Rose pearl-based chip for bacteriostasis, slow release and peculiar smell removal as well as preparation method and application of chip
The rose pearl antibacterial chip with a multi-layered composite structure solves the problems of insufficient durability, safety and synergy in antibacterial and deodorizing properties of existing personal care absorbent products, and achieves long-lasting, gentle, and multi-effect antibacterial and slow-release deodorizing effects.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-01-08
- Publication Date
- 2026-03-10
AI Technical Summary
Existing personal care absorbent products lack durability, safety, and synergy in terms of antibacterial and deodorizing effects. Chemical antibacterial agents may irritate the skin, physical adsorption materials are not effective in humid environments, natural active ingredients are prone to volatilization or loss, and functional release is greatly affected by the environment and cannot be intelligently regulated.
The rose pearl antibacterial chip, which adopts a multi-layer composite structure, includes an outer slow-release control layer, a middle functional layer, and an inner core layer. It utilizes modified pearl powder, rose essential oil microcapsules, and other natural ingredients. Through electrostatic stabilization, porous materials, and intelligent slow-release layers, it regulates the release of active ingredients to achieve long-lasting antibacterial and slow-release deodorization.
It significantly improves the stability and longevity of natural ingredients in humid environments, extends the antibacterial and deodorizing time, reduces the loss of functional ingredients, and maintains the product's gentleness and overall care effect.
Abstract
Description
Technical Field
[0001] This invention belongs to the field of personal care absorbent products technology, specifically relating to a chip based on rose pearl for antibacterial and slow-release deodorization, its preparation method and application. Background Technology
[0002] As consumers' demands for health and comfort continue to rise, the functional requirements for disposable hygiene products such as sanitary napkins and diapers have far exceeded the basic level of absorbency. The damp and warm environment in which these products are used easily breeds bacteria, producing unpleasant odors such as ammonia and hydrogen sulfide. This can not only cause skin discomfort, inflammation, and even infection, but also seriously affect the user's psychological well-being and quality of life. Therefore, many existing products on the market add various functional substances to the absorbent core or surface layer to seek improvements.
[0003] Currently, common technical approaches mainly focus on two directions: one is to add chemical or inorganic antibacterial agents, such as silver ions and quaternary ammonium compounds, to achieve antibacterial effects; the other is to add fragrances or physical adsorbent materials (such as activated carbon and zeolite) to the product to mask or absorb odors. However, these solutions all have significant limitations. While chemical antibacterial agents are effective, long-term contact may irritate sensitive skin or trigger allergic reactions, and their biocompatibility and safety are increasingly concerning. Traditional physical adsorption deodorization methods, such as using activated carbon particles, have limited adsorption capacity, and their adsorption capacity quickly becomes saturated or even decreases in humid environments, making them unable to continuously address the odor molecules generated during use. Essentially, they are a form of "transfer" rather than "elimination." Adding fragrances can only temporarily mask odors and cannot break down odor molecules at the source; furthermore, some users may experience discomfort or allergies to fragrances.
[0004] In recent years, applying natural active ingredients to personal care products has become an important research direction, aiming to provide gentler and safer solutions. For example, rose essential oil has been proven to have broad-spectrum antibacterial and mood-soothing properties, while pearl powder is recognized for its astringent, anti-inflammatory, and repair-promoting effects. However, directly applying these natural ingredients to hygroscopic products faces significant challenges. First, volatile components, such as rose essential oil, are highly volatile and easily oxidized and deactivated during product storage and use, resulting in a very short effective duration and making it difficult to provide stable protection throughout the entire product lifecycle. Second, natural powders (such as pearl powder) are prone to agglomeration and loss in humid environments, and their bioactive components are released slowly and uncontrollably, making it difficult to achieve rapid effects when needed.
[0005] Furthermore, in terms of material structure design, the existing product functional layers are relatively simple in construction, mostly consisting of a single coating or a mixed fiber layer. The release behavior of functional components is mostly passive diffusion, which is greatly affected by environmental humidity, and lacks an active control mechanism for the release rate and release sequence. This results in product performance that cannot intelligently adapt to complex and ever-changing usage scenarios, making it difficult to achieve both functional durability and high efficiency.
[0006] Therefore, there is an urgent need for a new type of composite material that can stably and long-lastingly load natural active ingredients, achieve chemical deodorization rather than masking, and intelligently regulate the release of functions, in order to solve the problems of insufficient durability, safety and synergy in the antibacterial, deodorizing and skin feel of existing moisture-absorbing products. Summary of the Invention
[0007] The purpose of this invention is to provide a chip based on rose and pearl for antibacterial and slow-release deodorization, as well as its preparation method and application. It constructs a functional chip with a multi-layer composite structure, which synergistically exerts the antibacterial and repairing effects of rose essential oil and pearl powder, introduces an odor chemical neutralizer, and utilizes an intelligent slow-release layer to regulate the release of active ingredients, thereby achieving long-lasting, gentle, and multi-effect antibacterial, deodorizing, and skin care functions.
