with a core-to-wall ratio of 1:1.4 are 32.4 J / g and 35.7 J / g, respectively, while the crystallization enthalpy (ΔHc) and melting enthalpy (ΔHm) of paraffin are 172.6 J / g and 174.6 J / g, respectively. Figure 7As shown in Figure b, DSC thermogram analysis of viscose fibers containing 1% and 3% wormwood essential oil / paraffin double-layer microcapsules shows that the phase transition peak morphology is consistent with that of the microcapsules, confirming that the microcapsules are successfully embedded in the fiber and there is no significant leakage of the core material. The phase transition temperature of the viscose fibers containing wormwood essential oil / paraffin double-layer microcapsules is mainly between 35-55°C. When the microcapsule content in the functional viscose fiber is 3%, the crystallization enthalpy (ΔHc) and melting enthalpy (ΔHm) are 24.5 J / g and 35.4 J / g, respectively. These findings verify that the wormwood essential oil / paraffin double-layer microcapsules are effectively incorporated into the functional viscose fiber, thereby improving its heat storage performance.
[0138] 4. Analysis of antibacterial properties of mugwort essential oil / paraffin double-layer microcapsules
[0139] Since wormwood essential oil has antibacterial effect, the antibacterial effect of wormwood essential oil / paraffin double-layer microcapsules was investigated. Figure 8 and attached Figure 9 The antibacterial efficacy of mugwort essential oil / paraffin bilayer microcapsules with different core-to-wall ratios against Escherichia coli was demonstrated. As the core-to-wall ratio increased, the radius of the inhibition zone gradually decreased, attributed to the decrease in the concentration of mugwort essential oil within the bilayer microcapsules. The inhibition zone radii were 6.5 mm, 2.5 mm, 1.5 mm, and 1 mm, respectively, with all zones exceeding zero, indicating long-lasting antibacterial activity and excellent antibacterial performance. Considering the particle size and phase transition ability of the microcapsules at different core-to-wall ratios, the best performance was achieved with a core-to-wall ratio of 1:1.4.
[0140] 5. Analysis of thermal and antibacterial properties of viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules
[0141] In order to analyze the effect of additives on the thermal stability of viscose fibers, thermogravimetric analysis of viscose fibers and functional fibers with sodium alginate added was carried out (see Appendix Figure 6 a), viscose fiber and functional viscose fiber have the ability to withstand temperatures up to 200 ° C. The thermal decomposition curve of functional viscose fiber is largely consistent with that of viscose fiber at up to 200 ° C, indicating that the microcapsule suspension and additives do not significantly affect the thermal stability of regenerated cellulose fiber. Figure 7 As shown in a, the mugwort essential oil / paraffin double-layer microcapsules have good heat storage capacity. Figure 7As shown in Figure b, the DSC analysis of the viscose fiber based on the double-layer microcapsules of wormwood essential oil / paraffin wax shows that the phase transition peak morphology is consistent with the phase transition peak morphology of the microcapsules, which confirms that the microcapsules are successfully embedded in the fiber and there is no large leakage of the core material. The phase transition temperature of the viscose fiber based on the double-layer microcapsules of wormwood essential oil / paraffin wax is mainly between 35°C and 55°C. When the content of microcapsules in the functional viscose fiber is 3%, the crystallization enthalpy (ΔHc) and melting enthalpy (ΔHm) are 24.5 J / g and 35.4 J / g, respectively. These findings verify that the double-layer microcapsules of wormwood essential oil / paraffin wax are effectively incorporated into the functional viscose fiber, thereby improving its heat storage performance.
