Environment-friendly mugwort cloud wool and preparation method thereof

Abstract

The application discloses an environment-friendly mugwort cloud wool and a preparation method thereof, and relates to the technical field of cloud wool. In the application, titanium dioxide powder is added into an ethyl sorbate solution, a polysorbate film is coated through an in-situ polymerization method, and then the ethyl sorbate is hydrolyzed to release carboxyl groups to obtain modified titanium dioxide powder, which is mixed with waste polyester and mugwort powder to form a spinning solution; secondly, N,N,N',N'-tetramethyl-p-phenylenediamine and 6-iodo-1-hexene are reacted to prepare a quaternary ammonium salt, a double bond is introduced into the compound, and then ultraviolet click reaction is carried out with 11-mercapto-undecyl trimethoxysilane to prepare a mercapto-modified quaternary ammonium salt; the mercapto-modified quaternary ammonium salt is used as an antistatic agent and is added into the spinning solution, and the environment-friendly mugwort cloud wool is prepared through wet spinning; the mercapto modification is helpful to the uniform dispersion of the quaternary ammonium salt in the spinning solution, and reduces the uneven fiber structure or breakage caused by uneven dispersion of the additive. The environment-friendly mugwort cloud wool prepared by the application has the effects of antibiosis and antistatic.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of cloud wool, in particular to an environment-friendly wormwood cloud wool and a preparation method thereof. BACKGROUND

[0002] In the development process of modern home textiles and textile materials, cloud wool has become the preferred material for the production of many home supplies and clothing due to its excellent softness and excellent warmth retention. Whether it is a quilt or a blanket that provides warmth and protection in cold winter days, or comfortable and skin-friendly clothing in daily wear, cloud wool plays an important role.

[0003] However, with the progress of science and technology and the diversification of living scenes, people's requirements for cloud wool materials are no longer limited to traditional advantages. In daily use, whether as bedding or home soft furnishings, due to the characteristics of its material, cloud wool is prone to adsorb human body dander, sweat and other secretions, which provides a breeding ground for bacteria and microorganisms. In dry climate environments, static problems also gradually emerge.

[0004] Therefore, the present application provides an environment-friendly wormwood cloud wool with antibacterial and antistatic properties. SUMMARY

[0005] The present application aims to provide an environment-friendly wormwood cloud wool and a preparation method thereof to solve the problems in the prior art.

[0006] In order to solve the above technical problems, the present application provides the following technical scheme: a preparation method of an environment-friendly wormwood cloud wool, comprising the following preparation steps:

[0007] (1) Mix dimethylphenylsilane, tris(pentafluorophenyl)borane, 4% of the mass of sorbic acid ethyl ester and toluene to obtain a mixture, add titanium dioxide powder, stir, add catalyst, the remaining sorbic acid ethyl ester, then add benzoic acid, filter and wash to obtain pretreated titanium dioxide powder, and hydrolyze the pretreated titanium dioxide powder with lipase to obtain modified titanium dioxide powder;

[0008] (2) Under nitrogen protection, mix N,N,N',N'-tetramethyl-p-phenylenediamine and 6-iodo-1-hexene at a molar ratio of 1.1-1.2:1 to obtain a mixture B, dissolve the mixture B in anhydrous toluene, heat to 60-80℃, stir for 4-6h, cool to room temperature, wash and dry to obtain a quaternary ammonium salt, mix 11-mercapto-undecyltrimethoxysilane and the quaternary ammonium salt at a molar ratio of 1.0-1.3:1 to obtain a mixture C, dissolve the mixture C in anhydrous toluene, add 300ppm of benzoyl peroxide, stir and irradiate with ultraviolet light to obtain a mercapto-modified quaternary ammonium salt;

[0009] (3) Waste polyester, modified titanium dioxide powder, mercapto-modified quaternary ammonium salt, Artemisia argyi powder and mixed aqueous solution are mixed in a mass ratio of 1: (0.05~0.10): (0.03~0.05): (0.05~0.08): (6~8), stirred at 25~30℃ to prepare a spinning solution, and hollow shaped fibers are obtained by wet spinning through a cloud-like spinneret. After being shaped, bundled in separate barrels, rapidly stretched and fully formed in three-dimensional crimping, environmentally friendly Artemisia argyi cloud-like fibers are obtained by heat setting.