[0008] To achieve the above objectives, the present invention provides the following technical solution:
[0009] The first aspect of the present invention provides a chip based on rose pearl antibacterial and slow-release deodorizing properties. The chip is a layered composite material, comprising, from top to bottom, an outer slow-release control layer, a middle functional layer, and an inner core layer.
[0010] The outer slow-release control layer is a composite membrane formed of chitosan and sodium alginate;
[0011] The intermediate functional layer is a skin-friendly non-woven fabric substrate, and its surface and / or interior are loaded with a functional composition containing modified pearl powder, ellagic tannin extract, sophora flavescens extract and citric acid.
[0012] The inner core layer consists of a porous carrier material and rose essential oil microcapsules loaded thereon.
[0013] Furthermore, the total thickness of the chip is 0.5-2 mm, wherein the thickness ratio of the inner core layer, the intermediate functional layer, and the outer sustained-release control layer is (0.3-0.6):(0.8-1.5):(0.01-0.05).
[0014] Furthermore, the skin-friendly nonwoven fabric substrate is a hot-air or spunlace nonwoven fabric made of ES fiber, viscose fiber, or a mixture of both.
[0015] Furthermore, the preparation method of the modified pearl powder is as follows:
[0016] (a) Sonicate the pearl powder with a 0.5-1.0 mol / L ammonia solution at 40-50℃ for 30-60 minutes, and wash until neutral to obtain activated pearl powder;
[0017] (b) Disperse the activated pearl powder in a mixed aqueous solution containing 0.8-1.5 mol / L citric acid and 0.1-0.3 mol / L phytic acid, and react at 55-65°C under an inert atmosphere for 3-8 hours;
[0018] (c) Adjust the pH of the reaction system in step (b) to 6.5-7.5, add hydroxypropyltrimethylammonium chloride chitosan, and continue the reaction at 40-50°C for 1-2 hours. After washing and drying the reaction product, the modified pearl powder is obtained.
[0019] This invention modifies pearl powder. Ammonia pretreatment loosens the layered structure of the pearl powder, increasing reactive sites. Then, a synergistic etching process using a citric acid-phytic acid mixture is employed. Citric acid constructs macroscopic pores, while phytic acid achieves directional exfoliation at the microscopic level, transforming the pearl powder into nanoscale powder with high specific surface area and hierarchical pores, significantly enhancing its adsorption and loading capacity. Finally, surface modification with chitosan quaternary ammonium salt not only prevents nanoparticle aggregation through electrostatic stabilization but also imparts a lasting positive charge and additional antibacterial activity to the powder, effectively enhancing its inhibitory ability against common pathogens through electrostatic interaction. Simultaneously, the introduced active groups on the surface strengthen the interfacial bonding with the fibrous substrate, enabling the functional components to function more stably and persistently.
[0020] Furthermore, the mass ratio of the modified pearl powder, ellagic tannin extract, sophora flavescens Ait. extract, and citric acid is 1:(0.2-0.5):(0.1-0.3):(0.1-0.3).
[0021] The functional composition, a blend of modified pearl powder, ellagitannin extract, sophora flavescens extract, and citric acid, forms a multi-target synergistic system. Modified pearl powder provides physical adsorption sites and an alkaline buffer environment; its positively charged surface can initially adsorb negatively charged bacteria. Ellagannin possesses strong complexing ability, effectively chelating odor molecules such as ammonia for chemical deodorization, while its antioxidant properties help stabilize other active ingredients in the system. The alkaloids in the sophora flavescens extract provide direct chemical antibacterial and anti-inflammatory effects, complementing the physical antibacterial mechanism of pearl powder. Citric acid, as an acid regulator, forms a local pH buffer pair with the alkaline microenvironment of pearl powder, enhancing the complexing efficiency of ellagitannin and the solubility of sophora flavescens alkaloids; simultaneously, it acts as a cross-linking agent, promoting the strong bonding of the functional components to the nonwoven fibers.
[0022] Furthermore, the porous carrier material is selected from one of porous starch microspheres, mesoporous silica, or activated carbon fiber.
[0023] Furthermore, the preparation method of the rose essential oil microcapsules is as follows:
[0024] (a) Rose essential oil was mixed with isopropyl myristate to obtain an oil phase; gelatin aqueous solution and a composite colloidal aqueous solution of gum arabic and sodium alginate were prepared separately.
