Deodorizing fiber containing rose essential oil, preparation method thereof, and fabric

Abstract

The present invention discloses a deodorizing fiber containing rose essential oil, a preparation method thereof, and a fabric, relating to the technical field of functional fabrics. The deodorizing fiber preparation method comprises the following steps: first, preparing rose essential oil microcapsules; then, subjecting cellulose fibers to an alkali soaking treatment to obtain pretreated fibers; then, loading the rose essential oil microcapsules and activated carbon onto the surfaces of the pretreated fibers to obtain nascent deodorizing fibers; and finally, heat-setting the nascent deodorizing fibers. The present invention can achieve sustained release of rose essential oil, prolong the release time of the rose essential oil, and has a good deodorizing effect.

Description

Technical Field

[0001] The invention relates to the technical field of functional fibers, in particular to a deodorizing fiber containing rose essential oil, a preparation method thereof, and a fabric. Background Art

[0002] In the field of textile materials, as people's living standards improve, the demand for functional fibers and fabrics is becoming increasingly diverse. Functional fibers containing natural ingredients have become a research hotspot, with deodorizing fibers containing rose essential oil attracting considerable attention. Rose essential oil not only has a captivating aroma but also boasts antibacterial, calming, and beauty-enhancing properties. Fabrics made by incorporating rose essential oil into fibers not only offer a pleasant sensory experience but are also expected to provide multiple beneficial effects in daily wear.

[0003] However, current deodorizing fibers and related fabrics containing rose essential oil have obvious defects. In terms of rose essential oil release, existing technologies are difficult to achieve stable and lasting release of essential oil. Some fiber preparation processes are simple, and rose essential oil is simply attached to the fiber surface or subjected to preliminary physical mixing, resulting in an unstable combination of essential oil and fiber. During daily wear, affected by factors such as friction, temperature changes and washing, rose essential oil will evaporate rapidly, making it impossible to achieve long-lasting fragrance distribution and efficacy. For example, in the early stages of wear, the fragrance may be relatively strong, but after several washes, the content of rose essential oil drops sharply, the fragrance becomes weak, and its beauty and antibacterial effects are greatly reduced, greatly reducing the use value of the fiber and fabric.

[0004] Existing deodorizing fibers containing rose essential oil also have shortcomings when it comes to deodorizing properties. While some products claim to have deodorizing effects, in actual use, they are unable to effectively remove odors from human sweat and external odors. Human sweat contains a variety of organic substances, which break down under the action of bacteria to produce various odors. Furthermore, the composition of odors in the external environment is also very complex. However, some current fibers rely solely on the weak antibacterial effect of rose essential oil to inhibit bacterial decomposition of odor sources. These fibers lack effective mechanisms for capturing and decomposing odor molecules, making them difficult to truly and effectively perform their deodorizing function and failing to meet consumers' demand for a fresh and comfortable wearing experience. Summary of the Invention

[0005] The present invention aims to provide a deodorizing fiber containing rose essential oil, a preparation method thereof, and a fabric thereof, to address the technical issues raised in the aforementioned background art, namely, the rapid release of rose essential oil and poor deodorizing effect. The present invention achieves sustained release of rose essential oil, prolongs its release duration, and exhibits excellent deodorizing effect.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] 1. A method for preparing a deodorizing fiber containing rose essential oil, comprising the following steps:

[0008] S1, preparing rose essential oil microcapsules;

[0009] S2, performing an alkali soaking treatment on the cellulose fibers to obtain pretreated fibers;

[0010] S3, loading rose essential oil microcapsules and activated carbon on the surface of the pretreated fiber to obtain the primary deodorizing fiber;

[0011] S4. Thermally fixing the nascent deodorizing fiber to obtain the product.

[0012] In the technical solution of the present invention, rose essential oil microcapsules are first prepared. By wrapping the rose essential oil, the essential oil components can be effectively protected, and its volatilization and oxidation in subsequent treatments can be reduced, thereby ensuring the long-term effectiveness of the essential oil's antibacterial deodorization and aroma sustained-release functions. Alkali soaking of cellulose fibers can increase the roughness and specific surface area of ​​the fiber surface, while introducing a large number of active groups, which not only significantly improves the fiber's adsorption capacity for rose essential oil microcapsules, but also creates more action sites for the combination of the two. Finally, through heat setting treatment, the microcapsules are more firmly combined with the fibers, and the stability of the fiber structure is enhanced. Activated carbon, as an adsorbent, can adsorb odors, thereby achieving a deodorizing effect. However, the adsorption effect of activated carbon will affect the aroma release and antibacterial and deodorizing functions of rose essential oil. Moreover, the adsorption of rose essential oil by activated carbon will occupy the adsorption space of activated carbon, resulting in a weakening of the adsorption effect of activated carbon. The present invention loads rose essential oil microcapsules and activated carbon on the fiber surface separately, rather than mixing them and loading them, thereby weakening the adsorption effect of activated carbon on rose essential oil. As Figure 1 This is a SEM image of the surface of the deodorizing fiber containing rose essential oil prepared in the present invention. From the electron microscope image, it can be observed that rose essential oil microcapsules and activated carbon are bound to the surface of the cellulose fiber.

