Core-shell structure material retaining effective components and preparation method thereof

Abstract

The invention relates to a core-shell structure material retaining effective components and a preparation method thereof, which comprises the following steps: mixing the effective components, a micro-nano hole inorganic material with a specific surface area of 120-980 m < 2 > / g and distilled water to obtain a raw material component, and carrying out hydrothermal treatment to fill the effective components into the micro-nano hole inorganic material to obtain a powder material, and forming an inorganic oxide coating layer on the surface of the powder material by a sol-gel method to obtain the core-shell structure material containing the effective components. The micro-nano hole inorganic material with a high specific surface area is matched with hydrothermal treatment and an inorganic oxide coating layer is formed, so that effective components of organic matters, such as caffeine obtained from coffee residues or tea residues, a lavender extract obtained from lavender, a wormwood extract obtained from wormwood and the like, can be effectively dissolved in water, and the organic matters can be effectively dissolved in water. And the material stably exists in the core-shell structure material and is not easily lost at a high temperature.

Description

Technical Field

[0001] This invention relates to a core-shell structured material, and more particularly to a core-shell structured material for textile yarns that retains effective components and its preparation method. Background Technology

[0002] Currently, in the production of functional yarns, porous materials containing effective components such as organic matter are usually added to the raw materials that form the yarn, thereby giving the spun yarn the intended functionality.

[0003] However, given that the effective components of organic matter are typically small molecular weight organic compounds with relatively poor heat resistance, they are prone to volatilization or even decomposition during the spinning process when ambient temperatures rise. Of particular concern is the current industry challenge of producing functional yarns using polyester or nylon melt spinning processes at temperatures exceeding 260°C. At these high temperatures, the effective components of the organic matter are almost entirely lost during the manufacturing process.

[0004] The common practice is to utilize porous materials in raw materials to retain the effective organic components within them. The nanoscale pores in the porous material then adsorb these components, reducing their loss during subsequent processing. However, this method, relying solely on the adsorption of these nanoscale pores, does not substantially improve the high-temperature spinning process, as the effective organic components continue to volatilize and dissipate in the high-temperature environment. Therefore, how to produce functional yarns using existing spinning processes while retaining the various effective organic components that give the yarn its functionality remains a key research and innovation topic in the textile technology field.

[0005] One of the existing related technologies is the published patent application TW201350150A, which discloses the use of a root component in fibers, fabrics or cloths, and discloses three ways to combine the effective components of organic matter into yarns.

[0006] The first method involves directly grinding a single root plant into a powder of 26μm to 60μm using a nano-powder mill, and then uniformly mixing the single root powder into a base material selected from polypropylene or any textile raw material. Taking polypropylene as an example, at a temperature of 160℃ to 180℃, the base material mixed with the single root powder is drawn into polypropylene fibers containing a single root, or further processed into fabric containing a single root.

[0007] The second method involves mixing the micro-powder into the gel to obtain granular micro-powder gel, and then adsorbing the micro-powder gel onto the fiber cloth at a temperature of 100°C to 120°C.

[0008] The third method involves grinding the entire root into powder using a pulverizer, then extracting it with a 70% alcohol solution (10 times its volume). The extract is collected, filtered through filter paper under vacuum, and then concentrated under reduced pressure to remove the solvent, yielding the root extract. This extract is then subjected to adsorption treatment with various adsorbents, including activated carbon, diatomaceous earth, and β-cyclodextrin, to obtain a nanoporous medium for adsorbing the root. Finally, the nanoporous medium is subjected to the aforementioned spinning or adsorption process. More specifically, when using activated carbon for adsorption, activated carbon is added to the alcohol extract containing the root extract, and the mixture is stirred for 6 hours to allow the activated carbon to adsorb the root extract. The resulting solution is then filtered and freeze-dried to obtain activated carbon that has adsorbed the root extract. When using diatomaceous earth or β-cyclodextrin for adsorption treatment, diatomaceous earth and β-cyclodextrin are added to two alcoholic extracts containing one root extract, respectively, and stirred for 12 hours to allow the diatomaceous earth and β-cyclodextrin to adsorb the one root extract, respectively. After filtration and freeze-drying, diatomaceous earth and β-cyclodextrin adsorbing the one root extract are obtained.

[0009] In the field of textile technology, patent application TW200425946A discloses the composition and preparation of nano- and micro-sized coated particles. The technology involves using a sol-gel method to coat liquid or solid microparticles formed from organic matter with an inorganic colloid as a dense or porous coating layer, thereby enhancing the material's physical properties and chemical and thermal resistance. The liquid or solid microparticles are obtained by stirring organic matter, such as fragrances, in the presence of surfactants, thereby forming microcells through emulsification. The inorganic colloid used to form the coating layer is made of materials such as silicon oxide, zirconium oxide, or titanium oxide. In particular, when the coating layer has a dense structure, it can protect the organic matter to reduce loss during processing or reduce contact with oxygen, thus improving the material's flame retardancy. When the coating layer has a porous structure, the coated organic matter can be removed by high-temperature treatment or extraction to form hollow particles, or the coated organic matter can be continuously released over time as adjustable-release coated microparticles.