[0010] Furthermore, in step (1), the molar ratio of dimethylphenylsilane, tris(pentafluorophenyl)borane, ethyl sorbate, titanium dioxide powder, toluene, catalyst and benzoic acid is (0.1~0.3):(0.05~0.15):(25.3~25.5):(0.5~2):(5~6):(0.02~0.05):(0.015~0.03).

[0011] Furthermore, the catalyst is a phosphazene base.

[0012] Furthermore, the specific steps for hydrolyzing the pretreated titanium dioxide powder with lipase in step (1) are as follows: mix titanium dioxide powder and deionized water at a mass ratio of 0.4~0.6:1, stir, add 0.05 times the mass of the pretreated titanium dioxide powder of soybean protein, 0.1% of the mass of the pretreated titanium dioxide powder of disodium hydrogen phosphate, and 0.03 times the mass of the pretreated titanium dioxide powder of RML lipase solution, react for 24 hours under a pressure of 30 mbar, filter, and wash to obtain modified titanium dioxide powder.

[0013] Furthermore, the RML lipase solution is prepared by dissolving 20000L of lipase Palatase in a 0.01M phosphate buffer solution with a pH of 7.4, and sonicating at 300W for 5 minutes to obtain a concentration of 300U / ml.

[0014] Furthermore, in step (2), the ultraviolet irradiation is 365nm ultraviolet light irradiation for 1.0~1.5h.

[0015] Furthermore, in step (3), the waste polyester is waste polyethylene terephthalate that has been crushed, washed and vacuum dried to obtain polyester fragments with a moisture content of 80 ppm.

[0016] Furthermore, the mixed aqueous solution in step (3) contains 12% N,N-dimethylformamide and 16% sulfuric acid by mass.

[0017] Furthermore, the process parameters for wet spinning in step (3) are as follows: the conveying speed is 0.59~0.61mL / min, the outer diameter of the spinneret hole on the spinneret plate is 1.0~1.3mm, and the inner diameter is 0.6~0.8mm. The spinning solution is spun through the hollow profile on the cloud spinneret to obtain hollow profile fibers.

[0018] Furthermore, in step (3), the heat setting temperature is 150~165℃ and the time is 20~25min.

[0019] Furthermore, an environmentally friendly Artemisia cloud-like fabric is prepared by wet spinning modified titanium dioxide powder, Artemisia powder, mercapto-modified quaternary ammonium salt, and waste polyester. The modified titanium dioxide powder is prepared by adding titanium dioxide powder to an ethyl sorbate solution, coating it with a polyethyl sorbate film by in-situ polymerization, and then hydrolyzing it. The mercapto-modified quaternary ammonium salt is prepared by quaternization reaction of N,N,N',N'-tetramethyl-p-phenylenediamine and 6-iodo-1-hexene, followed by UV-click reaction with 11-mercaptoundecyltrimethoxysilane.

[0020] Furthermore, the titanium dioxide powder has a particle size of 80~100nm; the artemisia powder has a particle size of 200 mesh.

[0021] Furthermore, the hydrolysis involves the release of carboxyl groups through enzymatic decomposition.

[0022] Compared with the prior art, the beneficial effects achieved by the present invention are:

[0023] The environmentally friendly Artemisia cloud wool prepared by this invention not only achieves antibacterial properties but also further improves its antistatic ability.

[0024] First, titanium dioxide powder is added to an ethyl sorbate solution, and a polyethyl sorbate film is coated by in-situ polymerization. The film can improve the compatibility between titanium dioxide and the Artemisia argyi velvet matrix and reduce stress concentration. Then, the ethyl sorbate is hydrolyzed to release carboxyl groups to obtain modified titanium dioxide powder. The modified titanium dioxide powder, Artemisia argyi powder and waste polyester are mixed to form a spinning solution. The carboxyl groups generated after hydrolysis can crosslink with the polar groups in the polyester fiber through hydrogen bonding, further increasing the interfacial interaction. The network structure of hydrogen bonding enhances the strength of the fiber, making it easier to stretch and shape in the subsequent spinning process and improving spinnability.