[0013] Preferably, in step S2, the alkali solution used for the alkali soaking treatment is a sodium hydroxide solution;

[0014] The mass fraction of the sodium hydroxide solution is 2 to 5 wt %.

[0015] Preferably, in step S3, rose essential oil microcapsules and activated carbon are loaded on the surface of the pretreated fiber through an impregnation-rolling process.

[0016] Preferably, in step S1, the method for preparing rose essential oil microcapsules comprises the following steps:

[0017] S11, dissolving gelatin and gum arabic in deionized water, adding rose essential oil, and stirring for emulsification to obtain an oil-in-water emulsion;

[0018] S12, adding glutaraldehyde to the oil-in-water emulsion to carry out a cross-linking reaction to obtain a primary product of rose essential oil microcapsules;

[0019] S13, dispersing titanium dioxide in the chitosan solution to obtain a chitosan-titanium dioxide modified solution;

[0020] S14, coating the surface of the microcapsules with a chitosan-titanium dioxide surface coating modification liquid coating to obtain rose essential oil microcapsules.

[0021] In the technical solution of the present invention, gelatin is first dissolved and then emulsified with rose essential oil. Gelatin, as a natural polymer wall material raw material, has good film-forming properties and biocompatibility. After dissolution, it can be evenly dispersed in water. Stirring and emulsification disperses the rose essential oil into tiny oil droplets, forming a stable oil-in-water emulsion. Glutaraldehyde is added to initiate a cross-linking reaction. The aldehyde groups at both ends of the glutaraldehyde molecules react with the amino groups in the gelatin molecules to form covalent bonds, interconnecting the wall material polymers and building a three-dimensional network structure. The wall material is solidified and tightly encapsulates the rose essential oil, preventing the essential oil from volatilizing and oxidizing, ensuring its antibacterial, deodorizing, and aromatic properties. Titanium dioxide is then dispersed in a chitosan solution. Chitosan molecules are rich in amino and hydroxyl groups and have excellent adsorption and film-forming properties. Titanium dioxide also possesses photocatalytic activity. The two combine to form a modified solution, which is then coated on the surface of the microcapsules. On the one hand, chitosan forms a dense protective film on the surface of the microcapsules, enhancing their mechanical strength and stability. Its amino groups also adsorb odor molecules. On the other hand, titanium dioxide, under light, generates photogenerated electron-hole pairs, which further generate superoxide and hydroxyl radicals. These oxidize and decompose adsorbed odor molecules into harmless substances. This, in synergy with the chitosan's adsorption, significantly enhances the microcapsules' odor removal ability. Furthermore, the activated carbon bound to the fiber surface adsorbs odors to the fiber surface, thereby enhancing the deodorizing effect of the chitosan and rose essential oil.

[0022] Preferably, in step S11, the mass ratio of gelatin to gum arabic is 10:1-3.

[0023] Preferably, in step S13, the mass ratio of chitosan to titanium dioxide is 5:0.5-1.0.

[0024] Preferably, in step S14, the chitosan-titanium dioxide surface coating modification liquid coating is coated on the surface of the microcapsules by an immersion method.

[0025] Preferably, in step S3, the activated carbon is modified, comprising the following steps:

[0026] oxidizing the activated carbon using nitric acid to obtain oxidized activated carbon;

[0027] 3-aminopropyltriethoxysilane was grafted onto the surface of oxidized activated carbon to obtain coupling agent-modified activated carbon;

[0028] The product is obtained by taking acrylic acid and coupling agent modified activated carbon as raw materials and carrying out graft polymerization reaction under the action of potassium persulfate initiator.

