Antioxidant fiber material and method for producing the same

Abstract

The application relates to an antioxidant fiber material and a preparation method thereof. The antioxidant fiber material comprises an organic fiber base, microcapsules and a coupling agent; the microcapsules comprise an antioxidant and a polymer covering the antioxidant, and the polymer has a structure as shown in a general formula (I); wherein the R group is a polyethylene glycol segment. The antioxidant fiber material can exhibit excellent antioxidant activity for a long time, and is beneficial to improving the wrinkle resistance, flame resistance, insulation and other properties of the fiber material.

Description

Technical Field

[0001] This invention relates to the technical field of electronic cigarettes, and in particular to an antioxidant fiber material and its preparation method. Background Technology

[0002] An electronic cigarette is an electronic product that heats e-liquid to produce an aerosol with a specific aroma. It includes components such as a cartridge containing the e-liquid, a mouthpiece, an atomizer coil, and a power source. The atomizer coil, as the core component of an electronic cigarette, can be divided into two types based on its material: ceramic coils and cotton coils. Cotton coils, with their advantages of fast wicking speed, high flavor fidelity, ease of processing, and low cost, are currently the mainstream atomizer coil material.

[0003] However, the wick is directly connected to the top airway and is very close to the mouthpiece's outlet, leaving it constantly exposed to the air, making it prone to microbial growth and adhesion. The reactive oxygen species (ROS) produced by microbial metabolism oxidize alcohols in the e-liquid into aldehydes, carboxylic acids, or esters, altering the composition and aroma of the aerosol formed by e-liquid atomization, making it difficult to control the quality of the vapor. Summary of the Invention

[0004] Therefore, it is necessary to provide an antioxidant fiber material and its preparation method, an atomizing core, and an electronic cigarette to solve the problem that the e-liquid in the cotton core is easily oxidized, which affects the quality of the vapor.

[0005] The above-mentioned objective of this invention is achieved through the following technical solution:

[0006] In a first aspect, the present invention provides an antioxidant fiber material, the raw materials of which include an organic fiber matrix, microcapsules and a coupling agent;

[0007] The microcapsules comprise an antioxidant and a polymer encapsulating the antioxidant, the polymer having a structure as shown in general formula (I):

[0008] (I);

[0009] Wherein, the R group is a polyethylene glycol segment, and the polyethylene glycol segment includes , , , and One or more of them.

[0010] In one embodiment, the polyethylene glycol segment is .

[0011] In one embodiment, the antioxidant includes one or more of vitamin antioxidants, polyphenol antioxidants, flavonoid antioxidants, and quinone antioxidants.

[0012] In one embodiment, the microcapsules have a particle size of 200 nm to 500 nm.

[0013] In one embodiment, the mass ratio of the organic fiber substrate, the microcapsule, and the coupling agent is 100:(0.5~20):(1~8).

[0014] In one embodiment, the coupling agent comprises a silane coupling agent.

[0015] In one embodiment, the organic fiber substrate is one or more of a woven fabric substrate, a knitted fabric substrate, and a nonwoven fabric substrate.

[0016] In a second aspect, the present invention provides a method for preparing an antioxidant fiber material, comprising the following steps:

[0017] A prepolymer containing triazine rings and polyethylene glycol segments, an antioxidant, an organic solvent, an emulsifier, and water are mixed to obtain a prepolymer emulsion.

[0018] The prepolymer is polymerized to form a polymer that coats the antioxidant, resulting in an emulsion containing microcapsules;

[0019] The emulsion containing microcapsules is dissolved in hot water, and a coupling agent is added to obtain a modified treatment solution;

[0020] The organic fiber substrate is modified using the aforementioned modification solution to obtain an antioxidant fiber material.

[0021] The prepolymer has a structure as shown in general formula (II):

[0022] (II);

[0023] The polymer has a structure as shown in general formula (I):

[0024] (I);

[0025] Wherein, the X group is one or more of F, Cl, Br, and I; the R group is a polyethylene glycol segment, wherein the polyethylene glycol segment includes... , , , and One or more of them.

[0026] In one embodiment, polymerizing the prepolymer to form a polymer coating the antioxidant includes the following steps:

[0027] Under heating conditions, the pH of the prepolymer emulsion is adjusted to 6-6.5 using an acid-binding agent, and the reaction is carried out for 10-120 minutes.

[0028] In one embodiment, the method for preparing the prepolymer includes the following steps:

[0029] Polyethylene glycol and cyanuric chloride are subjected to a prepolymerization reaction to obtain the prepolymer.