[0010] On the other hand, Tsinghua University filed a patent application CN103305965A, disclosing a silicon-carbon composite material with nanoporous structure, its preparation method and uses. The material includes nano-silicon particles and a nano-carbon fiber matrix. The nano-silicon particles are dispersed in the nano-carbon fiber matrix, and the nano-carbon fiber matrix has nanopores and micropores connecting the nanopores. The preparation method involves dissolving nano-silicon (Si) particles and polyacrylonitrile (PAN) in a solvent to prepare a mixed spinning solution. Then, the mixed spinning solution is electrospun, and the spun fine stream is solidified in a coagulation bath to obtain multi-porous PAN-Si nanocomposite fibers. Then, oxidation treatment and carbonization treatment are performed sequentially to obtain the aforementioned silicon-carbon composite material with nanoporous structure.

[0011] Secondly, patent application CN117758443A discloses a composite nonwoven fabric with high absorption performance and its preparation method. This patent application relates to the field of nonwoven fabrics. More specifically, it selects polylactic acid fiber, PE / PET composite fiber, and sodium alginate fiber as raw materials for composite nonwoven fabrics. Sodium alginate is used as the shell layer and polyethylene oxide is used as the core layer. A composite sodium alginate fiber with a core-shell structure is prepared by coaxial electrospinning. Gelatin and a composite organic framework are introduced into the shell layer, and an emulsion of eugenol is introduced into the core layer. Then, an antibacterial impregnation solution is prepared using the composite organic framework, chitosan, and dopamine hydrochloride. Subsequently, a titanium-based organic framework is synthesized using 2-aminoterephthalic acid as a ligand. Layered hydroxides are grown in situ on the titanium-based organic framework using copper nitrate and urea. Finally, the composition and content of the base fabric and the moisture-absorbing web are controlled so that a composite fiber web with a gradient structure is formed after layering and carding.

[0012] Furthermore, patent application CN117815458A discloses a sustained-release energy metabolism factor and a method for promoting osteofibrous membranes and their preparation, relating to the field of fibrous membrane technology, particularly including the following steps in the preparation method:

[0013] (1) Disperse the energy metabolism regulator in an organic solvent, then add a polymer, shake and mix to obtain a spinning solution; electrospin, dry to obtain a fiber membrane substrate;

[0014] (2) Place the fiber membrane substrate obtained in step (1) in a polyphenol compound solution, let it stand, take it out and rinse it to obtain a fiber membrane grafted with polyphenol compound.

[0015] (3) Place the fibrous membrane of the grafted polyphenol compound obtained in step (2) in an aqueous solution of fibronectin, let it stand, take it out and rinse it to obtain a slow-release energy metabolism factor and a bone fibrous membrane.

[0016] The feature of this patent application is that a core-shell structure is prepared by electrospinning, the core layer slowly releases and regulates energy metabolism factors, and the shell layer, in conjunction with polyphenolic compounds and grafted proteins, modifies the surface of the fibrous membrane substrate, thereby achieving vascularized bone tissue regeneration.

[0017] Among the existing technologies listed, it is evident that industry efforts focus on ensuring that the formed yarns, fabrics, composite fiber webs, fiber membranes, or composite materials retain the effective components necessary to perform their intended functions. However, it is also known that in current technologies, these effective components continue to volatilize and dissipate in subsequent processing environments. These prior technologies all employ relatively low-temperature processes, such as 160°C to 180°C for polypropylene yarns, or 100°C to 120°C for direct application to the yarn surface, or even lower-temperature electrospinning processes. There is still no suitable solution for melt spinning of polyester and nylon, which requires temperatures above 260°C. Therefore, how to produce functional yarns using existing high-temperature melt spinning processes while retaining the various organic effective components that impart functionality to the yarn remains a challenge requiring continued research and innovation from industry players. Summary of the Invention

[0018] One object of the present invention is to provide a method for preparing a core-shell structured material suitable for melt spinning of polyester and nylon while retaining the effective components.

[0019] Another object of the present invention is to provide a core-shell structured material suitable for melt spinning of polyester and nylon while retaining the effective components.

[0020] The present invention provides a method for preparing a core-shell structured material suitable for melt spinning of polyester and nylon while retaining effective components, comprising steps (a), (b), and (c).

[0021] Step (a) involves mixing the active ingredient, the micro / nano porous inorganic material, and distilled water, and dissolving the active ingredient in the distilled water to obtain the raw material components. The specific surface area of ​​the micro / nano porous inorganic material is in the range of 120 m². 2 / g to 980m 2 / g.