[0142] In order to explore the antibacterial properties of viscose fiber based on wormwood essential oil / paraffin double-layer microcapsules, the antibacterial properties of wormwood essential oil / paraffin double-layer microcapsules were firstly analyzed (see Appendix Figure 9 ), indicating that the antibacterial properties of the mugwort essential oil / paraffin double-layer microcapsules are good. At the same time, the antibacterial properties of the functional fiber with a microcapsule addition of 3% and the functional viscose fiber with sodium alginate as the additive and a microcapsule addition of 3% were analyzed (see Appendix). Figure 9 When the core-to-wall ratio of wormwood essential oil / paraffin double-layer microcapsules was 1:1.9, the mass of the encapsulated wormwood essential oil accounted for the highest proportion of the wormwood essential oil / paraffin double-layer microcapsules, and a very clear inhibition zone appeared around the wormwood essential oil / paraffin double-layer microcapsule tablets (see Appendix). Figure 9 a), which shows that wormwood essential oil can be slowly released from the double-layer structure of the microcapsule, and the antibacterial components of wormwood essential oil effectively inhibit the growth of Escherichia coli. As the mass proportion of paraffin in the wormwood essential oil / paraffin double-layer microcapsules increases further, when the core-wall ratio of wormwood essential oil / paraffin double-layer microcapsules is 1:1.6, the antibacterial zone around the wormwood essential oil / paraffin double-layer microcapsule tablets becomes smaller (see Appendix Figure 9 b), after measurement, the radius of the inhibition zone was 3.5 mm. When the core-wall ratio of the wormwood essential oil / paraffin double-layer microcapsule was 1:1.4, the inhibition zone liquid around the wormwood essential oil / paraffin double-layer microcapsule tablet became smaller (see Appendix Figure 9 c). When the core-to-wall ratio of wormwood essential oil / paraffin double-layer microcapsules is 1:1, there is still a clearly visible inhibition zone around the wormwood essential oil / paraffin double-layer microcapsule tablets (see Appendix Figure 9 d), which shows that when the core-to-wall ratio of wormwood essential oil / paraffin double-layer microcapsules is 1:1, wormwood essential oil / paraffin double-layer microcapsules still have a good antibacterial effect on E. coli. Combined with the particle size and phase change ability of microcapsules under different core-to-wall ratios, wormwood essential oil / paraffin double-layer microcapsules have the best performance when the core-to-wall ratio is 1:1.4. When viscose fiber without added microcapsules was exposed to bacterial solution and shaken for 18 hours, the results showed dense bacterial growth (attached Figure 9e). However, when the microcapsule addition amount is 3%, the functional viscose fiber achieves an antibacterial rate of 99.99% against Escherichia coli (see Appendix Figure 9 f). When sodium alginate is added as an additive to functional fiber and the microcapsule content is 3%, it can also produce a 99.99% antibacterial rate (attached Figure 9 g). The results showed that viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules had a significant inhibitory effect on Escherichia coli. The antibacterial mechanism is shown in the attached Figure 9 As shown in Figure 3, the antimicrobial mechanism involves the release of active antimicrobial components of wormwood essential oil, such as flavonoids, eucalyptol, and terpenoids, from the functional fibers. These compounds synergistically inhibit the growth of E. coli and kill it. The thermoregulatory properties of paraffin may also affect fungal growth.
[0143] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.
Claims
1. A method for preparing viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules, characterized in that: The method comprises the following preparation steps: S1. Preparation of mugwort essential oil / paraffin double-layer microcapsules: S11. Preparation of the oil phase: 47-50 parts of wormwood essential oil, 12-15 parts of paraffin slices, 200-250 parts of the oil phase modifier were ultrasonically treated for 10-15min at a frequency of 40kHz to obtain an oil phase; S12 preparation of the aqueous phase: 3-6 parts of gum arabic, 4-7 parts of sodium dodecylbenzenesulfonate and 0.5-1 parts of the modified nanosheets were added to 100-120 parts of deionized water and stirred continuously until completely dissolved to obtain an aqueous phase; S13. The aqueous phase and the oil phase were mixed and stirred at a high shear speed of 10,000 rpm / min using a homogenizer for 5-8 minutes. After ultrasonic treatment for 25-30 minutes, 2-4 drops of dibutyltin disilicate were added at 30°C while stirring at 2,500 rpm / min for 5-8 minutes. The temperature was raised to 40°C to initially form a polyurethane inner shell, and the reaction was continued with stirring at 1,800 rpm / min for 5-8 minutes. S14. 