[0030] In one embodiment, the prepolymerization reaction of polyethylene glycol and cyanuric chloride includes the following steps:

[0031] The polyethylene glycol is dissolved in an organic solvent to obtain a polyethylene glycol solution;

[0032] The polyethylene glycol solution was added dropwise to cyanuric chloride to obtain a mixed solution;

[0033] Under ice-salt bath conditions, the pH of the mixed solution is adjusted to 6-6.5 using an acid-binding agent, and the reaction is carried out for 10-120 minutes.

[0034] In one embodiment, one or more of the following conditions are met:

[0035] 1) The organic solvent includes one or more of acetone, ethanol, acetonitrile, chloroform, and carbon tetrachloride;

[0036] 2) The emulsifier includes Tween;

[0037] 3) The acid-binding agent includes one or more of sodium hydroxide, sodium carbonate, and sodium bicarbonate;

[0038] 4) The molar ratio of the polyethylene glycol to the cyanuric chloride is 3:2;

[0039] 5) The mass fraction of the microcapsules in the modified treatment solution is 0.5%~20%.

[0040] In one embodiment, the method for modifying the organic fiber substrate using the modified treatment liquid includes one or more of padding, impregnation, spraying, and brushing.

[0041] In a third aspect, the present invention provides an atomizing core comprising the antioxidant fiber material described above.

[0042] In a fourth aspect, the present invention provides an electronic cigarette comprising the atomizing core described above.

[0043] The present invention has the following beneficial effects:

[0044] The microcapsules designed in this invention encapsulate antioxidants within a polymer containing triazine rings and polyethylene glycol segments. This protects the antioxidants from environmental influences and controls their sustained release, ensuring stable antioxidant activity over a long period. Furthermore, the polymer, serving as the protective shell, contains stable triazine rings and hydrophilic polyethylene glycol segments, making it suitable as a fabric finishing agent to effectively enhance the wrinkle resistance, flame retardancy, and insulation properties of antioxidant fiber materials. Simultaneously, the coupling agent strengthens the bond between the microcapsules and the organic fiber substrate, preventing the microcapsules from being washed away by water or tar, further guaranteeing the long-term antioxidant activity of the antioxidant fiber material. Attached Figure Description

[0045] Figure 1 This is a flowchart of a method for preparing an antioxidant fiber material in one embodiment;

[0046] Figure 2 The graph shows the antioxidant activity test results of the antioxidant fiber materials of Example 1 and Comparative Example 1;

[0047] Figure 3 The graph shows the antioxidant activity test results of the antioxidant fiber materials of Example 2 and Comparative Example 2. Detailed Implementation

[0048] To make the above-mentioned objects, features, and advantages of the present invention more apparent and understandable, specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. Many specific details are set forth in the following description to provide a thorough understanding of the present invention. However, the present invention can be practiced in many other ways different from those described herein, and those skilled in the art can make similar modifications without departing from the spirit of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0049] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this invention, "a plurality of" means at least two, such as two, three, etc., unless otherwise explicitly specified.

[0050] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0051] In a first aspect, the present invention provides an antioxidant fiber material, the raw materials of which include an organic fiber matrix, microcapsules and a coupling agent;

[0052] Microcapsules comprise an antioxidant and a polymer encapsulating the antioxidant, having a structure as shown in general formula (I):

[0053] (I);

[0054] Wherein, the R group is a polyethylene glycol segment, and the polyethylene glycol segment includes , , , and One or more of them.

[0055] The microcapsules designed in this invention encapsulate antioxidants within a polymer containing triazine rings and polyethylene glycol segments. This protects the antioxidants from environmental influences and controls their sustained release, ensuring stable antioxidant activity over a long period. Furthermore, the polymer, serving as the protective shell, contains stable triazine rings and hydrophilic polyethylene glycol segments, making it suitable as a fabric finishing agent to effectively enhance the wrinkle resistance, flame retardancy, and insulation properties of antioxidant fiber materials. Simultaneously, the coupling agent strengthens the bond between the microcapsules and the organic fiber substrate, preventing the microcapsules from being washed away by water or tar, further guaranteeing the long-term antioxidant activity of the antioxidant fiber material.

[0056] Understandably, n represents a positive integer.

[0057] In some embodiments, the polyethylene glycol segments are .

[0058] In some embodiments, the antioxidant includes one or more of vitamin antioxidants, polyphenolic antioxidants, flavonoid antioxidants, and quinone antioxidants.