[0022] Step (b) involves hydrothermally treating the raw material components to inject an aqueous solution containing the effective ingredient into the pores of the micro / nano porous inorganic material, thereby obtaining a powder material containing the effective ingredient.

[0023] Step (c) involves forming an inorganic oxide coating layer with micro- and nano-pores on the surface of the powder material using a sol-gel method to obtain a core-shell structure material containing the active ingredient.

[0024] Preferably, in the method for preparing the core-shell structured material that retains the effective components according to the present invention, the effective components are selected from caffeine powder, lavender extract, artemisia extract, or any combination of the aforementioned components. The caffeine powder is obtained by processing caffeine raw materials that can extract caffeine, and the caffeine raw materials are selected from coffee grounds, tea grounds, or a combination of the aforementioned two.

[0025] Preferably, in the method for preparing the core-shell structured material that retains the effective components described in this invention, the micro-nano porous inorganic material is selected from zeolite, halloysite, activated carbon, or any combination of the three.

[0026] Preferably, in the method for preparing the core-shell structured material that retains the effective components according to the present invention, the particle size range of the micro-nano porous inorganic material is 0.1 μm to 1 μm.

[0027] Preferably, in the method for preparing the core-shell structured material that retains the effective components according to the present invention, the hydrothermal treatment is performed at 100°C to 160°C and 1.0 kg / cm². 2 G up to 6.0 kg / cm 2 Performed under G pressure for 2 hours.

[0028] Preferably, in the method for preparing the core-shell structured material retaining the effective components according to the present invention, step (b) includes: after performing the hydrothermal treatment, the aqueous solution containing the effective components is injected into the pores of the micro-nano porous inorganic material to obtain a mixed liquid containing powder material, and the mixed liquid is centrifuged and filtered to obtain a filter cake, and the filter cake is dried to obtain the powder material.

[0029] Preferably, in the method for preparing the core-shell structured material that retains the effective components according to the present invention, the inorganic oxide coating layer is composed of silicon oxide or titanium oxide, and step (c) includes: forming the inorganic oxide coating layer on the surface of the powder material by sol-gel method, collecting the precipitate, and washing, centrifuging and filtering, and drying the precipitate to obtain the core-shell structured material.

[0030] Secondly, this invention provides a core-shell structured material that retains effective components, comprising a powder material and an inorganic oxide coating layer. The powder material includes a micro / nano porous inorganic material and effective components. The micro / nano porous inorganic material includes multiple micro / nano-sized pores. The inorganic oxide coating layer is formed on the surface of the micro / nano porous inorganic material of the powder material. The effective components are present within the pores of the micro / nano porous inorganic material. Utilizing the high-temperature resistance and vapor pressure resistance of the inorganic material, it can withstand the vapor pressure generated by the effective components at high temperatures. The powder material is prepared by a method including the following steps: first mixing the effective components, with a specific surface area ranging from 120 m²... 2 / g to 980m 2 A raw material component is obtained by dissolving the active ingredient in distilled water at a concentration of / g of micro / nano porous inorganic material. The raw material component is then subjected to hydrothermal treatment, resulting in an aqueous solution containing the active ingredient being injected into the pores of the micro / nano porous inorganic material to obtain the powder material containing the active ingredient. The inorganic oxide coating layer is formed on the surface of the micro / nano porous inorganic material using a sol-gel method.

[0031] Preferably, in the core-shell structured material that retains the effective components described in this invention, the effective components are selected from caffeine powder, lavender extract, artemisia extract, or any combination of the aforementioned components. The caffeine powder is obtained by processing caffeine raw materials capable of extracting caffeine, and the caffeine raw materials are selected from coffee grounds, tea leaves, or any combination of the aforementioned two. The micro-nano porous inorganic material is selected from zeolite, halloysite, activated carbon, or any combination of the aforementioned three.

[0032] Preferably, in the core-shell structured material that retains the effective components according to the present invention, the particle size range of the micro-nano porous inorganic material is 0.1 μm to 1 μm.

