Silica gel foam containing agilawood, preparation method of silica gel foam and application of silica gel foam in pillow inner

By using porous carrier encapsulation technology of agarwood extract and modified cyclodextrin-chitosan complex, combined with activated azodicarbonamide foaming, the problem of insufficient health benefits of silicone foam is solved, achieving stable release of agarwood components and antibacterial effect, providing soft support and long lifespan silicone foam.

CN121873552APending Publication Date: 2026-04-17HUIZHOU XINYA KAILI TECH CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
HUIZHOU XINYA KAILI TECH CO LTD
Filing Date
2025-12-31
Publication Date
2026-04-17

AI Technical Summary

Technical Problem

Traditional silicone foam lacks health benefits. When agarwood is combined with silicone, the dispersion is poor, resulting in uneven release of active ingredients, which affects the product's functional stability and lifespan.

Method used

The agarwood functional component is composed of agarwood extract and modified cyclodextrin-chitosan complex, which encapsulates agarwood molecules through a porous three-dimensional network carrier, and combines activated azodicarbonamide and sodium bicarbonate for foaming to form a uniform and dense foam structure.

Benefits of technology

It achieves stable release of agarwood components and antibacterial effects, enhances its calming and sleep-aiding functions, ensures continuous fragrance release, provides a soft touch and good support, and extends service life.

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Abstract

The invention relates to the technical field of organic silicon materials, and particularly discloses agilawood-containing silica gel foam, a preparation method of the agilawood-containing silica gel foam and application of the agilawood-containing silica gel foam in a pillow inner. Comprising the following raw materials in parts by weight: 100 parts of organosiloxane, 5-8 parts of an agilawood functional component, 0.05-0.1 part of a catalyst, 4-7 parts of a cross-linking agent, 2-3 parts of a dispersing agent, 15-25 parts of a reinforcing agent, 3-6 parts of a foaming agent and 0.5-1.5 parts of an auxiliary agent, according to the preparation method, agilawood micromolecules are effectively prevented from being quickly volatilized and lost at the initial stage of processing and using, it is ensured that fragrance can be continuously and stably emitted, the functions of soothing the nerves and helping sleep are improved, and the prepared silica gel foam provides moderate hardness and high rebound resilience, is soft but not prone to collapse, provides lasting comfort, is long in service life, and is suitable for popularization and application. The method has a wide application prospect in the fields of smart home, health care and the like.
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Description

Technical Field

[0001] This invention relates to the field of organosilicon materials technology, specifically to a silicone foam containing agarwood, its preparation method, and its application in pillow cores. Background Technology

[0002] Silicone foam is a silicone rubber material with a three-dimensional interpenetrating network structure. It has excellent compression resilience, softness, breathability, and weather resistance, and is widely used in furniture, bedding, and medical fields. In bedding applications, especially pillow cores, silicone foam not only provides support that conforms to the curves of the human head and neck, but also does not easily breed bacteria, has a long service life, and brings a comfortable sleep experience.

[0003] However, with the improvement of living standards, consumers' functional needs for bedding are no longer limited to basic comfort, but are upgrading towards health, wellness, and therapeutic benefits. Traditional silicone foam has limited functionality and lacks health benefits, failing to meet people's growing demand for a healthy lifestyle.

[0004] Agarwood is a traditional Chinese medicine with effects such as promoting qi circulation and relieving pain, warming the stomach and stopping vomiting, and calming asthma. Its aromatic components have the effects of calming the nerves, aiding sleep, and relieving stress. Combining agarwood with silicone foam to develop pillow cores that combine comfort and health benefits has significant practical value. Chinese patent application CN115340765A discloses a novel agarwood silicone product composition, the composition, and a method for preparing the silicone product. This composition consists of solid silicone rubber compound or liquid silicone A and liquid silicone B, as well as a platinum catalyst, agarwood powder, sandalwood powder, clove powder, and costus root powder, and has a rich fragrance and is healthy and environmentally friendly. However, this composition only directly mixes agarwood powder and other ingredients with silicone, resulting in poor dispersibility, insufficient compatibility with silicone, uneven release of effective ingredients, and affecting the stability of product function. Chinese patent CN113861501A discloses a silicone cotton pillow and its preparation method. The method involves reacting a polyether mixture and isocyanate to obtain a preliminary polyurethane mixture, which is then placed in a sealed space and intermittently circulated with cold air to continue the reaction, resulting in a shaped polyurethane sponge block. This block is then cut to obtain a cotton pillow of the desired shape. The cotton pillow is then soaked in silicone, roller-pressed, and dried to obtain the silicone cotton pillow. However, this silicone cotton only forms a coating on the surface, which easily leads to uneven mechanical properties. With long-term use, the surface silicone is prone to peeling and cracking, affecting its service life.