[0029] In the technical solution of the present invention, as mentioned above, the effect of adsorption and deodorization is achieved by combining activated carbon on the fiber surface. The present invention team has found that although activated carbon and rose essential oil microcapsules are loaded on the fiber surface respectively, the adsorption of activated carbon to rose essential oil is weakened, but it is found through research that activated carbon still has obvious adsorption to rose essential oil. In order to further solve this problem, the present invention modifies activated carbon, first uses acid to activate activated carbon, and then grafts 3-aminopropyltriethoxysilane to load amino groups on the activated carbon surface, and utilizes amino groups to react with acrylic acid carboxyl groups and the polymerization reaction of acrylic acid, so that long chains of polyacrylic acid are grafted to the activated carbon surface, so that the activated carbon surface has good hydrophilic properties. The main components of rose essential oil are fat-soluble compounds such as terpenes and esters, and the molecular polarity is relatively weak. The polarity of the activated carbon surface after hydrophilic modification is relatively strong, so that polar repulsion is generated between the activated carbon surface and the non-polar rose essential oil, reducing the adsorption capacity of activated carbon to rose essential oil. On the other hand, the steric hindrance of the polypropylene polymer chain segment can physically block the adsorption of rose essential oil, thereby further reducing the adsorption effect of activated carbon on rose essential oil.

[0030] A deodorizing fiber containing rose essential oil is prepared by the above method.

[0031] A deodorizing fabric containing rose essential oil is prepared from deodorizing fibers containing rose essential oil.

[0032] Compared with the prior art, the present invention has the following beneficial effects:

[0033] 1. Rose essential oil microcapsules reduce volatilization and achieve slow release; chitosan-titanium dioxide coating synergizes with essential oil to exert antibacterial and deodorizing functions with long-lasting effects.

[0034] 2. Alkali treatment of the fiber increases the adsorption sites, and heat setting makes the microcapsules more firmly bonded to the fiber, thereby improving the stability of the fiber structure and the durability of its function.

[0035] 3. The modified activated carbon has good hydrophilicity, which reduces the adsorption of rose essential oil through polar repulsion and steric hindrance. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] Figure 1 This is an SEM image of the surface of the deodorizing fiber containing rose essential oil prepared in the present invention. DETAILED DESCRIPTION

[0037] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the implementation regulations described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0038] Example 1

[0039] A method for preparing deodorizing fiber containing rose essential oil comprises the following steps:

[0040] Step 1: Preparation of rose essential oil microcapsules:

[0041] Step 1-1: Weigh 10g of gelatin and 2.5g of gum arabic into a beaker. Add 300mL of deionized water. Place the beaker in a 50°C water bath and stir at 200 rpm using a magnetic stirrer until the gelatin and gum arabic are completely dissolved. Subsequently, slowly add 6mL of rose essential oil to the solution. Switch to a high-speed disperser and emulsify at 1200 rpm for 25 minutes to form a uniform and stable oil-in-water emulsion.

[0042] Step 1-2: Maintain the temperature of the oil-in-water emulsion at 10°C. Slowly add 5 mL of a 25% glutaraldehyde solution using a pipette. Stir continuously at 100 rpm for 1.5 hours to crosslink the gelatin and form the initial rose oil microcapsules. After the reaction, transfer the emulsion to a centrifuge tube and centrifuge at 4000 rpm for 12 minutes. Discard the supernatant and wash the precipitate three times with deionized water to remove unreacted glutaraldehyde and other impurities.

[0043] Step 1-3: Weigh 5.0 g of chitosan and add it to 300 mL of 2% acetic acid solution. Stir and dissolve at 40°C. Weigh 0.9 g of nano-titanium dioxide and add it to the chitosan solution. Ultrasonicate and disperse the titanium dioxide in the chitosan solution for 30 minutes using an ultrasonic cleaner to obtain a chitosan-titanium dioxide modified solution.

[0044] Steps 1-4: Add the primary rose essential oil microcapsules to the chitosan-titanium dioxide modification solution and incubate at 35°C with stirring at 80 rpm for 30 minutes to allow the modification solution to form a coating on the microcapsules. Remove excess modification solution by centrifugation (4000 rpm for 12 minutes) and washing with deionized water. Dry the coated microcapsules in a 50°C electric forced air drying oven for 2 hours to obtain rose essential oil microcapsules.

[0045] Step 2: Place 10g of cellulose fiber in a 3% sodium hydroxide solution and soak in a 30°C constant temperature water bath for 30 minutes. After soaking, remove the fiber and rinse it repeatedly with deionized water until neutral. Then, dry the fiber in a 60°C electric blast drying oven to obtain pretreated fiber.