[0033] The beneficial effect of this invention is that by using a 120m 2 / g to 980m 2 A high specific surface area micro / nano porous inorganic material is used, which, combined with hydrothermal treatment to infuse the active ingredients into the pores of the micro / nano porous inorganic material, and the formation of an inorganic oxide coating layer using the sol-gel method, allows the active ingredients to remain within the micro / nano-scale pores of the micro / nano porous inorganic material and be protected by the inorganic oxide coating layer. This results in a core-shell structure material containing the active ingredients with good temperature stability, preventing the active ingredients from volatilizing and dissipating under high-temperature environments. Furthermore, when this core-shell structure material containing the active ingredients is further applied to high-temperature spinning processes, the active ingredients can be retained without loss, thus enabling the manufacture of high-quality functional yarns. Attached Figure Description

[0034] Figure 1 This is a flowchart illustrating one embodiment of the method for preparing the core-shell structured material that retains the effective components of the present invention;

[0035] Figure 2 It is a three-dimensional sectional view, illustrating the following: Figure 1 The core-shell structure material obtained in the illustrated embodiment;

[0036] Figure 3 It is a flowchart illustrating the method of preparing core-shell structured materials that retain the effective components to obtain the embodiments 1 to 16, and the content analysis of the effective components in the embodiments 1 to 16;

[0037] Figure 4 It is a flowchart illustrating the method of preparing core-shell structured materials that retain the effective components to obtain the embodiments 1 to 16, and the temperature stability analysis of the effective components in the embodiments 1 to 16.

[0038] Figure 5 It is a three-dimensional bar graph illustrating the ash content test (5℃ / min to 800℃) analysis results of Examples 1 to 16 of the present invention;

[0039] Figure 6 It is a three-dimensional bar graph illustrating the analysis results of thermogravimetric losses (10℃ / min to 400℃) in Examples 1 to 16 of the present invention;

[0040] Figure 7 This is a line graph illustrating the analysis results of thermogravimetric losses (10°C / min to 400°C) in Examples 3, 7, 11, and 15 of the present invention and Comparative Examples 1 to 4; and

[0041] Figure 8 It is a line graph illustrating the analysis results of thermogravimetric loss (10°C / min to 400°C) in Examples 13 to 16 and Comparative Examples 4 to 7 of the present invention. Detailed Implementation

[0042] See Figure 1 The present invention provides a method for preparing a core-shell structured material that retains effective components, comprising steps (a), (b) and (c).

[0043] Step (a) involves mixing the active ingredient, the micro / nano porous inorganic material, and distilled water, and dissolving the active ingredient in the distilled water to obtain the raw material components. The specific surface area of ​​the micro / nano porous inorganic material is in the range of 120 m². 2 / g to 980m 2 / g.

[0044] Step (b) involves hydrothermally treating the raw material components to inject an aqueous solution containing the effective ingredient into the pores of the micro / nano porous inorganic material, thereby obtaining a powder material containing the effective ingredient.

[0045] Step (c) involves forming an inorganic oxide coating layer with micro- and nano-pores on the surface of the powder material using a sol-gel method to obtain a core-shell structure material containing the active ingredient.

[0046] It should be further noted that there are no particular limitations on the types of active ingredients, and suitable types can be selected according to usage requirements. In some embodiments of the present invention, the active ingredient is selected from caffeine powder, lavender extract, artemisia extract, or any combination of the foregoing. When the active ingredient is selected from caffeine powder, the source of the caffeine powder is not particularly limited. In some embodiments of the present invention, the caffeine powder is obtained by processing caffeine-extractable raw materials, such as coffee grounds, tea leaves, or a combination of the foregoing.

[0047] The micro / nano porous inorganic material in this invention refers to an inorganic material with an average particle size of less than 1 μm and an average pore size of less than 100 nm. Through the aforementioned micro / nano porous inorganic material, pores with an average diameter of less than 120 nm are formed. 2 / g to 980m 2 The high specific surface area of ​​ / g allows an appropriate amount of the active ingredient to be infused into the micro-nano porous inorganic material's micro-nano scale pores, and the active ingredient can be stably present within the micro-nano scale pores of the micro-nano porous inorganic material without being easily lost. In some embodiments of the present invention, the micro-nano porous inorganic material is selected from zeolite, halloysite, activated carbon, or any combination of the foregoing, and the particle size D90 of the micro-nano porous inorganic material ranges from 0.1μm to 1μm, preferably the particle size D50 ranges from 0.1μm to 0.5μm. It should be noted that the particle size D90 range is 0.1 μm to 1 μm, which means that the number of micro-nano porous inorganic materials with a particle size in the range of 0.1 μm to 1 μm accounts for 90% of the total number of micro-nano porous inorganic materials. Similarly, the particle size D50 range is 0.1 μm to 0.5 μm, which means that the number of micro-nano porous inorganic materials with a particle size in the range of 0.1 μm to 0.5 μm accounts for 50% of the total number of micro-nano porous inorganic materials.

[0048] In this invention, the high-pressure environment of the hydrothermal treatment effectively allows the aqueous solution containing the effective component in the raw material to be injected into the pores of the micro / nanoporous inorganic material with a high specific surface area. In some embodiments of this invention, to ensure that the aqueous solution containing the effective component in the raw material can be injected into the pores of the micro / nanoporous inorganic material and to prevent the loss of the effective component due to carbonization, the hydrothermal treatment is carried out in a hydrothermal reactor, with a temperature range of 100°C to 160°C and a pressure range of 1.0 kg / cm². 2 G up to 6.0 kg / cm 2 G. It should be noted that when the hydrothermal treatment temperature exceeds 160℃ and / or the pressure exceeds 6.0 kg / cm², 2 At time G, the active ingredient is prone to carbonization, resulting in a loss of filling amount. Preferably, the temperature range of the hydrothermal treatment is 120°C to 160°C.