[0025] Secondly, N,N,N',N'-tetramethyl-p-phenylenediamine and 6-iodo-1-hexene undergo a quaternization reaction to prepare quaternary ammonium salts, introducing double bonds into the compounds. Then, a mercapto-modified quaternary ammonium salt is prepared by UV-click reaction with 11-mercaptoundecyltrimethoxysilane. The mercapto-modified quaternary ammonium salt is added to the spinning solution as an antistatic agent, and environmentally friendly Artemisia argyi cloud wool is prepared by wet spinning. Mercapto modification helps the quaternary ammonium salt to be evenly dispersed in the spinning solution, avoids agglomeration, improves the utilization rate of the antistatic agent, and reduces fiber structure unevenness or breakage caused by uneven dispersion of additives. Detailed Implementation

[0026] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0027] To more clearly illustrate the method provided by the present invention, the following embodiments are provided in detail. The testing methods for various indicators of the environmentally friendly mugwort cloud wool produced in the following embodiments are as follows:

[0028] Mechanical properties: The environmentally friendly Artemisia cloud velvet prepared by the same mass of the example and the comparative example was tested for breaking strength in accordance with GB / T8960-2015 "Polyester drawn yarn".

[0029] Antibacterial properties: Environmentally friendly mugwort fleece prepared in the same mass as the examples and comparative examples was tested according to GB / T20944.3-2008 "Evaluation of antibacterial properties of textiles - Part 3: Vibration method". The bacteria used for testing were: Escherichia coli ATCC11229 and Staphylococcus aureus ATCC6538.

[0030] Antistatic performance test: The antistatic performance of the environmentally friendly mugwort cloud wool prepared by the same mass of the example and the comparative example was determined after 20 and 100 washes, in accordance with the method of GB / T12703.1-2008 "Evaluation of electrostatic properties of textiles".

[0031] Example 1: A method for preparing environmentally friendly mugwort cloud wool, comprising the following preparation steps:

[0032] A mixture of dimethylphenylsilane, tris(pentafluorophenyl)borane, 4% by mass of ethyl sorbate, and toluene was prepared. Titanium dioxide powder with a particle size of 80 nm was added, and the mixture was stirred at 300 rpm for 30 min. The catalyst and the remaining ethyl sorbate were added sequentially, and the mixture was stirred at 200 rpm for 15 min. Benzoic acid was then added, and the mixture was filtered. The powder was washed twice with acetone and twice with deionized water, and dried at 30°C to constant weight to obtain pretreated titanium dioxide powder. The pretreated titanium dioxide powder and deionized water were mixed at a mass ratio of 0.4:1 and stirred at 35°C and 150 rpm for 10 min. Then, 0% by mass of the pretreated titanium dioxide powder was added. Soybean protein (0.05 times its weight), disodium hydrogen phosphate (0.1% by weight of pretreated titanium dioxide powder), and RML lipase solution (0.03 times by weight of pretreated titanium dioxide powder) were reacted at 30 mbar for 24 h. The solid was filtered, washed twice with deionized water, and dried at 30 °C to constant weight to obtain modified titanium dioxide powder. The molar ratio of dimethylphenylsilane, tris(pentafluorophenyl)borane, ethyl sorbate, titanium dioxide powder, toluene, catalyst, and benzoic acid was 0.1:0.05:25.3:0.5:5:0.02:0.015. The catalyst was phosphazene base. The RML lipase solution was prepared by dissolving 20,000 L of palatase lipase in 0.01 M phosphate buffer at pH 7.4, sonicating at 300 W for 5 min, and achieving a concentration of 300 U / ml.

[0033] (2) Under nitrogen protection, N,N,N',N'-tetramethyl-p-phenylenediamine and 6-iodo-1-hexene were mixed in a molar ratio of 1.1:1 to obtain mixture B. Mixture B was dissolved in anhydrous toluene at a mass of 2 times that of mixture B. The mixture was heated to 60°C and stirred at 150 r / min for 4 h. After cooling to room temperature, the mixture was washed 3 times with saturated sodium bicarbonate solution, filtered to obtain the organic phase, and dried with anhydrous sodium sulfate to obtain quaternary ammonium salt. 11-mercaptoundecyltrimethoxysilane and quaternary ammonium salt were mixed in a molar ratio of 1.1:1 to obtain mixture C. Mixture C was dissolved in anhydrous toluene at a mass of 2 times that of mixture C. 300 ppm of benzoyl peroxide was added, and the mixture was stirred at 100 r / min for 5 min. The mixture was then irradiated with ultraviolet light at a wavelength of 365 nm and a power of 300 W for 1.0 h to obtain mercapto-modified quaternary ammonium salt.