[0059] Vitamin antioxidants, polyphenol antioxidants, flavonoid antioxidants, and quinone antioxidants are all natural antioxidants. They are inexpensive, readily available, safe, harmless, and have high antioxidant activity. They can inhibit the generation of reactive oxygen species or scavenge reactive oxygen free radicals.

[0060] Preferably, the antioxidants include one or more of vitamin A, vitamin C, vitamin D, vitamin E, and carotenoids.

[0061] More preferably, the antioxidant is vitamin E.

[0062] In some embodiments, the microcapsules have a particle size of 200 nm to 500 nm.

[0063] Microcapsules with a particle size in the nanometer range are called nanocapsules. They are multiphase functional materials that are easily dispersed and suspended in a medium to form colloidal solutions. Therefore, they can be uniformly distributed on organic fiber substrates. Furthermore, using nanocapsules to protect and transport antioxidants helps reduce the amount of antioxidants required, thus lowering the production cost of antioxidant fiber materials. In addition, nanocapsules themselves possess certain antibacterial activity, reducing the adhesion and growth of microorganisms, further enhancing the antioxidant activity of the organic fiber substrate.

[0064] In some embodiments, the mass ratio of the organic fiber substrate, microcapsules, and coupling agent is 100:(0.5~20):(1~8).

[0065] By using the above mass ratio, both the antioxidant activity of the antioxidant fiber material and the formation of a strong bond between the organic fiber substrate and the microcapsules can be guaranteed.

[0066] In some implementations, the coupling agent includes a silane coupling agent.

[0067] Silane coupling agents (AH) are reactive or compatible with both inorganic and organic substances. Through coupling reactions, they enable microcapsules to form a tight and strong bond with the organic fiber substrate, effectively preventing the microcapsules from being eluted and affecting the antioxidant activity of the antioxidant fiber material. Furthermore, silane coupling agents do not contain heavy metal ions or other highly toxic substances, making them safe and harmless to the environment and human body.

[0068] Preferably, the silane coupling agent includes one or more of vinyltriethoxysilane, vinyltrimethoxysilane, and vinyltri(β-methoxyethoxy)silane.

[0069] In some embodiments, the organic fiber substrate is one or more of a woven fabric substrate, a knitted fabric substrate, and a nonwoven fabric substrate.

[0070] Preferably, the organic fiber substrate is a nonwoven fabric substrate.

[0071] Non-woven fabrics have advantages such as light weight, high strength, good air permeability, strong adsorption, and easy processing and molding. They can effectively adsorb and atomize e-liquid and are highly safe to use.

[0072] In a second aspect, the present invention provides a method for preparing an antioxidant fiber material, comprising the following steps:

[0073] A prepolymer, antioxidant, organic solvent, emulsifier, and water are mixed to obtain a prepolymer emulsion;

[0074] The prepolymer is polymerized to form a polymer coated with antioxidants, resulting in an emulsion containing microcapsules;

[0075] Dissolve the emulsion containing microcapsules in hot water, add a coupling agent, and obtain a modified treatment solution;

[0076] An antioxidant fiber material is obtained by modifying an organic fiber substrate with a modification treatment solution.

[0077] The prepolymer has a structure as shown in general formula (II):

[0078] (I);

[0079] The polymer has a structure as shown in general formula (I):

[0080] (II);

[0081] Wherein, the X group is one or more of F, Cl, Br, and I, and the R group is a polyethylene glycol segment, wherein the polyethylene glycol segment includes... , , , and One or more of them.

[0082] This invention employs emulsion polymerization, where a prepolymer and antioxidant are fully emulsified and dispersed in a mixed solvent under the action of an emulsifier and mechanical stirring, with most of the prepolymer being solubilized in the emulsifier micelles to form a stable oil-in-water (W / O) emulsion polymerization system. The prepolymer, now solubilized in the micelles, then undergoes emulsion polymerization to form a polymer coating the surface of the antioxidant, thereby obtaining an emulsion containing microcapsules. Using a prepolymer containing triazine rings and polyethylene glycol segments for emulsion polymerization to prepare microcapsules offers advantages such as simplicity, efficiency, and good reproducibility.

[0083] Please see Figure 1 This is a flowchart of a method for preparing an antioxidant fiber material in one embodiment, which includes the following steps:

[0084] S1: Polyethylene glycol and cyanuric chloride undergo a prepolymerization reaction to obtain a prepolymer.