[0049] In some embodiments of the present invention, in order to ensure that the aqueous solution containing the effective component in the raw material component is injected into the pores of the micro-nano porous inorganic material in sufficient quantity, the holding time of the hydrothermal treatment is 2 hours when the temperature of the hydrothermal treatment reaches the set temperature condition, or when the pressure of the hydrothermal treatment reaches the set pressure condition.

[0050] In some embodiments of the present invention, step (b) involves, after the hydrothermal treatment, injecting the aqueous solution containing the effective component into the pores of the micro-nano porous inorganic material to obtain a mixed liquid containing the powder material, centrifuging and filtering the mixed liquid to obtain a filter cake, and then drying the filter cake to obtain the powder material.

[0051] This invention forms an inorganic oxide coating layer on the surface of the powder material, thereby preventing the surface of the core-shell structure material from cracking due to the high-temperature environment when it is subsequently applied to other high-temperature processes, such as nylon and polyester yarn processes at temperatures above 260°C. In other words, the inorganic oxide coating layer formed on the powder material will not crack due to the high-temperature environment, thus properly protecting the effective components in the core-shell structure material and avoiding the problem of effective components easily volatilizing and dissipating under high-temperature environments, as is the case in the prior art.

[0052] Specifically, the inorganic oxide coating layer not only prevents the active ingredients from volatilizing and dissipating under high-temperature processing conditions, but also allows the active ingredients to be slowly released from the core-shell structured material during subsequent use through the nanopores of the inorganic oxide coating layer, thereby exerting the beneficial effects of the active ingredients. In some embodiments of the present invention, the inorganic oxide coating layer is composed of silicon oxide or titanium oxide. Step (c) further involves forming the inorganic oxide coating layer on the surface of the powder material using a sol-gel method, collecting the precipitate, and then washing, centrifuging, filtering, and drying the precipitate to obtain the core-shell structured material. In some embodiments of the present invention, the conditions of the sol-gel method are not particularly limited. When the inorganic oxide coating layer is composed of silicon oxide or titanium oxide, the raw materials used are either alkoxides containing silicon or their salt compounds, or alkoxides containing titanium or their salt compounds. The above raw materials are mixed with the powder material and stirred at 60°C for 2 hours. The precipitate is then collected, washed with water, centrifuged, filtered, and dried to form the core-shell structure material. The silicon alkoxide is, for example, but not limited to, tetraethoxysilane and (3-aminopropyl)trimethoxysilane. The titanium alkoxide is, for example, but not limited to, isopropyl titanate and tetrabutyl titanate.

[0053] The present invention will be further described with reference to the following embodiments, but it should be understood that the embodiments are for illustrative purposes only and should not be construed as limiting the implementation of the present invention.

[0054] [Example 1]

[0055] See Figure 1 In step (a), the specific surface area is taken as 120m². 2 / g of zeolite was ground and refined to a particle size of less than 1μm, followed by acid washing to remove impurities, resulting in a micro / nano porous inorganic material. 100g of the active ingredient (caffeine powder), 100g of the micro / nano porous inorganic material, and 1.8 liters of distilled water were placed in a 3-liter hydrothermal reactor and mixed to dissolve the active ingredient in the distilled water, thus obtaining the raw material components.

[0056] In step (b), the raw material components are subjected to hydrothermal treatment in a hydrothermal reactor at 100°C for 2 hours, so that an aqueous solution containing the effective ingredient in the raw material components is injected into the pores of the micro-nano porous inorganic material to obtain a mixed liquid containing powder material, wherein the powder material contains the effective ingredient.

[0057] The mixed liquid is centrifuged and filtered to obtain a filter cake. The filter cake is then dried at 80°C for 24 hours and then dried at 120°C for 1 hour to remove moisture from the filter cake, thereby obtaining the powder material containing the effective ingredients.

[0058] In step (c), the powder material is mixed with distilled water to prepare a powder solution containing 10 wt% of the powder material. 5 parts by weight of isopropyl titanate and 13 parts by weight of isopropanol are mixed and stirred at 60°C for 1 hour to obtain an isopropyl titanate solution. Then, the isopropyl titanate solution, 30 parts by weight of isopropanol, 70 parts by weight of distilled water, and 50 parts by weight of the powder solution are mixed and stirred at 60°C for 2 hours to form a titanium oxide layer with nanopores (i.e., the inorganic oxide coating layer) on the surface of the powder material, and the precipitate is collected. Next, the precipitate is washed with water and centrifuged at 3000 rpm. After three cycles of washing and centrifugation, the washed precipitate is dried at 80°C for 24 hours to obtain the core-shell structured material containing the active ingredient.