20-25 parts of an aqueous solution of tetraethylene pentamine were added dropwise to the mixture obtained in step S13, and the temperature was raised to 50°C, the speed was adjusted to 600 rpm / min, and the polymerization reaction was carried out at 70°C for 2-3h, followed by slowly adding 5-7 parts of an aqueous solution of tetraethylene pentamine dropwise, and the reaction was continued for 40-45min to form a polyurea shell; S15. The product obtained in step S14 was washed three times with petroleum ether and deionized water and dried in an oven at 35 ° C for 0.5-1h to obtain wormwood essential oil / paraffin double-layer microcapsules; S2. Preparation of microcapsule spinning solution: 7-10 parts of the spinning solution and 2-4 parts of wormwood essential oil / paraffin double-layer microcapsule suspension were mixed and magnetically stirred for 40-50 min to achieve complete homogenization. 0.6-1 parts of sodium alginate were added to the spinning solution in 3-5 portions and magnetically stirred for 1-2 h to obtain a microcapsule spinning solution; S3 spinning: The microcapsule spinning solution obtained in step S3 is pressed into a nozzle immersed in a coagulation bath by a spinning pump, and the viscose stream ejected from the spinneret decomposes and coagulates in the coagulation bath to obtain viscose fibers based on wormwood essential oil / paraffin double-layer microcapsules; Wherein, the preparation of the oil phase modifier comprises the following steps: S31 was added 74-80 parts of petroleum ether in 165-170 parts of isophorone diisocyanate, stirred at a speed of 400-450rpm / min for 15-20min to obtain a mixture; S32 3-5 parts of a modifier enhancer, 4-8 parts of polyethylene glycol and 2-4 parts of triphenyl phosphate were added to the mixture and ultrasonically treated for 15-20 min to obtain an oil phase modifier; The preparation of the modified nanosheets in step S12 includes the following steps: S21. The montmorillonite was dispersed in deionized water to form a uniform suspension, and then a 5% concentration of zinc acetate solution was added and stirred at a speed of 400-450rpm / min for 0.5-1h to obtain a precursor mixture; S22. Sodium hydroxide solution was added to the precursor mixture to adjust the solution to alkaline, and a hydrothermal reaction was carried out at 120-150 ° C for 8-12h; S23. The product obtained by the hydrothermal reaction in step S22 is cooled, centrifuged, washed with deionized water until neutral, and dried to obtain modified nanosheets; The preparation of the modifying enhancer in step S32 comprises the following steps: S41. 8-10 parts of nano-silica were dispersed in 150-170 parts of anhydrous ethanol, ultrasonically treated at a frequency of 40 kHz for 20-30 min, and then 2-4 parts of γ-aminopropyltriethoxysilane were added and stirred at 50-60 ° C for 3-4h to obtain modified nano-silica; S42. Add 3-5 parts of dicumyl peroxide and 2-4 parts of antioxidant 1010 to the modified nano-silica and stir for 0.5-1 hour to finally obtain a modified reinforcing agent.
2. The method for preparing viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules according to claim 1, characterized in that: The coagulation bath composition was 120 g / L sulfuric acid, 15 g / L zinc sulfate and 220 g / L sodium sulfate.
3. The method for preparing viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules according to claim 1, characterized in that: The spinning parameters in step S3 are as follows: the injection pump speed is 25 mL / h, the needle inner diameter is 0.33 mm, the needle outer diameter is 0.64 mm, and the draft ratio is 2 times.
4. The method for preparing viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules according to claim 1, characterized in that: The tetraethylene pentamine aqueous solution in step S14 is a tetraethylene pentamine aqueous solution with a mass concentration of 7%.
5. The method for preparing viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules according to claim 1, characterized in that: The frequency of the ultrasonic treatment in step S32 is 40 kHz and the temperature is 30°C.
6. The method for preparing viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules according to claim 1, characterized in that: During the preparation of the modified reinforcing agent, the stirring speed is 450-500 rpm / min.
7. The method for preparing viscose fiber based on mugwort essential oil / paraffin double-layer microcapsules according to claim 1, characterized in that: In step S21, the mass ratio of montmorillonite to the zinc acetate solution with a mass concentration of 5% is 1:2-5.
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