[0085] Cyanide chloride (CC), chemically named 2,4,6-trichloro-1,3,5-triazine with the molecular formula C3N3Cl3, possesses a stable triazine ring and three reactive chlorine atoms, readily undergoing affinity substitution reactions with active end groups such as hydroxyl, amino, and thiol groups. The stepwise substitution of chlorine atoms on cyanide chloride with polyethylene glycol (PEG), containing hydroxyl groups, is a single-group reaction with high controllability. Furthermore, cyanide chloride and PEG are inexpensive, readily available, and widely used, often as textile dyes or finishing agents, and pose relatively low health risks.

[0086] Preferably, the molecular weight of polyethylene glycol is 200-600.

[0087] Polyethylene glycol with a molecular weight of 200-600 is a liquid and has broad compatibility with various solvents, making it very suitable for use as a wall material for preparing microcapsules.

[0088] More preferably, the molecular weight of polyethylene glycol is 400.

[0089] In some embodiments, the prepolymerization reaction of polyethylene glycol and cyanuric chloride includes the following steps:

[0090] Polyethylene glycol is dissolved in an organic solvent to obtain a polyethylene glycol solution;

[0091] The polyethylene glycol solution was added dropwise to cyanuric chloride to obtain a mixed solution;

[0092] Under ice-salt bath conditions, the pH of the mixed solution was adjusted to 6-6.5 using an acid-binding agent, and the reaction was carried out for 10-120 minutes.

[0093] Understandably, acid-binding agents are basic substances used to absorb acids generated in the reaction system, which can promote the polymerization reaction to proceed to the right.

[0094] In some embodiments, the acid-binding agent includes one or more of sodium hydroxide, sodium carbonate, and sodium bicarbonate.

[0095] Preferably, the acid-binding agent is sodium carbonate.

[0096] When the acid-binding agent is sodium carbonate, the prepolymerization reaction of polyethylene glycol and cyanuric chloride is as follows:

[0097]

[0098] In some implementations, the molar ratio of polyethylene glycol to cyanuric chloride is 3:2.

[0099] In some embodiments, the organic solvent includes one or more of acetone, ethanol, acetonitrile, chloroform, and carbon tetrachloride.

[0100] Preferably, the organic solvent is acetone.

[0101] S2: Mix prepolymer, antioxidant, organic solvent, emulsifier and water to obtain prepolymer emulsion.

[0102] Preferably, mixing the prepolymer, antioxidant, organic solvent, emulsifier, and water includes the following steps: dissolving the prepolymer and antioxidant in the organic solvent, and then adding the emulsifier and water for emulsification and dispersion.

[0103] In some embodiments, the organic solvent includes one or more of acetone, ethanol, acetonitrile, chloroform, and carbon tetrachloride.

[0104] Preferably, the organic solvent is acetone.

[0105] Preferably, the mass ratio of prepolymer to antioxidant is 7:10.

[0106] In some implementations, the emulsifier includes Tween.

[0107] Tween, also known as polysorbate, is a class of non-toxic and non-irritating nonionic surfactants. It is widely used as an emulsifier and solubilizer for oily substances. It can be mixed with prepolymers, antioxidants, organic solvents and water to form stable emulsion polymerization systems.

[0108] Preferably, the emulsifier includes one or more of Tween 20, Tween 40, Tween 60 and Tween 80.

[0109] More preferably, the emulsifier is Tween 80.

[0110] Preferably, the mass fraction of the emulsifier in the prepolymer emulsion is 1% to 5%.

[0111] S3: Polymerize the prepolymer to form a polymer coated with antioxidants, resulting in an emulsion containing microcapsules;

[0112] In some embodiments, polymerizing the prepolymer to form a polymer coated with an antioxidant includes the following steps:

[0113] Under heating conditions, the pH of the prepolymer emulsion is adjusted to 6-6.5 using an acid-binding agent, and the reaction is carried out for 10-120 minutes.

[0114] By using emulsifiers and mechanical stirring, antioxidants and prepolymers can be dispersed into micron or nano-sized particles. Then, by controlling the temperature and pH of the emulsion polymerization reaction, microcapsules of different particle sizes can be formed.

[0115] Preferably, the heating temperature is 50℃~120℃.

[0116] Preferably, the mass fraction of microcapsules in the emulsion containing microcapsules is 10% to 20%.

[0117] In some embodiments, the acid-binding agent includes one or more of sodium hydroxide, sodium carbonate, and sodium bicarbonate.

[0118] Preferably, the acid-binding agent is sodium carbonate.

[0119] S4: Dissolve the emulsion containing microcapsules in hot water, add a coupling agent, and obtain the modified treatment solution.

[0120] Preferably, the temperature of the hot water is ≥80℃.

[0121] Preferably, the mass fraction of microcapsules in the modified treatment solution is 0.5% to 20%.