[0059] See Figure 2 Specifically, the core-shell structure material comprises a powder material 1 and an inorganic oxide coating layer 2. The powder material 1 includes a micro-nano porous inorganic material 11 and an effective component 12. The micro-nano porous inorganic material 11 includes multiple micro-nano-level pores 110. The effective component 12 fills the pores 110. The inorganic oxide coating layer 2 is formed on the surface of the powder material 1.

[0060] [Examples 2 to 16]

[0061] Examples 2 to 16 are core-shell structured materials containing effective components prepared in a manner similar to that of Example 1, the difference being the specific surface area of ​​the zeolite as shown in Table 1, and the temperature of the hydrothermal treatment.

[0062] [Example 17]

[0063] Example 17 prepared a core-shell structured material containing the active ingredient in a manner similar to Example 1. The difference was that in Example 17, after obtaining a powder solution containing 10 wt% of the powder material in the same manner as in Example 1, 5 parts by weight of tetraethoxysilane, 5 parts by weight of (3-aminopropyl)trimethoxysilane, 13 parts by weight of isopropanol, and 1 part by weight of ammonia were mixed and stirred at 40°C to 60°C for 1 hour to obtain a silica sol. Then, the silica sol, 30 parts by weight of isopropanol, 1 part by weight of distilled water, and 50 parts by weight of the powder solution were mixed and stirred at 60°C for 2 hours to form a silicon oxide layer with micro- and nano-pores on the surface of the powder material, and the precipitate was collected. Next, the precipitate was washed with water and centrifuged at 3000 rpm. After three cycles of washing and centrifugation, the washed precipitate was dried at 80°C for 24 hours to obtain a core-shell structured material containing the active ingredient.

[0064] [Comparative Examples 1 to 7]

[0065] Referring to Table 1, Comparative Examples 1 to 7 obtained powder materials containing the active ingredient in a manner similar to that of Example 1, but the powder materials of Comparative Examples 1 to 7 did not form an inorganic oxide coating layer on the surface.

[0066] [Evaluation Items]

[0067] Analysis of the content of effective ingredients (ash content test): In order to analyze the total content of effective ingredients filling the micro-nano porous inorganic material, both the examples and comparative examples used powder materials containing effective ingredients for analysis. Example 1 is described below, and the remaining examples 2 to 17 and comparative examples 1 to 7 were carried out in the same manner.

[0068] See Figure 3 The original weight of the powder material in Example 1 was weighed and recorded. Then, Example 1 was heated from 25°C to 800°C at a heating rate of 5°C / min and held at that temperature for 2 hours, thereby burning off the organic components in the powder material at a high temperature of 800°C. After completion, the weight of the powder material after high-temperature treatment was weighed and recorded. Then, the weight of the powder material after high-temperature treatment was subtracted from the original weight of the powder material. The resulting weight difference is the weight loss due to heating, that is, the weight of the lost effective organic matter. The weight loss due to heating is then divided by the original weight of the powder material and multiplied by 100% to obtain the effective component content (wt%). The results are shown in Table 1. Figure 5 As shown.

[0069] Temperature stability analysis of the active ingredient: To analyze the temperature stability of the core-shell structure material containing the active ingredient under high temperature conditions, the core-shell structure material of the examples and the powder material of the comparative examples were heated to 400°C to simulate a high-temperature spinning process, and the loss of the active ingredient in each example and comparative example was analyzed. Example 3 is described below, and the remaining examples 1 to 2, 4 to 17 and comparative examples 1 to 7 were carried out in the same manner.

[0070] See Figure 4 In Example 3, the original weight of the core-shell structure material was obtained by weighing. Then, it was heated from 25°C to 400°C at a heating rate of 10°C / min for thermogravimetric analysis. The weight of the heat-treated core-shell structure material was then weighed again. Next, the original weight of the core-shell structure material in Example 3 was subtracted from the weight of the heat-treated core-shell structure material. The resulting weight difference represents the loss of effective components at 400°C. This weight difference was then divided by the original weight of the core-shell structure material and multiplied by 100% to obtain the effective component loss (wt%), as shown in Table 2. Finally, the effective component content of the powder material in Example 3 in Table 1 was subtracted from the effective component loss of the core-shell structure material in Example 3 in Table 2 to obtain the effective component content (wt%) after thermogravimetric analysis (10°C / min to 400°C). The results are summarized in Tables 1 to 3. Figure 6 According to Tables 1 to 3, under the same specific surface area and hydrothermal treatment temperature for micro- and nano-porous inorganic materials, the lower the loss of the effective components, the better the temperature stability of the effective components in the core-shell structure material.