[0046] Step 3: Weigh 5g of rose essential oil microcapsules and add them to 500mL of deionized water. Stir thoroughly to prepare a microcapsule suspension. Immerse the pretreated fiber in the microcapsule suspension and allow it to soak for 45 minutes at 40°C with stirring at 60 rpm to allow the microcapsules to fully adhere to the fiber surface. After impregnation, use a padder to squeeze the fiber, controlling the squeeze rate to 70%, and remove excess suspension.

[0047] Weigh 5g of modified activated carbon and add it to 500mL of deionized water, stirring evenly to prepare an activated carbon suspension. The fiber loaded with rose essential oil microcapsules was then immersed in the activated carbon suspension again. Stir at 40°C and 60 rpm for 30 minutes. The fiber was then padded with a padder, with a padded rate of 70%. This yielded the nascent deodorizing fiber.

[0048] Step 4: Spread the nascent deodorizing fiber on a surface dish, place it in an electric blast drying oven at 70°C, and heat-set it for 30 minutes to make the microcapsules and activated carbon more firmly bonded to the fiber, thereby obtaining a finished deodorizing fiber containing rose essential oil.

[0049] Preparation of modified activated carbon:

[0050] Weigh 10g of activated carbon into a beaker, add 400mL of 30% nitric acid, and place the beaker in a 60°C constant-temperature water bath. Stir at 150 rpm for 1 hour to oxidize the activated carbon. After the reaction, pour the solution into a Buchner funnel and filter it with suction. Wash the activated carbon with deionized water until the filtrate is neutral. Dry the oxidized activated carbon in an 80°C electric forced-air drying oven to obtain oxidized activated carbon.

[0051] 10 mL of 3-aminopropyltriethoxysilane (APTES) was added to 250 mL of ethanol (ethanol:water volume ratio 9:1) and stirred thoroughly. 5 g of oxidized activated carbon was then added to the solution and stirred at 40°C for 1.5 hours to allow APTES to graft onto the surface of the oxidized activated carbon. After the reaction, the activated carbon was separated by centrifugation (3000 rpm, 10 minutes) and washed twice with ethanol to remove unreacted APTES. The grafted activated carbon was then dried at 60°C to obtain coupling agent-modified activated carbon.

[0052] Weigh 3g of coupling agent-modified activated carbon, 5g of acrylic acid, and 0.2g of potassium persulfate into 300mL of deionized water and stir thoroughly. Then, add 0.2g of EDC (a condensing agent), adjust the pH to 4.5, and initiate graft polymerization in a 60°C water bath at 200 rpm for 2 hours. After the reaction, cool the solution to room temperature and separate the modified activated carbon by centrifugation (4000 rpm for 15 minutes). Wash three times with deionized water to remove unreacted acrylic acid and potassium persulfate. Dry the final modified activated carbon in a 50°C electric forced air drying oven.

[0053] Example 2

[0054] A method for preparing deodorizing fiber containing rose essential oil comprises the following steps:

[0055] Step 1: Preparation of rose essential oil microcapsules:

[0056] Step 1-1: Weigh 10g of gelatin and 1.5g of gum arabic into a beaker. Add 300mL of deionized water. Place the beaker in a 50°C water bath and stir with a magnetic stirrer at 200 rpm until the gelatin and gum arabic are completely dissolved. Next, slowly add 4mL of rose essential oil to the solution. Switch to a high-speed disperser and emulsify at 1200 rpm for 25 minutes to form a uniform and stable oil-in-water emulsion.

[0057] Step 1-2: Maintain the temperature of the oil-in-water emulsion at 10°C. Slowly add 5 mL of a 25% glutaraldehyde solution using a pipette. Stir continuously at 100 rpm for 1.5 hours to crosslink the gelatin and form the initial rose oil microcapsules. After the reaction, transfer the emulsion to a centrifuge tube and centrifuge at 4000 rpm for 12 minutes. Discard the supernatant and wash the precipitate three times with deionized water to remove unreacted glutaraldehyde and other impurities.

[0058] Step 1-3: Weigh 5.0 g of chitosan and add it to 300 mL of 2% acetic acid solution. Stir and dissolve at 40°C. Weigh 0.6 g of nano-titanium dioxide and add it to the chitosan solution. Ultrasonicate and disperse the titanium dioxide in the chitosan solution for 30 minutes using an ultrasonic cleaner to obtain a chitosan-titanium dioxide modified solution.

[0059] Steps 1-4: Add the primary rose essential oil microcapsules to the chitosan-titanium dioxide modification solution and incubate at 35°C with stirring at 80 rpm for 30 minutes to allow the modification solution to form a coating on the microcapsules. Remove excess modification solution by centrifugation (4000 rpm for 12 minutes) and washing with deionized water. Dry the coated microcapsules in a 50°C electric forced air drying oven for 2 hours to obtain rose essential oil microcapsules.