[0122] Preferably, the mass fraction of the coupling agent in the modified treatment solution is 1% to 8%.

[0123] S5: The organic fiber substrate is modified using a modification treatment solution to obtain an antioxidant fiber material.

[0124] In some embodiments, the method of modifying the organic fiber substrate using a modification treatment liquid includes one or more of padding, impregnation, spraying, and brushing.

[0125] Preferably, the method for modifying the organic fiber substrate using the modification treatment liquid is the padding method or the impregnation method.

[0126] Among them, the padding method uses organic fiber substrates with limited modification solution, which has the characteristics of fast modification speed and high cost-effectiveness; the impregnation method usually places the organic fiber substrate in an excessive amount of modification solution for modification reaction, which has the advantages of sufficient reaction and good modification effect.

[0127] Preferably, the padding method includes the following steps: fully impregnating the organic fiber substrate in a modification treatment solution at 60°C; padding the organic fiber substrate impregnated with the modification treatment solution, with a padding rate of 70%~100%; drying at 80°C~100°C; and setting and stretching at 150°C for 30s to obtain an antioxidant fiber material.

[0128] Understandably, the method of fully immersing the organic fiber substrate in a 60°C modification solution typically involves passing the substrate through a bath filled with the solution at a certain speed. Therefore, the amount of modification solution carried on the organic fiber substrate by the padding method is relatively limited. Residual filling refers to using pressure rollers to force the modification solution from the surface of the organic fiber substrate into its interior, expelling excess solution. Depending on the number of immersions and residual fillings, the padding method can be divided into different processes such as one-dip-one-paste and two-dip-two-paste. Residual filling rate, also known as liquid carry-over rate or liquid carry-over percentage, refers to the percentage of the mass of the modification solution carried on the organic fiber substrate to the mass of the organic fiber substrate itself.

[0129] Preferably, the impregnation method includes the following steps: immersing the organic fiber substrate in a modification treatment solution at 85°C for 30-40 minutes, wherein the mass ratio of the organic fiber substrate to the modification treatment solution is 1:10; removing excess water using a pressure roller and drying at 80°C-120°C to obtain an antioxidant fiber material.

[0130] Unlike padding, which involves immersing the organic fiber substrate in a high-temperature modification solution for an extended period (the immersion process itself is the modification reaction), padding uses a lower wetting temperature. Modification doesn't occur during immersion but rather during the high-temperature drying process, which is itself the reaction. Padding after immersion forces the modification into the substrate and removes excess liquid.

[0131] Preferably, in the antioxidant fiber material, the mass ratio of organic fiber substrate, microcapsule and coupling agent is 100:(0.5~20):(1~8).

[0132] In a third aspect, the present invention provides an atomizing core comprising the antioxidant fiber material described above.

[0133] In a fourth aspect, the present invention provides an electronic cigarette comprising the atomizing core described above.

[0134] The present invention will be further described in detail below with reference to specific embodiments.

[0135] Example 1

[0136] This embodiment utilizes an impregnation method to modify the organic fiber substrate.

[0137] (1) Dissolve 5.88g of polyethylene glycol (PEG-400) with a molecular weight of 400 in 10mL of acetone to obtain a PEG-400 solution; add the PEG-400 solution dropwise to cyanuric chloride (CC) with a molar ratio of PEG-400 to CC of 3:2 to obtain a mixed solution; adjust the pH of the mixed solution to 6~6.5 with a 10% Na2CO3 solution under ice-salt bath conditions and react for 120min to obtain a prepolymer solution.

[0138] (2) Dissolve the prepolymer solution and 10g of vitamin E in 20mL of acetone, add 0.3g of Tween 80, stir at 800rpm until homogeneous, add 10mL of deionized water while stirring to form a W / O type emulsion system, and continue to add 90mL of deionized water for dilution to obtain the prepolymer emulsion.

[0139] (3) Under stirring conditions, the prepolymer emulsion is heated to 80°C, and the pH of the prepolymer emulsion is adjusted to 6~6.5 using a 10% Na2CO3 solution. The reaction is carried out for 60 min to polymerize the prepolymer to form a polymer coated with vitamin E, resulting in a light yellow emulsion containing microcapsules. The mass fraction of microcapsules in the emulsion containing microcapsules is about 15%.

[0140] (4) Dissolve 16g of emulsion containing microcapsules in 184mL of hot water at 80℃, add 12g of silane coupling agent (AH), and continue stirring at 80℃ for 10min to obtain the modified treatment solution, which is denoted as Np Ve + AH solution; in the modified treatment solution, the mass fraction of microcapsules is 8% and the mass fraction of silane coupling agent is 6%.