[0034] (3) Waste polyester, modified titanium dioxide powder, mercapto-modified quaternary ammonium salt, Artemisia argyi powder with a particle size of 200 mesh, and mixed aqueous solution are mixed in a mass ratio of 1:0.05:0.03:0.05:6 and stirred at 25℃ and 200r / min for 15min to prepare a spinning solution. The spinning solution is wet-spun through a cloud-like spinneret to obtain hollow profiled fibers. After the hollow profiled fibers are fully formed by rapid setting, bin bundling, rapid stretching, and three-dimensional crimping, they are heat-set at 150℃ for 20min to obtain environmentally friendly Artemisia argyi cloud-like fibers. The mixed water-soluble The solution contains 12% N,N-dimethylformamide and 16% sulfuric acid by mass. The wet spinning process parameters are: a conveying speed of 0.59 mL / min, an outer diameter of 1.0 mm and an inner diameter of 0.6 mm for the spinneret holes, and the spinning solution is spun through a hollow profile spinneret to obtain hollow profile fibers. The waste polyester is waste polyethylene terephthalate that has been crushed and then ultrasonically cleaned with deionized water, acetone and isopropanol in sequence, and dried at 70℃ for 10 h to obtain polyester fragments with a water content of 80 ppm.

[0035] Example 2; A method for preparing environmentally friendly Artemisia argyi cloud wool, comprising the following preparation steps:

[0036] (1) Mix dimethylphenylsilane, tris(pentafluorophenyl)borane, 4% of ethyl sorbate and toluene to obtain a mixture. Add titanium dioxide powder with a particle size of 90 nm, stir at 300 r / min for 30 min, add catalyst and the remaining ethyl sorbate in sequence, stir at 200 r / min for 15 min, then add benzoic acid, filter, wash twice with acetone, then wash twice with deionized water, dry at 30 °C to constant weight to obtain pretreated titanium dioxide powder. Mix the pretreated titanium dioxide powder and deionized water at a mass ratio of 0.5:1, stir at 35 °C and 150 r / min for 10 min, add the pretreated titanium dioxide powder... 0.05 times the amount of soybean protein, 0.1% of the mass of pretreated titanium dioxide powder, disodium hydrogen phosphate, and 0.03 times the mass of pretreated titanium dioxide powder RML lipase solution were reacted at 30 mbar for 24 h. The solid was filtered, washed twice with deionized water, and dried at 30 °C to constant weight to obtain modified titanium dioxide powder. The molar ratio of dimethylphenylsilane, tris(pentafluorophenyl)borane, ethyl sorbate, titanium dioxide powder, toluene, catalyst, and benzoic acid was 0.2:0.1:25.4:1.5:5:0.03:0.025. The catalyst was phosphazene base. The RML lipase solution was prepared by dissolving 20,000 L of palatase lipase in 0.01 M phosphate buffer solution at pH 7.4, sonicating at 300 W for 5 min, and preparing a concentration of 300 U / ml.

[0037] (2) Under nitrogen protection, N,N,N',N'-tetramethyl-p-phenylenediamine and 6-iodo-1-hexene were mixed in a molar ratio of 1.2:1 to obtain mixture B. Mixture B was dissolved in anhydrous toluene at a mass of 3 times that of mixture B. The mixture was heated to 70°C and stirred at 150 r / min for 5 h. After cooling to room temperature, the mixture was washed 3 times with saturated sodium bicarbonate solution, filtered to obtain the organic phase, and dried with anhydrous sodium sulfate to obtain quaternary ammonium salt. 11-mercaptoundecyltrimethoxysilane and quaternary ammonium salt were mixed in a molar ratio of 1.2:1 to obtain mixture C. Mixture C was dissolved in anhydrous toluene at a mass of 3 times that of mixture C. 300 ppm of benzoyl peroxide was added, and the mixture was stirred at 100 r / min for 5 min. The mixture was then irradiated with ultraviolet light at a wavelength of 365 nm and a power of 300 W for 1.3 h to obtain mercapto-modified quaternary ammonium salt.