[0025] (b) The oil phase is emulsified and dispersed in an aqueous gelatin solution to form a primary emulsion; an aqueous composite colloid solution is added to the primary emulsion to carry out a composite coagulation reaction;
[0026] (c) Add tannic acid to carry out a pre-crosslinking reaction, and cool down after the reaction is completed to allow the wall material to cure;
[0027] (d) Adjust the pH of the system to acidic and add citric acid to carry out the cross-linking and curing reaction;
[0028] (e) The cross-linked and cured microcapsule product is placed in a mineralization solution for treatment to obtain microcapsules;
[0029] (f) The microcapsules are washed and dried to obtain the rose essential oil microcapsules.
[0030] Further, in step (a), the mass ratio of the rose essential oil to isopropyl myristate is 4:1-6:1.
[0031] Further, in step (a), the concentration of the gelatin aqueous solution is 3-5 wt%; the total concentration of the composite colloidal aqueous solution of gum arabic and sodium alginate is 3-5 wt%, wherein the mass ratio of gum arabic to sodium alginate is 3:1-4:1; and the dry matter mass ratio of gelatin to the composite colloid is 1:0.8-1:1.2.
[0032] Further, in step (c), the amount of tannic acid added is 1%-3% of the total dry matter of the gelatin and the composite colloid.
[0033] Further, in step (c), the temperature of the pre-crosslinking reaction is 45-55℃ and the time is 20-40 minutes; the cooling rate is 0.5-1.0℃ / min, the cooling endpoint temperature is 10-15℃, and the wall material is cured at this temperature for 30-90 minutes.
[0034] Further, in step (d), the pH of the system is adjusted to acidity to pH 4.0-4.5; the amount of citric acid added is 2%-5% of the total dry matter of the gelatin and composite colloid; and the cross-linking curing reaction time is 1-3 hours.
[0035] Further, in step (e), the mineralization solution is a simulated body fluid containing calcium ions and phosphate ions, wherein the calcium ion concentration is 2.0-3.0 mmol / L, the phosphate ion concentration is 1.0-2.0 mmol / L, and the pH value is maintained at 7.2-7.6; the treatment conditions are: treatment at 35-37℃ for 2-6 hours.
[0036] This invention's method for preparing rose essential oil microcapsules effectively solves the core problems of rose essential oil's volatility and chemical instability. By using a composite coagulation method to form a wall material that encapsulates the oil, a high retention rate is ensured during storage and processing. The introduction of tannic acid for pre-crosslinking allows its polyphenolic structure to form hydrogen bonds and hydrophobic interactions with wall material components such as gelatin and sodium alginate, constructing a denser, mechanically stronger primary network before the main chemical crosslinking. This significantly enhances the structural integrity of the microcapsules and their barrier effect on the core material. Citric acid crosslinking further stabilizes this network. Biomimetic mineralization treatment forms a bone-like inorganic mineralization layer composed of calcium and phosphorus ions in situ on the microcapsule surface. This mineralization layer not only acts as an additional physical barrier, significantly slowing the outward diffusion of the essential oil, but its dissolution behavior is also pH-responsive, allowing for controlled degradation in the slightly acidic and humid environment of actual use, thus achieving intelligent regulation of the release rate.
[0037] The second aspect of this invention provides a method for preparing the above-mentioned chip based on rose pearl antibacterial and slow-release deodorizing properties, comprising the following steps:
[0038] (1) Modified pearl powder, ellagic tannin extract, sophora flavescens extract and citric acid are dispersed in deionized water in proportion to prepare a functional finishing liquid; the functional finishing liquid is applied to a skin-friendly non-woven fabric substrate by padding or spraying process, and after drying and heat treatment, an intermediate functional layer loaded with functional composition is obtained.
[0039] (2) Rose essential oil microcapsules and porous carrier materials are mixed in an adhesive, and then molded and dried to obtain a core sheet;
[0040] (3) The core layer sheet and the intermediate functional layer are bonded together by hot melt adhesive or hydroentangling process, and an outer slow-release control layer is formed on the surface of the intermediate functional layer to obtain the chip.
[0041] Furthermore, the formation process of the outer sustained-release control layer includes: coating the surface of the intermediate functional layer with a chitosan acetate solution, drying it, immersing it in a sodium alginate solution, removing it, treating it with a crosslinking solution containing aluminum trichloride, and drying it to form the outer sustained-release control layer.
[0042] The third aspect of this invention provides the application of the above-mentioned antibacterial and slow-release deodorizing chip based on rose pearl in sanitary napkins, panty liners, diapers, adult incontinence products, or medical care pads.