[0071] Table 1

[0072]

[0073]

[0074] Table 2

[0075]

[0076] Table 3

[0077]

[0078] See Table 1. Figure 5 , Figure 6Examples 1 to 16 demonstrate that hydrothermal treatment effectively infuses the liquid containing the active ingredient from the raw material components into the pores of the micro / nano porous inorganic material. Furthermore, at the same hydrothermal treatment temperature, a larger specific surface area of ​​the micro / nano porous inorganic material results in a higher content of the active ingredient in the powder material. This was also confirmed by thermogravimetric analysis at 400°C, which showed the same level of active ingredient content remaining in Examples 1 to 16. Moreover, for the same specific surface area of ​​the micro / nano porous inorganic material, a higher hydrothermal treatment temperature increases the content of the active ingredient in the powder material, indicating improved temperature stability of the active ingredient within the micro / nano porous inorganic material. Performing the hydrothermal treatment at a high specific surface area and 140°C most effectively infuses the liquid containing the active ingredient into the pores of the micro / nano porous inorganic material, thereby resulting in a higher content of active ingredient in the powder material.

[0079] See Table 2. Figure 7 As shown in the results of Examples 3, 7, 11, and 15 and Comparative Examples 1 to 4, at a hydrothermal treatment temperature of 140°C, the content of the effective components in Examples 3, 7, 11, and 15 increased with the increase of the specific surface area of ​​the micro / nano porous inorganic materials. Furthermore, after thermogravimetric analysis at 400°C, the content of the effective components remaining in Examples 3, 7, 11, and 15 also showed this trend, as did the effective components in the powder materials of Comparative Examples 1 to 4. On the other hand, the core-shell structure materials of Examples 3, 7, 11, and 15, using materials with a specific surface area of ​​120 m², [further details needed]. 2 / g to 980m 2 / g of micro / nanoporous inorganic material, combined with hydrothermal treatment and the formation of an inorganic oxide coating layer, therefore, under the same specific surface area and hydrothermal treatment temperature, compared with the powder materials of Comparative Examples 1 to 4, the core-shell structure materials of Examples 3, 7, 11, and 15 have a lower effective component loss. Furthermore, from Figure 7 The results clearly show that Examples 3, 7, 11, and 15 have higher contents of the active ingredient, indicating that the active ingredient has good temperature stability in the core-shell structure materials of Examples 3, 7, 11, and 15. Comparative Examples 1 to 4 did not form an inorganic oxide coating layer. Therefore, under the same specific surface area and hydrothermal treatment temperature for the micro-nano porous inorganic materials, Comparative Examples 1 to 4 had a higher loss of active ingredient and a lower content of active ingredient, indicating that the active ingredient has poor temperature stability in the powder materials of Comparative Examples 1 to 4.

[0080] See Table 3. Figure 8 As can be seen from the results of Examples 13 to 16 and Comparative Examples 4 to 7, the specific surface area of ​​the micro-nano porous inorganic material is 980 m². 2At / g, the content of the active ingredient in Examples 13 to 16 increased with increasing hydrothermal treatment temperature, and this was also true after thermogravimetric analysis at 400°C, indicating that the temperature stability of the active ingredient in the core-shell structured materials of Examples 13 to 16 improved with increasing hydrothermal treatment temperature. On the other hand, the core-shell structured materials of Examples 13 to 16, by using a 980m... 2 The high specific surface area micro / nanoporous inorganic material, combined with hydrothermal treatment and the formation of an inorganic oxide coating, results in lower effective component loss in Examples 13 to 16, provided that the specific surface area of ​​the micro / nanoporous inorganic material and the hydrothermal treatment temperature are the same. Furthermore, from... Figure 8 The results clearly show that Examples 13 to 16 have a high content of active ingredients, indicating that the active ingredients have good temperature stability in the core-shell structure materials of Examples 13 to 16. In contrast, Comparative Examples 4 to 7 did not form an inorganic oxide coating layer. Therefore, under the same specific surface area and hydrothermal treatment temperature for the micro-nano porous inorganic materials, Comparative Examples 4 to 7 have a higher loss of active ingredients, and the content of active ingredients in the powder materials of Comparative Examples 4 to 7 is lower, indicating that the active ingredients are not coated in the powder materials of Comparative Examples 4 to 7 and are easily lost by heat.