[0038] (3) Waste polyester, modified titanium dioxide powder, mercapto-modified quaternary ammonium salt, Artemisia argyi powder with a particle size of 200 mesh, and mixed aqueous solution are mixed in a mass ratio of 1:0.07:0.04:0.07:7 and stirred at 28℃ and 200r / min for 15min to prepare a spinning solution. The spinning solution is wet-spun through a cloud-like spinneret to obtain hollow profiled fibers. After the hollow profiled fibers are fully formed by rapid setting, bin bundling, rapid stretching, and three-dimensional crimping, they are heat-set at 160℃ for 23min to obtain environmentally friendly Artemisia argyi cloud-like fibers. The mixed aqueous solution is used to prepare the spinning solution. The solution contains 12% N,N-dimethylformamide and 16% sulfuric acid by mass. The wet spinning process parameters are: a conveying speed of 0.60 mL / min, an outer diameter of 1.2 mm and an inner diameter of 0.7 mm for the spinneret holes, and the spinning solution is spun through a hollow profile spinneret to obtain hollow profile fibers. The waste polyester is waste polyethylene terephthalate that has been crushed and then ultrasonically cleaned with deionized water, acetone and isopropanol in sequence, and dried at 70℃ for 10 h to obtain polyester fragments with a water content of 80 ppm.

[0039] Example 3; A method for preparing environmentally friendly Artemisia argyi cloud wool, comprising the following preparation steps:

[0040] (1) Mix dimethylphenylsilane, tris(pentafluorophenyl)borane, 4% by mass of ethyl sorbate and toluene to obtain a mixture. Add titanium dioxide powder with a particle size of 100 nm, stir at 300 r / min for 30 min, add catalyst and the remaining ethyl sorbate in sequence, stir at 200 r / min for 15 min, then add benzoic acid, filter, wash twice with acetone, then wash twice with deionized water, and dry at 30 °C to constant weight to obtain pretreated titanium dioxide powder. Mix the pretreated titanium dioxide powder and deionized water at a mass ratio of 0.6:1, stir at 35 °C and 150 r / min for 10 min, and add the pretreated titanium dioxide powder. Soybean protein (0.05 times by weight), disodium hydrogen phosphate (0.1% by weight of pretreated titanium dioxide powder), and RML lipase solution (0.03 times by weight of pretreated titanium dioxide powder) were reacted at 30 mbar for 24 h. The solid was filtered, washed twice with deionized water, and dried at 30 °C to constant weight to obtain modified titanium dioxide powder. The molar ratio of dimethylphenylsilane, tris(pentafluorophenyl)borane, ethyl sorbate, titanium dioxide powder, toluene, catalyst, and benzoic acid was 0.3:0.15:25.5:2:6:0.05:0.03. The catalyst was phosphazene base. The RML lipase solution was prepared by dissolving 20,000 L of palatase lipase in 0.01 M phosphate buffer at pH 7.4, sonicating at 300 W for 5 min, and achieving a concentration of 300 U / ml.

[0041] (2) Under nitrogen protection, N,N,N',N'-tetramethyl-p-phenylenediamine and 6-iodo-1-hexene were mixed in a molar ratio of 1.2:1 to obtain mixture B. Mixture B was dissolved in anhydrous toluene at a mass of 3 times that of mixture B. The mixture was heated to 80°C and stirred at 150 r / min for 6 h. After cooling to room temperature, the mixture was washed 3 times with saturated sodium bicarbonate solution, filtered to obtain the organic phase, and dried with anhydrous sodium sulfate to obtain quaternary ammonium salt. 11-mercaptoundecyltrimethoxysilane and quaternary ammonium salt were mixed in a molar ratio of 1.3:1 to obtain mixture C. Mixture C was dissolved in anhydrous toluene at a mass of 3 times that of mixture C. 300 ppm of benzoyl peroxide was added, and the mixture was stirred at 100 r / min for 5 min. The mixture was then irradiated with ultraviolet light at a wavelength of 365 nm and a power of 300 W for 1.5 h to obtain mercapto-modified quaternary ammonium salt.