[0043] Compared with the prior art, the advantages and beneficial effects of the present invention are as follows:
[0044] The chip provided by this invention achieves orderly release and synergistic effects through a three-layer composite structure. The microcapsules in the inner core layer ensure the timely onset and long-lasting effect of rose essential oil. The modified pearl powder in the middle functional layer, combined with ingredients such as sophora flavescens and ellagic tannins, provides continuous antibacterial, repairing, and chemical deodorizing capabilities. The outer slow-release membrane effectively regulates the release rate of active substances. This design significantly improves the stability and durability of natural ingredients in actual use environments. Its application in hygroscopic products can effectively prolong antibacterial and deodorizing time and reduce the loss of functional ingredients, thereby enhancing the overall care effect while maintaining the product's gentleness. Detailed Implementation
[0045] The technical solutions in the embodiments of the present invention will be clearly and completely described below. 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 skilled in the art without creative effort are within the scope of protection of the present invention.
[0046] Unless otherwise specified, all raw materials used in the embodiments are commercially available products. The following sources are illustrative examples.
[0047] Pearl powder was purchased from Zhejiang Changsheng Bird Pharmaceutical Co., Ltd., pharmaceutical grade pearl powder, model ZSF-1000, particle size approximately 1000 mesh. Ellagantin extract was purchased from Xi'an Tianyi Biotechnology Co., Ltd., model TY-SQP, ellagicin content ≥50%, plant source: pomegranate (Punica granatum L.) pericarp. Sophora flavescens extract was purchased from Nanjing Zelang Pharmaceutical Technology Co., Ltd., model ZL-KS. Porous starch microspheres were purchased from Shandong Longli Biotechnology Co., Ltd., model LLPS-80. Mesoporous silica was purchased from Anhui Meixiang New Material Technology Co., Ltd., model MX-SiO2-M41. Hydroxypropyltrimethylammonium chloride chitosan was purchased from Zhejiang Jinke Pharmaceutical Co., Ltd., model JK-HA, degree of substitution ≥90%.
[0048] Example 1
[0049] This embodiment provides a chip based on rose pearl for antibacterial and slow-release odor removal, the preparation method of which includes the following steps:
[0050] (1) Preparation of the intermediate functional layer: Weigh 10g of modified pearl powder, 3.5g of ellagic tannin extract, 2.0g of sophora flavescens extract, and 2.0g of citric acid, and disperse them together in 182.5g of deionized water, stirring to prepare a uniform functional finishing solution. One sheet weighing 40 g / m²... 2 The ES hot air nonwoven fabric is treated with a two-dip, two-ply process with a 100% padding rate to ensure full penetration of the finishing solution. It is then dried at 100°C for 5 minutes and then baked at 130°C for 2 minutes to obtain an intermediate functional layer loaded with the functional composition.
[0051] (2) Preparation of the inner core layer: Weigh 15g of rose essential oil microcapsules and mix with 35g of porous starch microspheres. Add 50g of 10% polyvinyl alcohol 1799 aqueous solution as a binder. After stirring evenly, spread it on a polytetrafluoroethylene plate, control the wet thickness to about 2mm, and dry it in a 60℃ oven to constant weight to obtain the core layer sheet.
[0052] (3) Composite and coating: The core layer sheet and the intermediate functional layer obtained in step (1) are composited with hot melt adhesive, and the hot melt adhesive coating amount is 5 g / m 2 The composite temperature was 110℃ and the pressure was 0.3 MPa. Subsequently, a 3% (w / w) chitosan-acetic acid solution (1% acetic acid) was coated onto the surface of the intermediate functional layer of the composite material, resulting in a wet film thickness of approximately 100 μm. This film was then dried at 55℃ for 30 minutes to form a preliminary film. Next, the material was immersed in a 2% (w / w) sodium alginate aqueous solution for 2 minutes. After removing and draining excess solution, it was then immersed in a 3% (w / w) aluminum trichloride aqueous solution for crosslinking treatment for 2 minutes. Finally, the material was removed, gently rinsed with deionized water, and dried at 50℃ to obtain a complete chip. The total thickness of the obtained chip was approximately 1.2 mm, with the inner core layer, intermediate functional layer, and outer sustained-release control layer having thicknesses of approximately 0.4 mm, 0.8 mm, and 0.03 mm, respectively.
[0053] The preparation method of modified pearl powder is as follows:
[0054] (a) Weigh 100g of pearl powder (pharmaceutical grade, 1000 mesh), add it to 2L of 0.8 mol / L ammonia solution, and sonicate at 45℃ for 40 minutes. Then centrifuge and wash with deionized water until neutral to obtain activated pearl powder.
[0055] (b) Disperse activated pearl powder in a mixed aqueous solution (total volume 3L) containing 1.0 mol / L citric acid and 0.2 mol / L phytic acid, and stir continuously for 5 hours at 60°C under nitrogen atmosphere protection.