[0005] Therefore, developing a comfortable silicone foam material with excellent stability and long-lasting calming and health-promoting functions has significant practical value. Summary of the Invention

[0006] (a) Technical problems to be solved To address the shortcomings of existing technologies, this invention provides a silicone foam containing agarwood, its preparation method, and its application in pillow cores, thus solving the problem of traditional silicone foam lacking health benefits.

[0007] (II) Technical Solution To achieve the above objectives, the present invention discloses a silicone foam containing agarwood, comprising the following raw materials by weight: 100 parts of organosiloxane; 5-8 parts of agarwood functional components; Catalyst 0.05-0.1 parts; 4-7 parts of crosslinking agent; 2-3 parts dispersant; 15-25 parts of reinforcing agent; 3-6 parts of foaming agent; 0.5-1.5 parts of auxiliary agent; The organosiloxane is composed of vinyl-terminated polydimethylsiloxane and divinyltetramethyldisiloxane in a mass ratio of 88-90:10-12. The agarwood functional components are obtained by combining agarwood extract with a modified cyclodextrin-chitosan complex.

[0008] As a further aspect of the present invention: the agarwood functional components are prepared by the following method: S1. Mix nano-silica, ethanol solution, and propyltriethoxysilane isocyanate, heat to 65-75℃ and stir for 4-6 hours, add acetic acid solution to adjust pH to 4-5, mix evenly, then add chitosan, stir at 60-70℃ for 24-36 hours, centrifuge, wash with deionized water and anhydrous ethanol, freeze dry to obtain chitosan@SiO2; S2. After mixing isopropanol, β-cyclodextrin and dimethyl sulfoxide evenly, epichlorohydrin is added, the pH is adjusted to 9-10 with sodium hydroxide solution, and the mixture is stirred for 4-6 hours. Chitosan@SiO2 is then added and stirred to mix and react. After the reaction is complete, the mixture is filtered, washed with deionized water, and freeze-dried to obtain the modified cyclodextrin-chitosan complex. S3. Mix acetic acid solution, modified cyclodextrin-chitosan complex and agarwood extract, stir at room temperature for 6-8 hours, let stand at 0-5℃ for 24 hours, adjust pH to neutral with sodium hydroxide solution, filter, wash with deionized water, freeze dry to obtain agarwood functional components.

[0009] As a further aspect of the present invention: the mass ratio of nano-silica, ethanol solution, propyltriethoxysilane isocyanate, and chitosan in S1 is 100:3500-5000:5-20:105-200.

[0010] As a further aspect of the present invention: the ethanol solution in S1 is a 75wt% aqueous ethanol solution.

[0011] As a further aspect of the present invention: the acetic acid solution in S1 is an aqueous solution of acetic acid with a mass fraction of 1%.

[0012] As a further embodiment of the present invention: the mass ratio of isopropanol, β-cyclodextrin, dimethyl sulfoxide, epichlorohydrin, and chitosan@SiO2 in S2 is 600-900:100:35-52:21-32:110-130, the reaction temperature is 55-65℃, and the reaction time is 4-6h.

[0013] As a further aspect of the present invention: the acetic acid solution in S3 is a 1wt% acetic acid solution.

[0014] As a further aspect of the present invention: the preparation method of the agarwood extract in S3 includes the following steps: grinding the agarwood medicinal material into powder, passing it through a 40-mesh sieve, and using supercritical CO2 extraction method, with an extraction time of 2 hours, an extraction temperature of 40°C, and an extraction pressure of 18 MPa to obtain the agarwood extract.

[0015] As a further aspect of the present invention: the mass ratio of acetic acid solution, modified cyclodextrin-chitosan complex, and agarwood extract in S3 is 1400-1600:100:10-15.

[0016] As a further aspect of the present invention: the catalyst is a platinum catalyst; the crosslinking agent is methyl-terminated hydrogen-containing silicone oil; the dispersant is γ-methacryloyloxypropyltrimethoxysilane; the foaming agent is composed of activated azodicarbonamide and sodium bicarbonate in a mass ratio of 1:1; and the auxiliary agent is antioxidant 1076.

[0017] As a further aspect of the present invention: the activated azodicarbonamide contains 10wt% zinc oxide as an activator.

[0018] As a further aspect of the present invention: the reinforcing agent is hydrophobically modified fumed silica nanoparticles, and the specific preparation method includes the following steps: anhydrous ethanol, methyl silicate, cetyltrimethylammonium bromide surfactant, and polyvinylpyrrolidone are stirred and mixed, and then 25% ammonia and hexamethyldisilazane are added, wherein the mass ratio of anhydrous ethanol, methyl silicate, cetyltrimethylammonium bromide, polyvinylpyrrolidone, 25% ammonia and hexamethyldisilazane is 350-500:100:5-10:2-3:35-50:18-30, stirred and mixed, and reacted at 25-35℃ for 4-5 hours. After the reaction is completed, it is allowed to stand and age for 24 hours. After aging, it is dispersed using a high-speed shear disperser to obtain hydrophobically modified fumed silica nanoparticles.