[0042] (3) Waste polyester, modified titanium dioxide powder, mercapto-modified quaternary ammonium salt, Artemisia argyi powder with a particle size of 200 mesh, and a mixed aqueous solution are mixed in a mass ratio of 1:0.10:0.05:0.08:8 and stirred at 30℃ and 200r / min for 15min to prepare a spinning solution. The spinning solution is wet-spun through a cloud-like spinneret to obtain hollow profiled fibers. After the hollow profiled fibers are fully formed by rapid setting, bin bundling, rapid stretching, and three-dimensional crimping, they are heat-set at 165℃ for 25min to obtain environmentally friendly Artemisia argyi cloud-like fibers; wherein the mixed water-soluble The solution contains 12% N,N-dimethylformamide and 16% sulfuric acid by mass. The wet spinning process parameters are: a conveying speed of 0.61 mL / min, an outer diameter of 1.3 mm and an inner diameter of 0.8 mm for the spinneret orifice, and the spinning solution is spun through a hollow profile spinneret to obtain hollow profile fibers. The waste polyester is waste polyethylene terephthalate that has been crushed and then ultrasonically cleaned with deionized water, acetone and isopropanol in sequence, and dried at 70℃ for 10 h to obtain polyester fragments with a water content of 80 ppm.

[0043] Comparative Example 1; The difference between Comparative Example 1 and Example 2 is that step (1) is omitted, and the modified titanium dioxide powder in step (3) is replaced with titanium dioxide powder; the remaining steps are the same as in Example 2.

[0044] Comparative Example 2; The difference between Comparative Example 2 and Example 2 is that steps (1) and (3) are different. Step (1) is changed to: mixing dimethylphenylsilane, tris(pentafluorophenyl)borane, 4% of the mass of ethyl sorbate and toluene to obtain a mixture, adding titanium dioxide powder, stirring at 300 r / min for 30 min, adding catalyst and the remaining ethyl sorbate in sequence, stirring at 200 r / min for 15 min, then adding benzoic acid, filtering, washing twice with acetone, then washing twice with deionized water, drying at 30°C to constant weight to obtain pretreated titanium dioxide powder; wherein the molar ratio of dimethylphenylsilane, tris(pentafluorophenyl)borane, ethyl sorbate, titanium dioxide powder, toluene, catalyst and benzoic acid is 0.2:0.1:25.4:1.5:5:0.03:0.025; the catalyst is phosphazene base; the modified titanium dioxide powder in step (3) is replaced with pretreated titanium dioxide powder; the remaining steps are the same as in Example 2.

[0045] Comparative Example 3; The difference between Comparative Example 3 and Example 2 is that steps (2) and (3) are different. Step (2) is changed to: Under nitrogen protection, N,N,N',N'-tetramethyl-p-phenylenediamine and 6-iodo-1-hexene are mixed at a molar ratio of 1.2:1 to obtain mixture B. Mixture B is dissolved in anhydrous toluene at a mass of 3 times that of mixture B. The temperature is raised to 70°C and stirred at 150 r / min for 5 h. The mixture is cooled to room temperature, washed 3 times with saturated sodium bicarbonate solution, filtered to obtain the organic phase, and dried with anhydrous sodium sulfate to obtain quaternary ammonium salt. The mercapto-modified quaternary ammonium salt in step (3) is changed to quaternary ammonium salt. The remaining steps are the same as in Example 2.

[0046] Comparative Example 4; The difference between Comparative Example 4 and Example 2 is the difference in step (2). Step (2) is changed to: 11-mercaptoundecyltrimethoxysilane and octadecyldimethylhydroxyethyl quaternary ammonium nitrate are mixed at a molar ratio of 1.2:1 to obtain mixture C. Mixture C is dissolved in anhydrous toluene at a mass of 3 times that of mixture C. 300 ppm of benzoyl peroxide is added. The mixture is stirred at 100 r / min for 5 min and irradiated with ultraviolet light at a wavelength of 365 nm and a power of 300 W for 1.3 h to obtain mercapto-modified quaternary ammonium salt. The remaining steps are the same as in Example 2.