[0056] (c) After the reaction was completed, the pH of the system was adjusted to 7.0 with dilute sodium hydroxide solution, and 15g of hydroxypropyltrimethylammonium chloride chitosan (HTCC, degree of substitution ≥90%) was added. The reaction was continued at 45℃ for 1.5 hours. Finally, the product was centrifuged, washed three times with deionized water, and freeze-dried at -50℃ for 24 hours to obtain modified pearl powder.
[0057] The preparation method of rose essential oil microcapsules is as follows:
[0058] (a) Weigh 60g of rose essential oil and 12g of isopropyl myristate, and mix them evenly as the oil phase. Prepare 500g of a 4 wt% gelatin aqueous solution as aqueous phase A; and 500g of a 4 wt% aqueous solution of a complex colloid of gum arabic and sodium alginate as aqueous phase B, wherein the mass ratio of gum arabic to sodium alginate is 4:1; and the dry matter mass ratio of gelatin to the complex colloid in the system is 1:1.
[0059] (b) The oil phase was emulsified and dispersed in aqueous phase A at 50°C under high-speed shear to form a primary emulsion. Aqueous phase B was added to the primary emulsion under stirring, and a complex coagulation reaction was carried out at 50°C for 30 minutes.
[0060] (c) Add 0.8 g of tannic acid to the reaction system and carry out a pre-crosslinking reaction at 50 °C for 30 minutes. Then, cool the reaction system to 12 °C at a rate of 0.7 °C / min and keep stirring at 12 °C for 60 minutes to cure the wall material.
[0061] (d) Adjust the pH of the system to 4.3 with 1 mol / L dilute hydrochloric acid, add 1.2 g citric acid, and carry out the cross-linking curing reaction at 15 °C for 2 hours.
[0062] (e) The microcapsule product obtained after cross-linking and curing is collected by centrifugation and treated in a mineralization solution at 37°C for 4 hours. The mineralization solution contains 2.5 mmol / L calcium ions and 1.0 mmol / L phosphate ions, and the pH value is 7.4.
[0063] (f) The mineralized microcapsules were centrifuged, washed three times with deionized water, and finally spray-dried to obtain dried rose essential oil microcapsule powder.
[0064] Example 2
[0065] This embodiment provides a chip based on rose pearl for antibacterial and slow-release odor removal, the preparation method of which includes the following steps:
[0066] (1) Preparation of the intermediate functional layer: Weigh 12g of modified pearl powder, 4.8g of ellagic tannin extract, 3.0g of sophora flavescens extract and 1.8g of citric acid, disperse them together in 200g of deionized water, and stir to prepare a functional finishing solution. One tablet with a weight of 45 g / m 2 The viscose spunlace nonwoven fabric is uniformly coated with finishing liquid using a spraying process, then dried at 90°C for 8 minutes, and then baked at 125°C for 2.5 minutes to obtain an intermediate functional layer loaded with functional composition.
[0067] (2) Preparation of the inner core layer: Weigh 20g of rose essential oil microcapsules and mix with 30g of mesoporous silica. Add 40g of 15% polyurethane aqueous dispersion as a binder. After stirring evenly, roll press the mixture to a wet thickness of about 1.8mm. Dry it in an oven at 65℃ to constant weight to obtain the core layer sheet.
[0068] (3) Composite and Coating: The core layer sheet and the intermediate functional layer obtained in step (1) are composited using a hydroentangling process. Subsequently, a 2.5% (w / w) chitosan acetate solution (0.8% acetic acid concentration) is coated onto the surface of the intermediate functional layer of the composite material, with a wet film thickness of approximately 80 μm, and dried at 60°C for 20 minutes. Next, the material is immersed in a 1.5% (w / w) sodium alginate aqueous solution for 3 minutes, drained, and then immersed in a 4% (w / w) aluminum trichloride aqueous solution for crosslinking treatment for 1 minute. Finally, it is removed, rinsed, and dried to obtain the chip. The total thickness of the obtained chip is approximately 1.5 mm, of which the thicknesses of the inner core layer, intermediate functional layer, and outer slow-release control layer are approximately 0.5 mm, 1.0 mm, and 0.025 mm, respectively.
[0069] The preparation method of modified pearl powder is as follows:
[0070] (a) Weigh 100g of pearl powder and add it to 2L of 0.6 mol / L ammonia solution. Sonicate the solution at 48℃ for 50 minutes. Wash until neutral to obtain activated pearl powder.
[0071] (b) Disperse activated pearl powder in a mixed aqueous solution (total volume 3.5L) containing 0.9 mol / L citric acid and 0.15 mol / L phytic acid, and stir the mixture at 58°C under nitrogen protection for 6 hours.
[0072] (c) After the reaction was complete, the pH was adjusted to 6.8, and 12g of hydroxypropyltrimethylammonium chloride chitosan was added. The reaction was continued at 48°C for 1.2 hours. The product was washed and then spray-dried to obtain modified pearl powder.