[0019] A method for preparing the agarwood-containing silicone foam includes the following steps: Step 1: Add organosiloxane to a mixer and mix at a temperature of 80-90℃, a speed of 30-40r / min, and a time of 10-15min. Then add reinforcing agent and dispersant and mix at 80-90℃ and 40-50r / min for 20-30min. Then add agarwood functional components and mix at 60-70℃ and 30-40r / min for 15-20min to obtain functional base adhesive. Step 2: Transfer the functional base rubber to a two-roll mill, add the additives and crosslinking agent, mix for 8-10 minutes, then add the catalyst and foaming agent, mix for 5-8 minutes to obtain a uniform rubber compound. Step 3: Place the adhesive material into a mold preheated to 100℃, heat and pressurize, release the pressure, open the mold, take it out, and let it cool naturally to room temperature to obtain silicone foam containing agarwood.

[0020] As a further aspect of the present invention: the temperature for heating and pressurizing in step three is 160-170℃, the pressure for heating and pressurizing is 6-8MPa, and the holding time is 15-21min.

[0021] An application of the agarwood-containing silicone foam, wherein the agarwood-containing silicone foam is used in a pillow core.

[0022] (iii) Beneficial technical effects Compared with the prior art, the beneficial effects of the present invention are as follows: (1) In this invention, the agarwood extract is extracted using supercritical CO2, preserving its natural calming active ingredients. According to traditional Chinese medicine theory, agarwood's effects of "regulating qi and relieving pain, warming the middle jiao and stopping vomiting, and regulating qi and relieving asthma" can be gently applied to the body through nasal inhalation during pillow use, alleviating anxiety and improving sleep difficulties. Chitosan@SiO2 is used as the backbone, grafted with hydrophobic β-cyclodextrin, forming a porous, high-specific-surface-area three-dimensional network composite carrier. The agarwood extract is effectively encapsulated in the cavities of β-cyclodextrin and anchored to the chitosan@SiO2 backbone through hydrogen bonds and van der Waals forces, effectively preventing the rapid volatilization and loss of agarwood molecules during processing and initial use. During use, with changes in ambient temperature and humidity, and slight pressure, agarwood molecules slowly desorb and release from the carrier, ensuring a continuous and stable release of aroma and enhancing its calming and sleep-aiding functions.

[0023] (2) In the foaming process of the silicone foam in this invention, the exposed agarwood extract is easily decomposed and deteriorated. The use of a composite carrier provides an effective thermal barrier protection for the agarwood molecules, allowing them to maintain their biological activity and aroma characteristics after processing, thus ensuring the functionality of the final product. Furthermore, agarwood has natural antibacterial properties, which, in synergy with chitosan, have excellent antibacterial effects, effectively preventing the growth of bacteria in the pillow core during use.

[0024] (3) In this invention, activated azodicarbonamide and sodium bicarbonate are compounded, and zinc oxide is added as an activator. The foaming process and cross-linking process are carried out simultaneously, resulting in uniform and fine bubbles, thus preparing a low-density, high-resilience foam structure. When used as a pillow core, it can provide a soft touch and good support, effectively disperse pressure, and provide excellent comfort. The reinforcing agent, through hydrophobic modification, has excellent compatibility with organosiloxane matrices, avoiding the aggregation of nanoparticles and enabling it to be uniformly dispersed in the silicone rubber network, forming a strong three-dimensional reinforcing network. It provides moderate hardness and high resilience, the foam is soft but not easy to collapse, provides lasting comfort, and has a long service life.

[0025] (4) The silicone foam prepared in this invention has a long-lasting fragrance, a comfortable feel during use, good support, and is durable. It has broad application prospects in smart home, health care and other fields. Detailed Implementation

[0026] To facilitate understanding of the present invention, a more complete description will be provided below. Preferred embodiments of the invention are given below. However, the invention can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a thorough and complete understanding of the disclosure of the invention.

[0027] Example 1 A functional component of agarwood, the preparation method of which includes the following steps: S1. Mix nano-silica, ethanol solution, and propyltriethoxysilane isocyanate, heat to 65°C and stir for 6 hours. Add acetic acid solution to adjust the pH to 4. After mixing evenly, add chitosan. The mass ratio of nano-silica, ethanol solution, propyltriethoxysilane isocyanate, and chitosan is 100:3500:5:105. Stir at 60°C for 36 hours, centrifuge, wash with deionized water and anhydrous ethanol, and freeze dry to obtain chitosan@SiO2. S2. Isopropanol, β-cyclodextrin, and dimethyl sulfoxide were mixed evenly, and epichlorohydrin was added. The pH was adjusted to 9 using sodium hydroxide solution, and the mixture was stirred for 4 hours. Chitosan@SiO2 was then added, with the mass ratio of isopropanol, β-cyclodextrin, dimethyl sulfoxide, epichlorohydrin, and chitosan@SiO2 being 600:100:35:21:110. The mixture was stirred and reacted at 55°C for 6 hours. After the reaction was completed, the mixture was filtered, washed with deionized water, and freeze-dried to obtain the modified cyclodextrin-chitosan complex. S3. Mix acetic acid solution, modified cyclodextrin-chitosan complex and agarwood extract in a mass ratio of 1400:100:10, stir at room temperature for 6 hours, let stand at 0℃ for 24 hours, adjust pH to neutral with sodium hydroxide solution, filter, wash with deionized water, freeze dry to obtain agarwood functional components.