[0141] (5) Cut cotton fiber spunlace nonwoven fabric into nonwoven fabric bases with a size of 100mm×100mm; take 20g of nonwoven fabric base and soak it in Np Ve + AH solution at 85℃ for 30min, the mass ratio of nonwoven fabric base to Np Ve + AH solution is 1:10; take out the nonwoven fabric base, remove excess water by pressing with a roller, and wash with deionized water to remove residual solution on the surface of the nonwoven fabric base; dry it under hot air at 110℃ to obtain antioxidant fiber material.

[0142] Example 2

[0143] This embodiment utilizes the padding method to modify the organic fiber substrate.

[0144] (1) Dissolve 5.88g of polyethylene glycol (PEG-400) with a molecular weight of 400 in 10mL of acetone to obtain a PEG-400 solution; add the PEG-400 solution dropwise to cyanuric chloride (CC) with a molar ratio of PEG-400 to CC of 3:2 to obtain a mixed solution; adjust the pH of the mixed solution to 6~6.5 with a 10% Na2CO3 solution under ice-salt bath conditions and react for 120min to obtain a prepolymer solution.

[0145] (2) Dissolve the prepolymer solution and 10g of vitamin E in 20mL of acetone, add 0.3g of Tween 80, stir at 800rpm until homogeneous, add 10mL of deionized water while stirring to form a W / O type emulsion system, and continue to add 90mL of deionized water for dilution to obtain the prepolymer emulsion.

[0146] (3) Under stirring conditions, the prepolymer emulsion is heated to 120°C, and the pH of the prepolymer emulsion is adjusted to 6~6.5 using a 10% Na2CO3 solution. The reaction is carried out for 30 minutes to polymerize the prepolymer to form a polymer coated with vitamin E, resulting in a light yellow emulsion containing microcapsules. The mass fraction of microcapsules in the emulsion containing microcapsules is about 15%.

[0147] (4) Dissolve 24g of emulsion containing microcapsules in 184mL of hot water at 80℃, add 12g of silane coupling agent (AH), and continue stirring at 80℃ for 10min to obtain the modified treatment solution, which is denoted as Np Ve + AH solution; in the modified treatment solution, the mass fraction of microcapsules is 12% and the mass fraction of silane coupling agent is 6%.

[0148] (5) Cut cotton fiber spunlace nonwoven fabric into nonwoven fabric base with a size of 100mm×100mm; take 20g of nonwoven fabric base and immerse it in Np Ve +AH solution at 60℃; take out the nonwoven fabric base, use a pressure roller to roll off the residue with a roll-off rate of 100%, and wash with deionized water to remove the residual solution on the surface of the nonwoven fabric base; dry it under hot air at 110℃, and set and stretch it at 150℃ for 30s to obtain antioxidant fiber material.

[0149] Comparative Example 1

[0150] This comparative example utilizes an impregnation method to modify an organic fiber substrate.

[0151] (1) Dissolve 5.88g of polyethylene glycol (PEG-400) with a molecular weight of 400 in 10mL of acetone to obtain a PEG-400 solution; add the PEG-400 solution dropwise to cyanuric chloride (CC) with a molar ratio of PEG-400 to CC of 3:2 to obtain a mixed solution; adjust the pH of the mixed solution to 6~6.5 with a 10% Na2CO3 solution under ice-salt bath conditions and react for 120min to obtain a prepolymer solution.

[0152] (2) Dissolve the prepolymer solution and 10g of vitamin E in 20mL of acetone, add 0.3g of Tween 80, stir at 800rpm until homogeneous, add 10mL of deionized water while stirring to form a W / O type emulsion system, and continue to add 90mL of deionized water for dilution to obtain the prepolymer emulsion.

[0153] (3) Under stirring conditions, the prepolymer emulsion is heated to 80°C, and the pH of the prepolymer emulsion is adjusted to 6~6.5 using a 10% Na2CO3 solution. The reaction is carried out for 60 min to polymerize the prepolymer to form a polymer coated with vitamin E, resulting in a light yellow emulsion containing microcapsules. The mass fraction of microcapsules in the emulsion containing microcapsules is about 15%.

[0154] (4) Dissolve 16g of emulsion containing microcapsules in 172mL of hot water at 80℃, and continue stirring at 80℃ for 10min to obtain a modified treatment solution with a microcapsule mass fraction of 8%, which is denoted as Np Ve solution.