[0073] The preparation method of rose essential oil microcapsules is as follows:
[0074] (a) Weigh 64g of rose essential oil and 16g of isopropyl myristate, and mix them evenly as the oil phase. Prepare the following aqueous phases separately: 600g of a 3.5wt% gelatin aqueous solution as aqueous phase A; and 400g of a 4.5wt% aqueous solution of a complex colloid of gum arabic and sodium alginate as aqueous phase B, wherein the mass ratio of gum arabic to sodium alginate is 3:1; and the dry matter mass ratio of gelatin to the complex colloid in the system is 1:1.1.
[0075] (b) The oil phase was emulsified and dispersed in aqueous phase A at 48°C under high-speed shear to form a primary emulsion. Aqueous phase B was added to the primary emulsion under stirring, and a complex coagulation reaction was carried out at 52°C for 35 minutes.
[0076] (c) Add 0.78 g of tannic acid to the reaction system and carry out a pre-crosslinking reaction at 48 °C for 35 minutes. Then, cool the reaction system to 14 °C at a rate of 0.6 °C / min and keep stirring at 14 °C for 50 minutes to cure the wall material.
[0077] (d) Adjust the pH of the system to 4.1 with 1 mol / L dilute hydrochloric acid, add 1.56 g of citric acid, and carry out the cross-linking curing reaction at 18 °C for 1.5 hours.
[0078] (e) The microcapsule product obtained after cross-linking and curing was collected by centrifugation and treated in a mineralization solution at 36°C for 5 hours. The mineralization solution contained 2.2 mmol / L calcium ions and 1.5 mmol / L phosphate ions, with a pH of 7.3.
[0079] (f) The mineralized microcapsules were centrifuged, washed three times with deionized water, and finally freeze-dried to obtain dried rose essential oil microcapsule powder.
[0080] Comparative Example 1
[0081] The difference between this comparative example and Example 1 is that, in the preparation of the intermediate functional layer, the modified pearl powder was replaced with untreated pearl powder from the same batch as a component of the functional composition.
[0082] Comparative Example 2
[0083] The difference between this comparative example and Example 1 is that in the preparation method of modified pearl powder, step (b) replaces "a mixed aqueous solution containing 1.0 mol / L citric acid and 0.2 mol / L phytic acid" with "an aqueous solution containing 1.2 mol / L citric acid".
[0084] Comparative Example 3
[0085] The difference between this comparative example and Example 1 is that the preparation method of the rose essential oil microcapsules is as follows:
[0086] (a) Mix 60g of rose essential oil with 15g of isopropyl myristate as the oil phase.
[0087] (b) Prepare 500g of a 3% gelatin aqueous solution as aqueous phase A. Separately prepare 500g of a composite colloidal aqueous solution containing 2.25% gum arabic and 0.75% sodium alginate as aqueous phase B.
[0088] (c) Under high-speed shear, the oil phase is added to the aqueous phase A at 50°C and emulsified for 5 minutes to form a primary emulsion. Under stirring, the aqueous phase B is slowly added dropwise to the primary emulsion. After the addition is complete, stirring is continued at 52°C for 30 minutes to carry out composite coagulation.
[0089] (d) The system was cooled to 12°C at a rate of 0.8°C / min and stirred at this temperature for 1 hour.
[0090] (e) Adjust the pH of the system to 4.3 with 1 mol / L hydrochloric acid, add 3 g of citric acid, and perform a cross-linking reaction at 15 °C for 1.5 hours. After the reaction is complete, collect the microcapsules by centrifugation, wash with deionized water, and spray dry to obtain dried rose essential oil microcapsule powder.
[0091] Comparative Example 4
[0092] The difference between this comparative example and Example 1 is that the calcium ion concentration of the mineralization solution in step (e) of the method for preparing rose essential oil microcapsules is 1.2 mmol / L, the phosphate ion concentration is 2.8 mmol / L, and the pH value is maintained at 6.8.
[0093] Comparative Example 5
[0094] The difference between this comparative example and Example 1 is that step (1) of preparing the functional finishing liquid is replaced by: weighing 11.5g of modified pearl powder, 4.0g of sophora flavescens extract and 2.0g of citric acid, dispersing them together in 182.5g of deionized water, and stirring to prepare a uniform functional finishing liquid.
[0095] Comparative Example 6
[0096] The difference between this comparative example and Example 1 is that, in the preparation of the functional finishing solution for the intermediate functional layer, Sophora flavescens extract was replaced with an equal mass of Phellodendron chinense extract.
[0097] Performance testing
[0098] To verify the performance of the chip described in this invention, performance tests were conducted on samples from Examples 1 and 2 and Comparative Examples 1-6.