[0028] Example 2 A functional component of agarwood, the preparation method of which includes the following steps: S1. Mix nano-silica, ethanol solution, and propyltriethoxysilane isocyanate, heat to 70°C and stir for 5 hours. Add acetic acid solution to adjust the pH to 4.5. After mixing evenly, add chitosan. The mass ratio of nano-silica, ethanol solution, propyltriethoxysilane isocyanate, and chitosan is 100:4000:15:160. Stir at 65°C for 32 hours, centrifuge, wash with deionized water and anhydrous ethanol, and freeze-dry to obtain chitosan@SiO2. S2. Isopropanol, β-cyclodextrin, and dimethyl sulfoxide were mixed evenly, and epichlorohydrin was added. The pH was adjusted to 9.5 using sodium hydroxide solution, and the mixture was stirred for 5 hours. Chitosan@SiO2 was then added, with the mass ratio of isopropanol, β-cyclodextrin, dimethyl sulfoxide, epichlorohydrin, and chitosan@SiO2 being 800:100:48:28:120. The mixture was stirred and reacted at 60°C for 5 hours. After the reaction was completed, the mixture was filtered, washed with deionized water, and freeze-dried to obtain the modified cyclodextrin-chitosan complex. S3. Mix acetic acid solution, modified cyclodextrin-chitosan complex and agarwood extract in a mass ratio of 1500:100:12, stir at room temperature for 7 hours, let stand at 2°C for 24 hours, adjust pH to neutral with sodium hydroxide solution, filter, wash with deionized water, freeze dry to obtain agarwood functional components.

[0029] Example 3 A functional component of agarwood, the preparation method of which includes the following steps: S1. Mix nano-silica, ethanol solution, and propyltriethoxysilane isocyanate, heat to 75°C and stir for 4 hours. Add acetic acid solution to adjust the pH to 5. After mixing evenly, add chitosan. The mass ratio of nano-silica, ethanol solution, propyltriethoxysilane isocyanate, and chitosan is 100:5000:20:200. Stir at 70°C for 24 hours, centrifuge, wash with deionized water and anhydrous ethanol, and freeze dry to obtain chitosan@SiO2. S2. Isopropanol, β-cyclodextrin, and dimethyl sulfoxide were mixed evenly, and epichlorohydrin was added. The pH was adjusted to 10 using sodium hydroxide solution, and the mixture was stirred for 6 hours. Chitosan@SiO2 was then added, with the mass ratio of isopropanol, β-cyclodextrin, dimethyl sulfoxide, epichlorohydrin, and chitosan@SiO2 being 900:100:52:32:130. The mixture was stirred and reacted at 65°C for 4 hours. After the reaction was completed, the mixture was filtered, washed with deionized water, and freeze-dried to obtain the modified cyclodextrin-chitosan complex. S3. Mix acetic acid solution, modified cyclodextrin-chitosan complex and agarwood extract in a mass ratio of 1600:100:15, stir at room temperature for 8 hours, let stand at 5°C for 24 hours, adjust pH to neutral with sodium hydroxide solution, filter, wash with deionized water, freeze dry to obtain agarwood functional components.

[0030] Example 4 A hydrophobically modified fumed silica nanoparticle, the preparation method of which includes the following steps: Anhydrous ethanol, methyl silicate, cetyltrimethylammonium bromide surfactant, and polyvinylpyrrolidone were stirred and mixed, and then 25% ammonia and hexamethyldisilazane were added. The mass ratio of anhydrous ethanol, methyl silicate, cetyltrimethylammonium bromide, polyvinylpyrrolidone, 25% ammonia, and hexamethyldisilazane was 350:100:5:2:35:18. The mixture was stirred and mixed, and reacted at 25°C for 5 hours. After the reaction was completed, the mixture was allowed to stand and age for 24 hours. After aging, the mixture was dispersed using a high-speed shear disperser to obtain hydrophobically modified fumed silica nanoparticles.

[0031] Example 5 A hydrophobically modified fumed silica nanoparticle, the preparation method of which includes the following steps: Anhydrous ethanol, methyl silicate, cetyltrimethylammonium bromide surfactant, and polyvinylpyrrolidone were stirred and mixed, and then 25% ammonia and hexamethyldisilazane were added. The mass ratio of anhydrous ethanol, methyl silicate, cetyltrimethylammonium bromide, polyvinylpyrrolidone, 25% ammonia, and hexamethyldisilazane was 450:100:8:2.5:42:25. The mixture was stirred and mixed, and reacted at 30°C for 4.5 h. After the reaction was completed, the mixture was allowed to stand and age for 24 h. After aging, the mixture was dispersed using a high-speed shear disperser to obtain hydrophobically modified fumed silica nanoparticles.