[0155] (5) Cut cotton fiber spunlace nonwoven fabric into nonwoven fabric bases with a size of 100mm×100mm; take 20g of nonwoven fabric base and soak it in Np Ve solution at 60℃ for 30min, the mass ratio of nonwoven fabric base to Np Ve solution is 1:10; take out the nonwoven fabric base, remove excess water by pressing with a roller, and wash with deionized water to remove residual solution on the surface of the nonwoven fabric base; dry it under hot air at 110℃ to obtain antioxidant fiber material.

[0156] Comparative Example 2

[0157] This comparative example utilizes the padding method to modify the organic fiber substrate.

[0158] (1) Dissolve 5.88g of polyethylene glycol (PEG-400) with a molecular weight of 400 in 10mL of acetone, and add it dropwise to cyanuric chloride (CC). The molar ratio of PEG-400 to CC is 3:2 to obtain a mixed solution. Under ice-salt bath conditions, adjust the pH of the mixed solution to 6~6.5 using a 10% Na2CO3 solution and react for 120min to obtain a prepolymer solution.

[0159] (2) Dissolve the prepolymer solution obtained above and 10g of vitamin E in 20 mL of acetone, add 0.3 g of Tween 80, stir at 800 rpm until homogeneous, add 10 mL of deionized water while stirring to form a W / O type emulsion system, and continue to add 90 mL of deionized water for dilution to obtain the prepolymer emulsion.

[0160] (3) Under stirring conditions, the prepolymer emulsion is heated to 80°C, and the pH of the prepolymer emulsion is adjusted to 6~6.5 using a 10% Na2CO3 solution. The reaction is carried out for 60 min to polymerize the prepolymer to form a polymer coated with vitamin E, resulting in a light yellow emulsion containing microcapsules. The mass fraction of microcapsules in the emulsion containing microcapsules is about 15%.

[0161] (4) Dissolve 16g of emulsion containing microcapsules in 172mL of hot water at 80℃, and continue stirring at 80℃ for 10min to obtain a modified treatment solution with a microcapsule mass fraction of 8%, which is denoted as Np Ve solution.

[0162] (5) Cut cotton fiber spunlace nonwoven fabric into nonwoven fabric base with a size of 100mm×100mm; take 20g of nonwoven fabric base and immerse it in Np Ve +AH solution at 60℃; take out the nonwoven fabric base, use a pressure roller to roll off the residue with a roll-off rate of 100%, and wash with deionized water to remove the residual solution on the surface of the nonwoven fabric base; dry it under hot air at 110℃, and set and stretch it at 150℃ for 30s to obtain antioxidant fiber material.

[0163] Test case

[0164] The antioxidant activity of the above-mentioned antioxidant fiber materials was evaluated using the ABTS free radical scavenging method.

[0165] ABTS refers to 2,2'-adiazo-bis-3-ethylbenzothiazoline-6-sulfonic acid. Its nitrogen atom emits an atom to form a cationic free radical ABTS•, which appears blue-green. If a substance can decolorize a blue-green ABTS• solution, it indicates that the substance can scavenge free radicals and has antioxidant activity.

[0166] The antioxidant fiber materials from Example 1 and Comparative Example 1 were cut into small pieces, and 0.2g of each sample was weighed and added to ABTS solution. After standing for 30 minutes, the solution color was observed, and the results were as follows. Figure 2 As shown. The antioxidant fiber materials from Example 2 and Comparative Example 2 were cut into small pieces, and 0.2g of each sample was weighed and added to ABTS solution. After standing for 30 minutes, the solution color was observed, and the results are as follows. Figure 3 As shown.

[0167] Depend on Figure 2 It can be seen that after 30 minutes of treatment with the sample in Comparative Example 1, the blue-green ABTS solution slightly faded, indicating that the antioxidant fiber material prepared in Comparative Example 1 has weak antioxidant activity. After 30 minutes of treatment with the sample in Example 1, the blue-green ABTS solution completely faded and became colorless and transparent, indicating that the antioxidant fiber material prepared in Example 1 has strong antioxidant activity.

[0168] Depend on Figure 3 It can be seen that after 30 minutes of treatment with the sample in Comparative Example 2, the blue-green ABTS solution showed almost no change, indicating that the antioxidant fiber material prepared in Comparative Example 2 did not have antioxidant activity. After 30 minutes of treatment with the sample in Example 2, the blue-green ABTS solution completely faded and became colorless and transparent, indicating that the antioxidant fiber material prepared in Example 2 had strong antioxidant activity.