[0081] In summary, this invention proposes a core-shell structure material and its preparation method that retains effective components, mainly by using a core-shell structure with a diameter of 120m. 2 / g to 980m 2 The invention involves a high specific surface area micro / nano porous inorganic material, which, through hydrothermal treatment, infuses the active ingredients into the pores of the micro / nano porous inorganic material, forming an inorganic oxide coating layer on the surface of the powder material. This allows the active ingredients to exist stably within the pores of the micro / nano porous inorganic material and be protected by the inorganic oxide coating layer, preventing them from volatilizing and dissipating at high temperatures, especially during high-temperature melt spinning processes. Furthermore, experimental verification shows that the core-shell structured material containing the active ingredients prepared by the method of this invention can also have its active ingredients protected by the inorganic oxide coating layer during high-temperature melt spinning processes, such as at temperatures above 260°C, thus facilitating the production of high-quality functional yarns. Therefore, the invention effectively achieves its objectives.

[0082] However, the above description is merely an embodiment of the present invention and should not be construed as limiting the scope of the present invention. Any simple equivalent changes and modifications made in accordance with the claims and description of the present invention shall still fall within the scope of the patent of the present invention.

Claims

1. A method for preparing a core-shell structured material that retains its effective components, characterized in that: The method for preparing the core-shell structured material that retains the effective components includes: (a) A mixture of an active ingredient, a micro / nano porous inorganic material, and distilled water is prepared, and the active ingredient is dissolved in the distilled water to obtain a raw material composition. The specific surface area of ​​the micro / nano porous inorganic material is in the range of 120 m². 2 / g to 980m 2 / g; (b) The raw material components are subjected to hydrothermal treatment so that the aqueous solution containing the effective component in the raw material components is injected into the pores of the micro-nano porous inorganic material to obtain a powder material containing the effective component; and (c) An inorganic oxide coating layer with micro- and nano-pores is formed on the surface of the powder material by sol-gel method to obtain a core-shell structure material containing the effective components.

2. The method for preparing a core-shell structured material retaining effective components according to claim 1, characterized in that: The active ingredient is selected from caffeine powder, lavender extract, artemisia extract, or any combination thereof. The caffeine powder is obtained by processing caffeine raw materials from which caffeine can be extracted, and the caffeine raw materials are selected from coffee grounds, tea leaves, or a combination thereof.

3. The method for preparing a core-shell structured material retaining effective components according to claim 1, characterized in that: The micro-nano porous inorganic material is selected from zeolite, halloysite, activated carbon, or a combination of the three.

4. The method for preparing a core-shell structured material retaining effective components according to claim 1, characterized in that: The particle size range of the micro-nano porous inorganic material is 0.1 μm to 1 μm.

5. The method for preparing a core-shell structured material retaining effective components according to claim 1, characterized in that: The hydrothermal treatment is performed at 100℃ to 160℃ and 1.0 kg / cm². 2 G up to 6.0 kg / cm 2 Performed under G pressure for 2 hours.

6. The method for preparing a core-shell structured material retaining effective components according to claim 1, characterized in that: Step (b) involves, after the hydrothermal treatment, injecting the aqueous solution containing the effective components into the pores of the micro-nano porous inorganic material to obtain a mixed liquid containing the powder material, centrifuging and filtering the mixed liquid to obtain a filter cake, and then drying the filter cake to obtain the powder material.

7. The method for preparing a core-shell structured material retaining effective components according to claim 1, characterized in that: The inorganic oxide coating layer is composed of silicon oxide or titanium oxide, and step (c) involves forming the inorganic oxide coating layer on the surface of the powder material using the sol-gel method, collecting the precipitate, and then washing, centrifuging, filtering, and drying the precipitate to obtain the core-shell structure material.

8. A core-shell structured material that retains effective components, characterized in that: The core-shell structure material that retains the effective components comprises: Powder materials include inorganic materials with micro-nano pores containing multiple micro-nano scale pores, and effective components present in the micro-nano scale pores; and An inorganic oxide coating layer is formed on the surface of the micro-nano porous inorganic material of the powder material; The powder material is prepared by first mixing the effective components, and has a specific surface area of ​​120m². 2 / g to 980m 2 / g of micro / nano porous inorganic material and distilled water, and the active ingredient is dissolved in the distilled water to obtain the raw material component. Then the raw material component is subjected to hydrothermal treatment so that the aqueous solution containing the active ingredient in the raw material component is injected into the pores of the micro / nano porous inorganic material to obtain the powder material containing the active ingredient. The inorganic oxide coating layer is formed on the surface of the micro / nano porous inorganic material by sol-gel method.

9. The core-shell structured material retaining effective components according to claim 8, characterized in that: The active ingredient is selected from caffeine powder, lavender extract, artemisia extract, or any combination thereof. The caffeine powder is obtained by processing caffeine raw materials that can extract caffeine, and the caffeine raw materials are selected from coffee grounds, tea leaves, or any combination thereof. The micro-nano porous inorganic material is selected from zeolite, halloysite, activated carbon, or any combination thereof.

10. The core-shell structured material retaining effective components according to claim 8, characterized in that: The particle size range of the micro-nano porous inorganic material is 0.1 μm to 1 μm.

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