[0032] Example 6 A hydrophobically modified fumed silica nanoparticle, the preparation method of which includes the following steps: Anhydrous ethanol, methyl silicate, cetyltrimethylammonium bromide surfactant, and polyvinylpyrrolidone were stirred and mixed. Then, 25% ammonia and hexamethyldisilazane were added. The mass ratio of anhydrous ethanol, methyl silicate, cetyltrimethylammonium bromide, polyvinylpyrrolidone, 25% ammonia, and hexamethyldisilazane was 500:100:10:3:50:30. The mixture was stirred and mixed, and reacted at 35°C for 4 hours. After the reaction was completed, the mixture was allowed to stand and age for 24 hours. After aging, the mixture was dispersed using a high-speed shear disperser to obtain hydrophobically modified fumed silica nanoparticles.

[0033] Example 7 A silicone foam containing agarwood is prepared by the following steps: 100 parts by weight of organosiloxane are added to a mixer for mixing, wherein the organosiloxane is composed of vinyl-terminated polydimethylsiloxane and divinyltetramethyldisiloxane in a mass ratio of 88:12. The mixing temperature is 80℃, the speed is 30r / min, and the time is 15min. Then, 15 parts of reinforcing agent and 2 parts of dispersant γ-methacryloyloxypropyltrimethoxysilane are added and mixed at 80℃ and 40r / min for 30min. Then, 5 parts of agarwood functional components are added and mixed at 60℃ and 30r / min for 20min to obtain functional base glue. Step 2: Transfer the functional base rubber to a two-roll mill, add 0.5 parts of antioxidant 1076 and 4 parts of crosslinking agent methyl-terminated hydrogen-containing silicone oil, mix for 8 minutes, then add 0.05 parts of platinum catalyst and 3 parts of foaming agent. The foaming agent is composed of activated azodicarbonamide and sodium bicarbonate in a mass ratio of 1:1. Mix for 5 minutes to obtain a uniform rubber compound. Step 3: Place the rubber material into a mold preheated to 100℃, raise the temperature and pressurize it to 160℃ and 6MPa, and keep it heated and pressurized for 21 minutes. After depressurization, open the mold, take it out, and let it cool naturally to room temperature to obtain silicone foam containing agarwood.

[0034] The preparation method of the agarwood functional components in this embodiment is completely consistent with the preparation method of the agarwood functional components in Example 1. The reinforcing agent is hydrophobically modified fumed silica, and its preparation method is completely consistent with the preparation method of hydrophobically modified fumed silica in Example 4.

[0035] Example 8 A silicone foam containing agarwood is prepared by the following steps: 100 parts by weight of organosiloxane are added to a mixer for mixing, wherein the organosiloxane is composed of vinyl-terminated polydimethylsiloxane and divinyltetramethyldisiloxane in a mass ratio of 89:11. The mixing temperature is 85℃, the speed is 35r / min, and the time is 12min. Then, 20 parts of reinforcing agent and 2.4 parts of dispersant γ-methacryloyloxypropyltrimethoxysilane are added and mixed at 85℃ and 45r / min for 25min. Then, 6 parts of agarwood functional components are added and mixed at 65℃ and 35r / min for 16min to obtain functional base glue. Step 2: Transfer the functional base rubber to a two-roll mill, add 1 part of antioxidant 1076 and 5 parts of crosslinking agent methyl-terminated hydrogen-containing silicone oil, mix for 9 minutes, then add 0.08 parts of platinum catalyst and 4 parts of foaming agent. The foaming agent is composed of activated azodicarbonamide and sodium bicarbonate in a mass ratio of 1:1. Mix for 6 minutes to obtain a uniform rubber compound. Step 3: Place the rubber material into a mold preheated to 100℃, raise the temperature and pressurize it to 165℃ and 7MPa, and keep it heated and pressurized for 18 minutes. After depressurization, open the mold, take it out, and let it cool naturally to room temperature to obtain silicone foam containing agarwood.

[0036] The preparation method of the agarwood functional components in this embodiment is completely consistent with the preparation method of the agarwood functional components in Example 2. The reinforcing agent is hydrophobically modified fumed silica nanoparticles, and its preparation method is completely consistent with the preparation method of hydrophobically modified fumed silica nanoparticles in Example 5.