[0047] Comparative Example 5; The difference between Comparative Example 5 and Example 2 lies in step (2). Step (2) is changed to: Under nitrogen protection, N,N,N',N'-tetramethyl-p-phenylenediamine and 6-iodo-1-hexene are mixed at a molar ratio of 1.2:1 to obtain mixture B. Mixture B is dissolved in anhydrous toluene at a mass of 3 times that of mixture B. The mixture is heated to 70°C and stirred at 150 r / min for 5 h. After cooling to room temperature, the mixture is washed 3 times with saturated sodium bicarbonate solution. The organic phase is filtered and dried with anhydrous sodium sulfate to obtain a quaternary ammonium salt. 11-mercaptoundecyltrimethoxysilane and the quaternary ammonium salt are mixed at a molar ratio of 1.2:1 to obtain mixture C. Mixture C is dissolved in anhydrous toluene at a mass of 3 times that of mixture C. 300 ppm of benzoyl peroxide is added and the mixture is stirred at 100 r / min for 1.3 h to obtain a mercapto-modified quaternary ammonium salt. The remaining steps are the same as in Example 2.

[0048] Example of effect

[0049] Table 1 below shows the performance analysis results of the environmentally friendly Artemisia cloud wool produced using Examples 1 to 3 and Comparative Examples 1 to 5 of the present invention.

[0050] Table 1

[0051]

[0052] A comparison of the experimental data from Example 2 with those from Comparative Examples 1 and 2 reveals that, in this invention, titanium dioxide powder is added to an ethyl sorbate solution, and an in-situ polymerization method is used to coat a polyethyl sorbate film. This film improves the compatibility between titanium dioxide and the Artemisia argyi cloud wool matrix, reducing stress concentration. Then, the ethyl sorbate is hydrolyzed to release carboxyl groups, yielding modified titanium dioxide powder. The modified titanium dioxide powder, Artemisia argyi powder, and waste polyester are then wet-spun to prepare Artemisia argyi cloud wool. The carboxyl groups generated after hydrolysis can crosslink with the polar groups in the polyester fiber through hydrogen bonds, further increasing interfacial interaction. The network structure of the hydrogen-bonded crosslinks enhances the fiber strength, making it easier to stretch and shape during subsequent spinning processes, thus improving spinnability.

[0053] A comparison of the experimental data from Example 2 with those from Comparative Examples 3, 4, and 5 reveals that the present invention involves the quaternization reaction of N,N,N',N'-tetramethyl-p-phenylenediamine and 6-iodo-1-hexene to prepare a quaternary ammonium salt, introducing double bonds into the compound. This is followed by an addition reaction with excess 11-mercaptoundecyltrimethoxysilane to prepare a mercapto-modified quaternary ammonium salt. Using the mercapto-modified quaternary ammonium salt as an antistatic agent, Artemisia argyi fibers are placed in an antistatic agent solution, and an antistatic film is prepared under ultraviolet light to obtain environmentally friendly Artemisia argyi fibers. The positively charged nitrogen atoms in the quaternary ammonium salt can adsorb water molecules from the environment to form a conductive layer. The mercapto groups in the quaternary ammonium salt, through click chemistry, firmly anchor the antistatic agent to the Artemisia argyi fibers in a covalent bond form, improving the durability of the film.

[0054] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No markings in the claims should be construed as limiting the scope of the claims.