[0169] The comparison between Example 1 and Comparative Example 1, and between Example 2 and Comparative Example 2, shows that regardless of whether the impregnation method or the padding method is used, after modifying the nonwoven fabric substrate with NpVe + AH solution, the microcapsules containing vitamin E antioxidant can be firmly fixed on the nonwoven fabric substrate using silane coupling agent. Therefore, the microcapsules are not easily washed off in subsequent processing, allowing the antioxidant fiber material to exhibit strong antioxidant activity over a long period of time. This is beneficial for removing reactive oxygen free radicals in e-liquid and preventing uncontrollable changes in the flavor and composition of the smoke.

[0170] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0171] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention. Therefore, the protection scope of this invention patent should be determined by the appended claims, and the specification and drawings can be used to interpret the content of the claims.

Claims

1. A method for preparing an antioxidant fiber material, characterized in that, Includes the following steps: A prepolymer, antioxidant, organic solvent, emulsifier, and water are mixed to obtain a prepolymer emulsion; The prepolymer is polymerized to form a polymer that coats the antioxidant, resulting in an emulsion containing microcapsules; The emulsion containing microcapsules is dissolved in hot water, and a coupling agent is added to obtain a modified treatment solution; The organic fiber substrate is modified using the aforementioned modification solution to obtain an antioxidant fiber material. The prepolymer has a structure as shown in general formula (II): （Ⅱ）； The polymer has a structure as shown in general formula (I): （Ⅰ）； Wherein, the X group is Cl; the R group is a polyethylene glycol segment, wherein the polyethylene glycol segment includes... ; The process of polymerizing the prepolymer to form a polymer coated with the antioxidant includes the following steps: Under heating conditions, the pH of the prepolymer emulsion is adjusted to 6-6.5 using an acid-binding agent, and the reaction is carried out for 10-120 minutes. The method for preparing the prepolymer includes the following steps: Polyethylene glycol and cyanuric chloride are subjected to a prepolymerization reaction to obtain the prepolymer.

2. The method for preparing the antioxidant fiber material as described in claim 1, characterized in that, The prepolymerization reaction of polyethylene glycol and cyanuric chloride includes the following steps: The polyethylene glycol is dissolved in an organic solvent to obtain a polyethylene glycol solution; The polyethylene glycol solution was added dropwise to cyanuric chloride to obtain a mixed solution; Under ice-salt bath conditions, the pH of the mixed solution is adjusted to 6-6.5 using an acid-binding agent, and the reaction is carried out for 10-120 minutes.

3. The method for preparing the antioxidant fiber material as described in claim 1, characterized in that, One or more of the following conditions must be met: 1) The organic solvent includes one or more of acetone, ethanol, acetonitrile, chloroform, and carbon tetrachloride; 2) The emulsifier includes Tween; 3) The acid-binding agent includes one or more of sodium hydroxide, sodium carbonate, and sodium bicarbonate; 4) The molar ratio of the polyethylene glycol to the cyanuric chloride is 3:2; 5) The mass fraction of the microcapsules in the modified treatment solution is 0.5%~20%.

4. The method for preparing the antioxidant fiber material as described in claim 1, characterized in that, The method for modifying an organic fiber substrate using the modified treatment liquid includes one or more of the following: padding, impregnation, spraying, and brushing.

5. An antioxidant fiber material prepared by the preparation method according to any one of claims 1-4, characterized in that, Its raw materials include an organic fiber substrate, microcapsules, and a coupling agent, wherein the coupling agent includes a silane coupling agent, and the silane coupling agent binds the microcapsules and the organic fiber substrate through a coupling reaction; The microcapsules include an antioxidant and a polymer that encapsulates the antioxidant.

6. The antioxidant fiber material as described in claim 5, characterized in that, The antioxidants include one or more of the following: vitamin antioxidants, polyphenolic antioxidants, flavonoid antioxidants, and quinone antioxidants.

7. The antioxidant fiber material as described in claim 5, characterized in that, The microcapsules have a particle size of 200nm~500nm.

8. The antioxidant fiber material as described in claim 5, characterized in that, The mass ratio of the organic fiber substrate, the microcapsule, and the coupling agent is 100:(0.5~20):(1~8).

9. The antioxidant fiber material according to any one of claims 5-8, characterized in that, The silane coupling agent includes one or more of vinyltriethoxysilane, vinyltrimethoxysilane, and vinyltri(β-methoxyethoxy)silane.

10. The antioxidant fiber material according to any one of claims 5-8, characterized in that, The organic fiber substrate is one or more of woven fabric substrate, knitted fabric substrate, and nonwoven fabric substrate.

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