[0037] Example 9 A silicone foam containing agarwood is prepared by the following steps: 100 parts by weight of organosiloxane are added to a mixer for mixing, wherein the organosiloxane is composed of vinyl-terminated polydimethylsiloxane and divinyltetramethyldisiloxane in a mass ratio of 89:11. The mixing temperature is 85℃, the rotation speed is 35r / min, and the time is 12min. Then, 24 parts of reinforcing agent and 2.8 parts of dispersant γ-methacryloyloxypropyltrimethoxysilane are added and mixed at 85℃ and 45r / min for 28min. Then, 7 parts of agarwood functional components are added and mixed at 65℃ and 35r / min for 18min to obtain functional base glue. Step 2: Transfer the functional base rubber to a two-roll mill, add 1.2 parts of antioxidant 1076 and 6 parts of crosslinking agent methyl-terminated hydrogen-containing silicone oil, mix for 9 minutes, then add 0.09 parts of platinum catalyst and 5 parts of foaming agent. The foaming agent is composed of activated azodicarbonamide and sodium bicarbonate in a mass ratio of 1:1. Mix for 7 minutes to obtain a uniform rubber compound. Step 3: Place the rubber material into a mold preheated to 100℃, raise the temperature and pressurize it to 165℃ and 7MPa, and keep it heated and pressurized for 20 minutes. After depressurization, open the mold, take it out, and let it cool naturally to room temperature to obtain silicone foam containing agarwood.

[0038] The preparation method of the agarwood functional components in this embodiment is completely consistent with the preparation method of the agarwood functional components in Example 2. The reinforcing agent is hydrophobically modified fumed silica nanoparticles, and its preparation method is completely consistent with the preparation method of hydrophobically modified fumed silica nanoparticles in Example 5.

[0039] Example 10 A silicone foam containing agarwood is prepared by the following steps: 100 parts by weight of organosiloxane are added to a mixer for mixing, wherein the organosiloxane is composed of vinyl-terminated polydimethylsiloxane and divinyltetramethyldisiloxane in a mass ratio of 90:10. The mixing temperature is 90℃, the speed is 40r / min, and the time is 10min. Then, 25 parts of reinforcing agent and 3 parts of dispersant γ-methacryloyloxypropyltrimethoxysilane are added and mixed at 90℃ and 50r / min for 20min. Then, 8 parts of agarwood functional components are added and mixed at 70℃ and 40r / min for 15min to obtain functional base glue. Step 2: Transfer the functional base rubber to a two-roll mill, add 1.5 parts of antioxidant 1076 and 7 parts of crosslinking agent methyl-terminated hydrogen-containing silicone oil, mix for 10 minutes, then add 0.1 parts of platinum catalyst and 6 parts of foaming agent. The foaming agent is composed of activated azodicarbonamide and sodium bicarbonate in a mass ratio of 1:1. Mix for 8 minutes to obtain a uniform rubber compound. Step 3: Place the rubber material into a mold preheated to 100℃, raise the temperature and pressurize it to 170℃ and 8MPa, and keep it heated and pressurized for 15 minutes. After depressurization, open the mold, take it out, and let it cool naturally to room temperature to obtain silicone foam containing agarwood.

[0040] The preparation method of the agarwood functional components in this embodiment is completely consistent with the preparation method of the agarwood functional components in Example 3. The reinforcing agent is hydrophobically modified fumed silica nanoparticles, and its preparation method is completely consistent with the preparation method of hydrophobically modified fumed silica nanoparticles in Example 6.

[0041] Comparative Example 1 A method for preparing silicone foam containing agarwood, compared with Example 9, differs only in that the agarwood functional components are replaced with agarwood extract in equal amounts, while the other components and preparation methods are completely consistent with Example 9.

[0042] Comparative Example 2 A method for preparing silicone foam containing agarwood is compared with that in Example 9, except that the preparation method of the agarwood functional component is different, while the other components and preparation methods are completely the same as in Example 9.

[0043] The preparation method of the agarwood functional components in this comparative example includes the following steps: Acetic acid solution, nano-silica, chitosan, β-cyclodextrin, and agarwood extract were mixed in a mass ratio of 1500:45:21:34:12. The mixture was stirred at room temperature for 7 hours, then allowed to stand at 2°C for 24 hours. The pH was adjusted to neutral using sodium hydroxide solution. The mixture was filtered, washed with deionized water, and freeze-dried to obtain the agarwood functional components.

[0044] Comparative Example 3 A method for preparing agarwood-containing silicone foam, compared with Example 9, differs only in that the reinforcing agent hydrophobically modified fumed silica is replaced with an equal amount of nano silica, while the other components and preparation methods are completely consistent with Example 9.

[0045] Comparative Example 4 A method for preparing silicone foam containing agarwood is compared with that in Example 9, except that no agarwood functional component is added, while the other components and preparation methods are completely the same as in Example 9.

[0046] The nano-silica used in the examples and comparative examples of this invention was purchased from Jiangsu Lianyungang Pengrui Chemical Co., Ltd., with an average particle size of 15 nm; chitosan was purchased from Shandong Aokang Biotechnology Co., Ltd.; β-cyclodextrin was purchased from Zhengzhou Anhua Food Additives Co., Ltd.; other raw materials and reagents not specified can be obtained from commercial sources.