[0060] Step 2: Place 10g of cellulose fiber in a 3% sodium hydroxide solution and soak in a 30°C constant temperature water bath for 30 minutes. After soaking, remove the fiber and rinse it repeatedly with deionized water until neutral. Then, dry the fiber in a 60°C electric blast drying oven to obtain pretreated fiber.

[0061] Step 3: Weigh 5g of rose essential oil microcapsules and add them to 500mL of deionized water. Stir thoroughly to prepare a microcapsule suspension. Immerse the pretreated fiber in the microcapsule suspension and allow it to soak for 45 minutes at 40°C with stirring at 60 rpm to allow the microcapsules to fully adhere to the fiber surface. After impregnation, use a padder to squeeze the fiber, controlling the squeeze rate to 70%, and remove excess suspension.

[0062] Weigh 3 g of modified activated carbon (prepared as in Example 1) and add it to 500 mL of deionized water. Stir thoroughly to prepare an activated carbon suspension. Fibers loaded with rose essential oil microcapsules were again immersed in the activated carbon suspension at 40°C, stirring at 60 rpm for 30 min. The fibers were then padded using a padder, with a padded rate of 70%. This yielded virgin deodorizing fibers.

[0063] Step 4: Spread the nascent deodorizing fiber on a surface dish, place it in an electric blast drying oven at 70°C, and heat-set it for 30 minutes to make the microcapsules and activated carbon more firmly bonded to the fiber, thereby obtaining a finished deodorizing fiber containing rose essential oil.

[0064] Example 3

[0065] A method for preparing deodorizing fiber containing rose essential oil comprises the following steps:

[0066] Step 1: Preparation of rose essential oil microcapsules:

[0067] Step 1-1: Weigh 10g of gelatin and 2g of gum arabic into a beaker. Add 300mL of deionized water. Place the beaker in a 50°C water bath and stir with a magnetic stirrer at 200 rpm until the gelatin and gum arabic are completely dissolved. Next, slowly add 5mL of rose essential oil to the solution. Switch to a high-speed disperser and emulsify at 1200 rpm for 25 minutes to form a uniform and stable oil-in-water emulsion.

[0068] Step 1-2: Maintain the temperature of the oil-in-water emulsion at 10°C. Slowly add 5 mL of a 25% glutaraldehyde solution using a pipette. Stir continuously at 100 rpm for 1.5 hours to crosslink the gelatin and form the initial rose oil microcapsules. After the reaction, transfer the emulsion to a centrifuge tube and centrifuge at 4000 rpm for 12 minutes. Discard the supernatant and wash the precipitate three times with deionized water to remove unreacted glutaraldehyde and other impurities.

[0069] Step 1-3: Weigh 5.0 g of chitosan and add it to 300 mL of 2% acetic acid solution. Stir and dissolve at 40°C. Weigh 0.8 g of nano-titanium dioxide and add it to the chitosan solution. Ultrasonicate and disperse the titanium dioxide in the chitosan solution for 30 minutes using an ultrasonic cleaner to obtain a chitosan-titanium dioxide modified solution.

[0070] Steps 1-4: Add the primary rose essential oil microcapsules to the chitosan-titanium dioxide modification solution and incubate at 35°C with stirring at 80 rpm for 30 minutes to allow the modification solution to form a coating on the microcapsules. Remove excess modification solution by centrifugation (4000 rpm for 12 minutes) and washing with deionized water. Dry the coated microcapsules in a 50°C electric forced air drying oven for 2 hours to obtain rose essential oil microcapsules.

[0071] Step 2: Place 10g of cellulose fiber in a 3% sodium hydroxide solution and soak in a 30°C constant temperature water bath for 30 minutes. After soaking, remove the fiber and rinse it repeatedly with deionized water until neutral. Then, dry the fiber in a 60°C electric blast drying oven to obtain pretreated fiber.

[0072] Step 3: Weigh 5g of rose essential oil microcapsules and add them to 500mL of deionized water. Stir thoroughly to prepare a microcapsule suspension. Immerse the pretreated fiber in the microcapsule suspension and allow it to soak for 45 minutes at 40°C with stirring at 60 rpm to allow the microcapsules to fully adhere to the fiber surface. After impregnation, use a padder to squeeze the fiber, controlling the squeeze rate to 70%, and remove excess suspension.