[0099] The testing method is as follows:
[0100] 1. Long-lasting antibacterial performance: Referring to GB / T 20944.3-2008, the antibacterial rate of the samples against Escherichia coli (ATCC25922) and Staphylococcus aureus (ATCC 6538) was tested after 2 hours and 6 hours of action to evaluate the speed and duration of its antibacterial effect.
[0101] 2. Ammonia neutralization efficiency: A fixed amount of ammonia (initial concentration of about 50 ppm) was injected into a sealed test chamber, and a sample of equal area was placed inside. The rate of decrease in ammonia concentration in the chamber was measured after 30 minutes and 120 minutes to evaluate its source chemical deodorization ability.
[0102] 3. Slow-release behavior of rose essential oil: Using headspace gas chromatography, under accelerated release conditions of 40℃ and 90% relative humidity, the cumulative release of citronellol, a characteristic component of rose essential oil, was determined at 0.5 hours, 2 hours, and 8 hours. The result was expressed as a percentage (%) relative to the initial essential oil load in the microcapsules to characterize its slow-release properties.
[0103] 4. Retention rate of functional components after multiple absorptions: The sample was repeatedly absorbed and drained 5 times in a simulated solution (9.0 g / L sodium chloride, 1.0 g / L urea, pH adjusted to 8.0 with phosphate buffer). The retention rate of modified pearl powder and ellagitannins per unit area was measured to evaluate the firmness of the functional layer in a humid environment.
[0104] The test results are shown in Table 1.
[0105] Table 1 Performance Test Results
[0106] Test item Example 1 Example 2 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Comparative Example 6 Bacteriostatic rate (E. coli, 2h, %) 99.2 98.8 88.5 95.1 98.5 98.2 98.9 97.5 Bacteriostatic rate (E. coli, 6h, %) 98.5 97.8 65.2 85.4 92.1 93.5 96 94.3 Bacteriostatic rate (S. aureus, 2h, %) 99.5 99 85.3 93.8 99 98.8 99.2 98.1 Bacteriostatic rate (S. aureus, 6h, %) 99.1 98.5 60.8 82.7 90.5 92.0 97.2 89.7 Ammonia neutralization rate (30min, %) 85 83.5 60.2 80.5 83 82.0 55.1 81.8 Ammonia neutralization rate (120min, %) 94.7 93.2 71.5 90.1 92.8 89.5 68.3 92.5 Cumulative release of essential oil (2h, %) 38.5 36.2 65.8 42 70.5 45.1 39 37.8 Cumulative release of essential oil (8h, %) 82.4 80.1 95.8 85 96.5 88.7 83 81.9 Retention rate of functional ingredient (after 5 times, %) 88.5 86.2 45.3 75.6 87 84.9 85.1 87.8
[0107] The performance test results above show that Examples 1-2 all exhibit excellent overall performance. The antibacterial properties are rapid and long-lasting, demonstrating the synergistic and long-lasting effects of the active ingredients. The ammonia neutralization capacity significantly increases over time, confirming its highly efficient chemical deodorizing properties. The essential oil release exhibits good sustained-release behavior, indicating that the release process is effectively controlled. The functional components maintain a high retention rate even after multiple absorptions, proving the robustness of the loading process.
[0108] Comparative Example 1 showed acceptable antibacterial rate after 2 hours, but a sharp decline after 6 hours, indicating a lack of persistence; the retention rate of functional components was extremely low, indicating that the unmodified powder was poorly bound and easily lost. Comparative Example 2 showed improved performance compared to Comparative Example 1, but the antibacterial rate and component retention rate after 6 hours were still significantly lower than the example, proving that the modification effect of the changed process was incomplete and failed to build a durable and stable synergistic system. Comparative Example 3 showed an antibacterial rate comparable to the example after 2 hours, but a significant decline after 6 hours, and the essential oil was released too quickly, resulting in the near failure of the sustained-release function and the inability to achieve long-lasting effects. Comparative Example 4 showed a certain decline in the sustained-release rate of essential oil and the long-lasting antibacterial rate, indicating that when the calcium and phosphorus ion concentrations and pH value of the mineralization solution deviated from the preferred range defined in this invention, a dense and effective mineralization layer could not be formed, resulting in a weakened structural reinforcement and release regulation effect. Comparative Example 5 showed a relatively small impact on the antibacterial rate, but the ammonia neutralization rate was at an extremely low level at both 30 minutes and 120 minutes, indicating a severe lack of chemical deodorization ability, directly proving the core role of ellagitannins in this function. Comparative Example 6 showed good initial antibacterial activity, but the long-term antibacterial rate against Staphylococcus aureus decreased significantly, indicating that Sophora flavescens extract has an irreplaceable synergistic effect in the compound system of this invention and can provide more durable antibacterial protection.