[0047] The silica gel foams containing agarwood prepared in Examples 7-10 and Comparative Examples 1-4 were subjected to relevant performance tests, as follows: To verify the efficacy of the agarwood-containing silicone foam pillow core of this invention, 400 patients with sleep problems were selected for treatment, including 231 males and 169 females, aged between 18 and 60 years old. They were randomly divided into 8 groups of 50 people each. They used the pillow cores corresponding to Examples 7-10 and Comparative Examples 1-4 respectively when sleeping. They used the pillow core of this invention continuously for 6 months, and stopped using other drugs and health products during the period. There were no significant differences in gender, age, and disease course among the patients before treatment, so the patients were comparable.

[0048] 1. Diagnostic criteria: Refer to the diagnostic criteria specified in the "Standards for Diagnosis and Efficacy of Diseases and Syndromes in Traditional Chinese Medicine": (1) Insomnia manifests as difficulty falling asleep, with a sleep onset time exceeding 30 minutes; (2) Decreased sleep quality, sleep maintenance disorder, ≥2 awakenings per night, early awakening, and decreased sleep quality; (3) Total sleep time is reduced, usually less than 6 hours; (4) In addition to the above symptoms, there are sleep-related daytime dysfunctions, including: 1) fatigue or malaise; 2) impaired attention or memory; 3) decreased learning, work and / or social abilities; 4) mood swings or irritability; 5) daytime sleepiness; 6) decreased interest and energy; 7) increased tendency to make mistakes while working or driving; 8) tension, headache, dizziness, or other physical symptoms related to sleep deprivation; 9) excessive concern about sleep; Efficacy evaluation criteria: The criteria are determined with reference to the "Standards for Diagnosis and Efficacy Evaluation of Diseases in Traditional Chinese Medicine" formulated by the State Administration of Traditional Chinese Medicine. Cure: Symptoms and signs disappear, and mental state recovers; Effective: Symptoms and signs basically disappear, but fatigue is not fully recovered; Ineffective: Symptoms do not improve, and the condition remains the same as before treatment; The average value of the above test results is shown in Table 1: Table 1

[0049] As shown in Table 1, the number of patients cured in Examples 7-10 of this invention is significantly higher than that in Comparative Examples 1-4, indicating excellent therapeutic effects. The effective rate of Example 9 reaches 92%. In Comparative Example 1, the pure agarwood extract replaced the modified functional components, resulting in easy loss of aroma and reduced efficacy. Although effective, the cure rate was low and it could not continuously regulate sleep. In Comparative Example 2, the agarwood functional components were obtained through simple mixing, resulting in an unstable carrier structure and a lack of a three-dimensional sustained-release network formed by chemical bonds. The carrier had weak adsorption force on the agarwood components, and the release rate of active ingredients was uneven, reducing the effective rate. In Comparative Example 3, ordinary nano-silica replaced the hydrophobic modifier, leading to poor compatibility and uneven formation of micropores inside the foam. Aroma molecules easily escaped quickly from the gaps, exacerbating aroma loss and greatly reducing the effect. In Comparative Example 4, no agarwood-related active ingredients were added; only ordinary silicone foam was used, which could only provide basic support and comfort, without any pharmacological effect on regulating sleep, resulting in poor improvement.

[0050] 2. Persistence: The persistence of the pillow core's aroma was measured. Under natural conditions, sensory evaluation was conducted, mainly focusing on the sleep-aiding aroma of agarwood, including the concentration and quality of the agarwood aroma. The score was based on a scale of 0 to 10, with higher scores indicating better aroma characteristics of agarwood. The tests were conducted after continuous use of the pillow core for 1 day, 10 days, 30 days, 90 days, and 180 days. The average value of the above test results is shown in Table 2: Table 2

[0051] As can be seen from the test results in Table 2, the samples corresponding to Examples 7-10 of this invention exhibit excellent aroma persistence. Even after 180 days, the sample corresponding to Example 9 still achieved a score of 6.4, mainly due to the composite carrier, which effectively locks in the volatile components of agarwood, allowing for slow release and good persistence. Comparative Example 1 showed the worst aroma persistence, primarily because the added agarwood extract offered almost no protection, remaining completely exposed to the open-pore structure of the silicone foam. Comparative Example 2, prepared through simple mixing of functional components, failed to form a robust encapsulation, resulting in rapid release and loss of agarwood components in the early stages. In Comparative Example 3, nano-silica tended to aggregate, leading to localized defects that became channels for rapid aroma loss.

[0052] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention. All equivalent changes and improvements made within the scope of the present invention should still fall within the scope of the present invention.

Claims

1. A silica gel foam containing linaloe, characterized by: By weight, it includes the following raw materials: 100 parts of organosiloxane; 5-8 parts of agarwood functional components; Catalyst 0.05-0.1 parts; 4-7 parts of crosslinking agent; 2-3 parts dispersant; 15-25 parts of reinforcing agent; 3-6 parts of foaming agent; 0.5-1.5 parts of auxiliary agent; The organosiloxane is composed of vinyl-terminated polydimethylsiloxane and divinyltetramethyldisiloxane in a mass ratio of 88-90:10-12. The agarwood functional components are obtained by combining agarwood extract with a modified cyclodextrin-chitosan complex.