[0073] Weigh 4 g of modified activated carbon (prepared as in Example 1) and add it to 500 mL of deionized water. Stir thoroughly to prepare an activated carbon suspension. Fibers loaded with rose essential oil microcapsules were again immersed in the activated carbon suspension at 40°C, stirring at 60 rpm for 30 min. The fibers were then paddled using a padder, with a paddle rate of 70%. This yielded virgin deodorizing fibers.

[0074] Step 4: Spread the nascent deodorizing fiber on a surface dish, place it in an electric blast drying oven at 70°C, and heat-set it for 30 minutes to make the microcapsules and activated carbon more firmly bonded to the fiber, thereby obtaining a finished deodorizing fiber containing rose essential oil.

[0075] Example 4

[0076] A method for preparing deodorizing fiber containing rose essential oil comprises the following steps:

[0077] Step 1: Preparation of rose essential oil microcapsules:

[0078] Step 1-1: Weigh 10g of gelatin and 3g of gum arabic into a beaker. Add 300mL of deionized water. Place the beaker in a 50°C water bath and stir with a magnetic stirrer at 200 rpm until the gelatin and gum arabic are completely dissolved. Next, slowly add 7mL of rose essential oil to the solution. Switch to a high-speed disperser and emulsify at 1200 rpm for 25 minutes to form a uniform and stable oil-in-water emulsion.

[0079] Step 1-2: Maintain the temperature of the oil-in-water emulsion at 10°C. Slowly add 5 mL of a 25% glutaraldehyde solution using a pipette. Stir continuously at 100 rpm for 1.5 hours to crosslink the gelatin and form the initial rose oil microcapsules. After the reaction, transfer the emulsion to a centrifuge tube and centrifuge at 4000 rpm for 12 minutes. Discard the supernatant and wash the precipitate three times with deionized water to remove unreacted glutaraldehyde and other impurities.

[0080] Step 1-3: Weigh 5.0 g of chitosan and add it to 300 mL of 2% acetic acid solution. Stir and dissolve at 40°C. Weigh 1.0 g of nano-titanium dioxide and add it to the chitosan solution. Ultrasonicate and disperse the titanium dioxide in the chitosan solution for 30 minutes using an ultrasonic cleaner to obtain a chitosan-titanium dioxide modified solution.

[0081] Steps 1-4: Add the primary rose essential oil microcapsules to the chitosan-titanium dioxide modification solution and incubate at 35°C with stirring at 80 rpm for 30 minutes to allow the modification solution to form a coating on the microcapsules. Remove excess modification solution by centrifugation (4000 rpm for 12 minutes) and washing with deionized water. Dry the coated microcapsules in a 50°C electric forced air drying oven for 2 hours to obtain rose essential oil microcapsules.

[0082] Step 2: Place 10g of cellulose fiber in a 5% sodium hydroxide solution and soak in a 30°C constant temperature water bath for 30 minutes. After soaking, remove the fiber and rinse it repeatedly with deionized water until neutral. Then, dry the fiber in a 60°C electric blast drying oven to obtain pretreated fiber.

[0083] Step 3: Weigh 5g of rose essential oil microcapsules and add them to 500mL of deionized water. Stir thoroughly to prepare a microcapsule suspension. Immerse the pretreated fiber in the microcapsule suspension and allow it to soak for 45 minutes at 40°C with stirring at 60 rpm to allow the microcapsules to fully adhere to the fiber surface. After impregnation, use a padder to squeeze the fiber, controlling the squeeze rate to 70%, and remove excess suspension.

[0084] Weigh 6 g of modified activated carbon (prepared as in Example 1) and add it to 500 mL of deionized water. Stir thoroughly to prepare an activated carbon suspension. Fibers loaded with rose essential oil microcapsules were again immersed in the activated carbon suspension at 40°C, stirring at 60 rpm for 30 min. The fibers were then paddled using a padder, with a paddle rate of 70%. This yielded virgin deodorizing fibers.

[0085] Step 4: Spread the nascent deodorizing fiber on a surface dish, place it in an electric blast drying oven at 70°C, and heat-set it for 30 minutes to make the microcapsules and activated carbon more firmly bonded to the fiber, thereby obtaining a finished deodorizing fiber containing rose essential oil.

[0086] Example 5

[0087] A method for preparing deodorizing fiber containing rose essential oil comprises the following steps:

[0088] Step 1: Preparation of rose essential oil microcapsules:

[0089] Step 1-1: Weigh 10g of gelatin and 1g of gum arabic into a beaker. Add 300mL of deionized water. Place the beaker in a 50°C water bath and stir with a magnetic stirrer at 200 rpm until the gelatin and gum arabic are completely dissolved. Next, slowly add 3mL of rose essential oil to the solution. Switch to a high-speed disperser and emulsify at 1200 rpm for 25 minutes to form a uniform and stable oil-in-water emulsion.