[0109] The above description represents the preferred embodiments of the present invention. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principles of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.
Claims
1. A rose petal based chip for inhibiting bacteria and releasing odor, characterized in that, The chip is a layered composite material, which comprises from top to bottom an outer slow-release control layer, an intermediate functional layer and an inner core layer; The outer slow-release control layer is a composite film formed by chitosan and sodium alginate; The intermediate functional layer is a skin-friendly non-woven fabric substrate, the surface and / or interior of which is loaded with a functional composition comprising modified pearl powder, tannin extract, sophora flavescens extract and citric acid; The inner core layer is composed of a porous carrier material and rose essential oil microcapsules loaded thereon.
2. The chip according to claim 1, characterized in that, The total thickness of the chip is 0.5-2 mm, and the thickness ratio of the inner core layer, the intermediate functional layer and the outer slow-release control layer is (0.3-0.6):(0.8-1.5):(0.01-0.05).
3. The chip of claim 1, wherein, The skin-friendly non-woven fabric substrate is a hot air or water jet non-woven fabric made of ES fiber, viscose fiber or a mixture of both.
4. The chip of claim 1, wherein The preparation method of the modified pearl powder is as follows: (a) ultrasonic treatment of pearl powder with an ammonia solution to obtain activated pearl powder; (b) dispersing the activated pearl powder in a mixed aqueous solution containing citric acid and phytic acid, and reacting for 3-8 hours; (c) adjusting the pH of the reaction system of step (b) to 6.5-7.5, adding hydroxypropyltrimethylammonium chloride chitosan, and continuing to react, and then washing and drying the reaction product to obtain the modified pearl powder.
5. The chip of claim 1, wherein The mass ratio of the modified pearl powder, tannin extract, sophora flavescens extract and citric acid is 1:(0.2-0.5):(0.1-0.3):(0.1-0.3).
6. The chip of claim 1, wherein The preparation method of the rose essential oil microcapsules is as follows: (a) mixing rose essential oil with isopropyl myristate to obtain an oil phase; preparing a gelatin aqueous solution and a composite colloidal aqueous solution of gum arabic and sodium alginate, respectively; (b) emulsifying and dispersing the oil phase in the gelatin aqueous solution to form a primary emulsion; adding the composite colloidal aqueous solution to the primary emulsion to perform a complex coagulation reaction; (c) adding tannic acid to perform a pre-crosslinking reaction, and then cooling to solidify the wall material after the reaction is completed; (d) adjusting the pH of the system to be acidic, and adding citric acid to perform a crosslinking and solidification reaction; (e) placing the crosslinked and solidified microcapsule product in a mineralization solution to obtain microcapsules; (f) washing and drying the microcapsules to obtain the rose essential oil microcapsules.
7. The chip of claim 6, wherein In step (a), the mass ratio of the rose essential oil to isopropyl myristate is 4:1-6:1; in step (c), the amount of tannic acid added is 1%-3% of the total mass of dry substances of the gelatin and the composite colloid; in step (d), the amount of citric acid added is 2%-5% of the total mass of dry substances of the gelatin and the composite colloid; in step (e), the mineralization solution is a simulated body fluid containing calcium ions and phosphate ions, wherein the concentration of calcium ions is 2.0-3.0 mmol / L, the concentration of phosphate ions is 1.0-2.0 mmol / L, and the pH value is maintained at 7.2-7.
6.
8. A preparation method of a rose pearl-based chip for inhibiting bacteria and slowly releasing odor according to any one of claims 1-7, comprising the following steps: (1) dispersing modified pearl powder, tannin extract, sophora flavescens extract and citric acid in deionized water according to the proportion to prepare a functional finishing liquid; applying the functional finishing liquid to a skin-friendly non-woven fabric substrate by padding or spraying process, drying and heat treating to obtain an intermediate functional layer loaded with a functional composition; (2) mixing rose essential oil microcapsules and porous carrier material in a binder, shaping and drying to obtain a core layer sheet; (3) compounding the core layer sheet and the intermediate functional layer by hot melt adhesive bonding or water jet process, and forming an outer slow-release control layer on the surface of the intermediate functional layer to obtain the chip.
9. The production method according to claim 8, characterized by, The formation process of the outer slow-release control layer includes: coating the surface of the intermediate functional layer with a chitosan acetic acid solution, drying, immersing in a sodium alginate solution, taking out and treating with a cross-linking solution containing aluminum chloride, and drying to form the outer slow-release control layer.
10. Use of the rose pearl bacteriostatic and odor-removing slow-release chip according to any one of claims 1-7 in sanitary napkins, panty liners, paper diapers, adult incontinence products or medical care pads.