Claims

1. A method for preparing environment-friendly wormwood cloud velvet, characterized in that, The preparation steps include: (1) a mixture of dimethylphenylsilane, tris(pentafluorophenyl)borane, 4% of ethyl sorbate and toluene is mixed to obtain a mixture, titanium dioxide powder is added, stirring, catalyst, the rest of the ethyl sorbate is added in turn, and benzoic acid is added, filtered and washed to obtain pretreated titanium dioxide powder, and the pretreated titanium dioxide powder is hydrolyzed by lipase to obtain modified titanium dioxide powder; (2) under nitrogen protection, N,N,N',N'-tetramethyl-p-phenylenediamine and 6-iodo-1-hexene are mixed to obtain a mixture B, the mixture B is dissolved in anhydrous toluene, heated to 60-80℃, stirred for 4-6h, cooled to room temperature, washed and dried to obtain a quaternary ammonium salt, 11-mercaptoundecyltrimethoxysilane and the quaternary ammonium salt are mixed to obtain a mixture C, the mixture C is dissolved in anhydrous toluene, 300ppm of benzoyl peroxide is added, stirred and irradiated by ultraviolet light to obtain a thiol-modified quaternary ammonium salt; (3) waste polyester, modified titanium dioxide powder, thiol-modified quaternary ammonium salt, artemisia powder and mixed aqueous solution are mixed according to the mass ratio of 1:(0.05-0.10):(0.03-0.05):(0.05-0.08):(6-8), stirred at 25-30℃, configured into a spinning solution, and hollow profiled fibers are prepared by wet spinning through a cloud wool spinneret, and after shaping, barrel separation, rapid drawing and three-dimensional crimping, heat setting is performed to obtain environment-friendly artemisia cloud wool; The catalyst in step (1) is a phosphazene base; The mixed aqueous solution in step (3) contains 12% of N,N-dimethylformamide and 16% of sulfuric acid by mass fraction.

2. The method for preparing an environmentally friendly Artemisia argyi cloud-like fabric according to claim 1, characterized in that, The molar ratio of dimethylphenylsilane, tris(pentafluorophenyl)borane, ethyl sorbate, titanium dioxide powder, toluene, catalyst and benzoic acid in step (1) is (0.1-0.3):(0.05-0.15):(25.3-25.5):(0.5-2):(5-6):(0.02-0.05):(0.015-0.03).

3. The method for preparing an environmentally friendly Artemisia argyi cloud-like fabric according to claim 1, characterized in that, The specific steps for hydrolyzing the pretreated titanium dioxide powder with lipase in step (1) are as follows: The pretreated titanium dioxide powder and deionized water are mixed according to the mass ratio of 0.4-0.6:1, stirred, and 0.05 times the mass of the pretreated titanium dioxide powder of soybean protein, 0.1% of the pretreated titanium dioxide powder of sodium phosphate dibasic and 0.03 times the mass of the pretreated titanium dioxide powder of RML lipase enzyme solution are added, and the reaction is carried out under 30mbar pressure for 24h, filtered and washed to obtain modified titanium dioxide powder.

4. The method for preparing an environmentally friendly Artemisia cloud-like fabric according to claim 1, characterized in that, The ultraviolet light irradiation in step (2) is irradiated by 365nm ultraviolet light for 1.0-1.5h.

5. The method as claimed in claim 1, wherein the environment friendly artemisia cloud wool is prepared by the steps of: The waste polyester in step (3) is waste polyethylene terephthalate which is crushed, cleaned and vacuum dried to obtain polyester fragments with a water content of 80ppm.

6. The method for preparing an environmentally friendly Artemisia argyi cloud-like fabric according to claim 1, characterized in that, The process parameters of the wet spinning in the step (3) are as follows: the delivery speed is 0.59-0.61 mL / min, the outer diameter of the spinning hole on the spinneret is 1.0-1.3 mm, and the inner diameter is 0.6-0.8 mm, and the spinning solution is spun into hollow profiled fibers through the hollow profiled spinneret.

7. The method for preparing an environmentally friendly Artemisia argyi cloud-like fabric according to claim 1, characterized in that, The temperature of the heat setting in the step (3) is 150-165 DEG C.

8. The method for preparing an environmentally friendly Artemisia argyi cloud-like fabric according to claim 1, characterized in that, The time of the heat setting in the step (3) is 20-25 min.

9. An eco-friendly mugwort cloud wool, characterized by, The environment-friendly wormwood cloud wool is prepared by the preparation method in any one of claims 1-8.

10. The environment-friendly mugwort cloud wool according to claim 9, characterized in that, The particle size of the titanium dioxide powder is 80-100 nm, and the wormwood powder particle is 200 mesh.

11. The environment-friendly mugwort cloud wool according to claim 10, characterized in that, The hydrolysis is to release carboxyl groups through enzymatic hydrolysis.

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