[0090] Step 1-2: Maintain the temperature of the oil-in-water emulsion at 10°C. Slowly add 5 mL of a 25% glutaraldehyde solution using a pipette. Stir continuously at 100 rpm for 1.5 hours to crosslink the gelatin and form the initial rose oil microcapsules. After the reaction, transfer the emulsion to a centrifuge tube and centrifuge at 4000 rpm for 12 minutes. Discard the supernatant and wash the precipitate three times with deionized water to remove unreacted glutaraldehyde and other impurities.

[0091] Step 1-3: Weigh 5.0 g of chitosan and add it to 300 mL of 2% acetic acid solution. Stir and dissolve at 40°C. Weigh 0.5 g of nano-titanium dioxide and add it to the chitosan solution. Ultrasonicate and disperse the titanium dioxide in the chitosan solution for 30 minutes using an ultrasonic cleaner to obtain a chitosan-titanium dioxide modified solution.

[0092] Steps 1-4: Add the primary rose essential oil microcapsules to the chitosan-titanium dioxide modification solution and incubate at 35°C with stirring at 80 rpm for 30 minutes to allow the modification solution to form a coating on the microcapsules. Remove excess modification solution by centrifugation (4000 rpm for 12 minutes) and washing with deionized water. Dry the coated microcapsules in a 50°C electric forced air drying oven for 2 hours to obtain rose essential oil microcapsules.

[0093] Step 2: Place 10g of cellulose fiber in a 2% sodium hydroxide solution and soak in a 30°C constant temperature water bath for 30 minutes. After soaking, remove the fiber and rinse it repeatedly with deionized water until neutral. Then, dry the fiber in a 60°C electric blast drying oven to obtain pretreated fiber.

[0094] Step 3: Weigh 5g of rose essential oil microcapsules and add them to 500mL of deionized water. Stir thoroughly to prepare a microcapsule suspension. Immerse the pretreated fiber in the microcapsule suspension and allow it to soak for 45 minutes at 40°C with stirring at 60 rpm to allow the microcapsules to fully adhere to the fiber surface. After impregnation, use a padder to squeeze the fiber, controlling the squeeze rate to 70%, and remove excess suspension.

[0095] Weigh 2 g of modified activated carbon (prepared as in Example 1) and add it to 500 mL of deionized water. Stir thoroughly to prepare an activated carbon suspension. Fibers loaded with rose essential oil microcapsules were again immersed in the activated carbon suspension at 40°C, stirring at 60 rpm for 30 minutes. The fibers were then paddled using a padder, with a paddle rate of 70%. This yielded virgin deodorizing fibers.

[0096] Step 4: Spread the nascent deodorizing fiber on a surface dish, place it in an electric blast drying oven at 70°C, and heat-set it for 30 minutes to make the microcapsules and activated carbon more firmly bonded to the fiber, thereby obtaining a finished deodorizing fiber containing rose essential oil.

[0097] Comparative Example 1

[0098] The difference between Comparative Example 1 and Example 1 is that during the preparation of the deodorizing fiber, the rose essential oil microcapsules were replaced with rose essential oil of equal mass.

[0099] Comparative Example 2

[0100] The difference between Comparative Example 2 and Example 1 is that the step of bonding the modified activated carbon to the fiber is omitted during the preparation of the deodorizing fiber, that is, the modified activated carbon is not bonded to the fiber.

[0101] Comparative Example 3

[0102] The difference between Comparative Example 3 and Example 1 is that the modified activated carbon is replaced with ordinary activated carbon of equal mass during the preparation of the deodorizing fiber.

[0103] Comparative Example 4

[0104] The difference between Comparative Example 4 and Example 1 is that the rose essential oil microcapsule primary product is not coated with the chitosan-titanium dioxide modified liquid layer during the preparation of the deodorizing fiber.

[0105] Performance testing:

[0106] 1. Deodorization performance test: Referring to GB / T 31105-2014 "Determination of Textile Odors", the ammonia removal rate of the fiber was determined by gas chromatography. Specifically, 5g of the deodorizing fiber sample was placed in a 250mL sealed glass container, and ammonia with a concentration of 50ppm was injected. The container was left to stand for 30 minutes at 25℃ and 65% humidity. The ammonia concentration in the container was detected by gas chromatograph. The deodorization rate was calculated according to the formula: Deodorization rate (%) = (C0-C t ) / C0×100%, where C0 is the initial ammonia concentration, C t The test results are shown in Table 1.