2. The silica gel foam containing linaloe according to claim 1, characterized in that: The agarwood functional components are prepared by the following method: S1. Mix nano-silica, ethanol solution, and propyltriethoxysilane isocyanate, heat to 65-75℃ and stir for 4-6 hours, add acetic acid solution to adjust pH to 4-5, mix evenly, then add chitosan, stir at 60-70℃ for 24-36 hours, centrifuge, wash, freeze dry to obtain chitosan@SiO2. S2. Isopropanol, β-cyclodextrin, and dimethyl sulfoxide were mixed evenly, and epichlorohydrin was added. The pH was adjusted to 9-10 using sodium hydroxide solution. The mixture was stirred for 4-6 hours, and chitosan@SiO2 was added. The mixture was stirred and mixed to allow the reaction to occur. After the reaction was completed, the mixture was filtered, washed, and freeze-dried to obtain the modified cyclodextrin-chitosan complex. S3. Mix acetic acid solution, modified cyclodextrin-chitosan complex and agarwood extract, stir at room temperature for 6-8 hours, let stand at 0-5℃ for 24 hours, adjust pH to neutral with sodium hydroxide solution, filter, wash, freeze dry to obtain agarwood functional components.

3. The silica gel foam containing linaloe according to claim 2, characterized in that: The mass ratio of nano-silica, ethanol solution, propyltriethoxysilane isocyanate, and chitosan in S1 is 100:3500-5000:5-20:105-200.

4. The silicone foam containing agarwood according to claim 2, characterized in that: The mass ratio of isopropanol, β-cyclodextrin, dimethyl sulfoxide, epichlorohydrin, and chitosan@SiO2 in S2 is 600-900:100:35-52:21-32:110-130, the reaction temperature is 55-65℃, and the reaction time is 4-6h.

5. The silicone foam containing agarwood according to claim 2, characterized in that: The mass ratio of acetic acid solution, modified cyclodextrin-chitosan complex, and agarwood extract in S3 is 1400-1600:100:10-15.

6. The silicone foam containing agarwood according to claim 1, characterized in that: The catalyst is a platinum catalyst; the crosslinking agent is methyl-terminated hydrogen-containing silicone oil; the dispersant is γ-methacryloyloxypropyltrimethoxysilane; the foaming agent is composed of activated azodicarbonamide and sodium bicarbonate in a mass ratio of 1:1; and the auxiliary agent is antioxidant 1076.

7. The silicone foam containing agarwood according to claim 1, characterized in that: The reinforcing agent is hydrophobically modified fumed silica nanoparticles. The specific preparation method includes the following steps: anhydrous ethanol, methyl silicate, cetyltrimethylammonium bromide surfactant, and polyvinylpyrrolidone are stirred and mixed, and then 25% ammonia and hexamethyldisilazane are added. The mass ratio of anhydrous ethanol, methyl silicate, cetyltrimethylammonium bromide, polyvinylpyrrolidone, 25% ammonia, and hexamethyldisilazane is 350-500:100:5-10:2-3:35-50:18-30. The mixture is stirred and mixed, and reacted at 25-35℃ for 4-5 hours. After the reaction is completed, the mixture is allowed to stand and age for 24 hours. After aging, the mixture is dispersed using a high-speed shear disperser to obtain hydrophobically modified fumed silica nanoparticles.

8. A method for preparing a silica gel foam containing agarwood as described in any one of claims 1-7, characterized in that: Includes the following steps: Step 1: Add organosiloxane to a mixer and mix at a temperature of 80-90℃, a speed of 30-40r / min, and a time of 10-15min. Then add reinforcing agent and dispersant and mix at 80-90℃ and 40-50r / min for 20-30min. Then add agarwood functional components and mix at 60-70℃ and 30-40r / min for 15-20min to obtain functional base adhesive. Step 2: Transfer the functional base rubber to a two-roll mill, add the additives and crosslinking agent, mix for 8-10 minutes, then add the catalyst and foaming agent, mix for 5-8 minutes to obtain a uniform rubber compound. Step 3: Place the adhesive material into a mold preheated to 100℃, heat and pressurize, release the pressure, open the mold, take it out, and let it cool naturally to room temperature to obtain silicone foam containing agarwood.

9. The method for preparing a silica gel foam containing agarwood according to claim 8, characterized in that: In step three, the temperature for heating and pressurizing is 160-170℃, the pressure for heating and pressurizing is 6-8MPa, and the holding time is 15-21min.

10. An application of a silicone foam containing agarwood as described in any one of claims 1-7, characterized in that: The silicone foam containing agarwood is used in the pillow core.

Citation Information

Patent Citations

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