[0107] 2. Rose Essential Oil Sustained-Release Performance Test: Gas chromatography-mass spectrometry was used to measure the amount of essential oil released. 10g of deodorizing fiber was placed in a 1L sealed container. At 25°C and 65% humidity, 100mL of the gas from the container was sampled at intervals of 7 and 30 days. The concentration of phenylethanol, a characteristic component of rose essential oil, was measured using headspace sampling. The cumulative release rate was calculated to characterize the essential oil's sustained-release properties. The test results are shown in Table 1.

[0108] 3. Washability Test: Referring to GB / T 8629-2017, "Textile Testing - Household Washing and Drying Procedure," samples were washed 50 times with a standard detergent at 40°C for 30 minutes each wash. Deodorization was then repeated after drying to assess the washability stability of the fiber's functional components. See Table 1 for test results.

[0109] Table 1:

[0110]

[0111] 4. Test of adsorption rate of rose essential oil on activated carbon: 1g modified activated carbon and 1g ordinary activated carbon were added into 10mL rose essential oil-ethanol solution (essential oil concentration 1mg / mL) respectively, and shaken at 25℃ for 24h. The remaining essential oil concentration in the solution was determined by GC-MS. The adsorption rate (%) was calculated as (C0-C t ) / C0×100% to calculate the adsorption rate and compare the adsorption capacity of essential oils by activated carbon before and after modification. The calculated adsorption rate of rose essential oil by modified activated carbon was 5.6%, while that of standard activated carbon was 37.3%. This demonstrates that modified activated carbon significantly reduces its adsorption of rose essential oil.

[0112] Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments, or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A method for preparing deodorant fiber containing rose essential oil, characterized in that: The following steps are involved: S1. Preparation of rose essential oil microcapsules: S11, dissolving gelatin and gum arabic in deionized water, adding rose essential oil, and stirring for emulsification to obtain an oil-in-water emulsion; S12, adding glutaraldehyde to the oil-in-water emulsion to carry out a cross-linking reaction to obtain a primary product of rose essential oil microcapsules; S13, dispersing titanium dioxide in the chitosan solution to obtain a chitosan-titanium dioxide modified solution; S14, coating the surface of the microcapsules with a chitosan-titanium dioxide surface coating modification liquid coating to obtain rose essential oil microcapsules; S2, performing an alkali soaking treatment on the cellulose fibers to obtain pretreated fibers; S3, loading rose essential oil microcapsules and modified activated carbon on the surface of the pretreated fiber to obtain the primary deodorizing fiber; The preparation method of the modified activated carbon comprises the following steps: oxidizing the activated carbon using nitric acid to obtain oxidized activated carbon; 3-aminopropyltriethoxysilane was grafted onto the surface of oxidized activated carbon to obtain coupling agent-modified activated carbon; Acrylic acid and coupling agent modified activated carbon are used as raw materials, and a graft polymerization reaction is carried out under the action of potassium persulfate initiator to obtain the product; S4. Thermally fixing the nascent deodorizing fiber to obtain the product.

2. The method for preparing a deodorant fiber containing rose essential oil according to claim 1, characterized in that: In step S2, the alkali solution used in the alkali soaking treatment is a sodium hydroxide solution; The mass fraction of the sodium hydroxide solution is 2-5 wt%.

3. The method for preparing a deodorant fiber containing rose essential oil according to claim 1, characterized in that: In step S3, rose essential oil microcapsules and activated carbon are loaded on the surface of the pretreated fiber through an impregnation-rolling process.

4. The method for preparing a deodorant fiber containing rose essential oil according to claim 1, characterized in that: In step S11, the mass ratio of gelatin to gum arabic is 10:1-3.

5. The method for preparing a deodorant fiber containing rose essential oil according to claim 1, characterized in that: In step S13, the mass ratio of chitosan to titanium dioxide is 5:0.5-1.

0.

6. The method for preparing a deodorant fiber containing rose essential oil according to claim 1, characterized in that: In the step S14, the chitosan-titanium dioxide surface coating modification liquid coating is coated on the surface of the microcapsule by an immersion method.

7. A deodorizing fiber containing rose essential oil, characterized in that: The method is prepared by any one of claims 1 to 6.

8. A deodorizing fabric containing rose essential oil, characterized in that: The deodorizing fiber is prepared from the deodorizing fiber containing rose essential oil as claimed in claim 7.

Images