Modified silicon dioxide microcapsule, composition as well as preparation and application of modified silicon dioxide microcapsule

Abstract

The invention relates to a modified silicon dioxide microcapsule, a composition as well as preparation and application thereof, the composition is used for textile processing and has remarkable comprehensive effects of helping sleep and improving microcirculation, and due to modification of PEI, the washing fastness of fabrics is remarkably improved.

Description

Technical Field

[0001] The present invention belongs to the field of functional additives, and particularly relates to a modified silica microcapsule, a composition, and their preparation and applications. Background Art

[0002] Currently, commonly used drugs for treating sleep disorders have extensive side effects (addiction and tolerance to benzodiazepines). Therefore, there is an urgent need to improve the methods for treating sleep disorders. It is necessary to prepare a general processing composition additive with good efficacy and few side effects. This low side effect rate is expected to be achieved when applying natural essential oil compositions.

[0003] The unique fragrance and various uses of lavender essential oil (LEO) have made it an increasingly concerned topic in the fields of aromatherapy, herbal medicine, food, perfume, and cosmetics. It has been proven to have various pharmacological effects, including antibacterial, antioxidant, anti-inflammatory, immunomodulatory, and potential anti-cancer properties. In addition, studies have also shown its effectiveness in pain management and the treatment of a series of neuropsychiatric diseases, such as stress, depression, and anxiety. In addition, its potential applications as an antiemetic, an antipsoriatic, and a wound healing promoter have also been explored.

[0004] However, due to the high volatility, low water solubility, and strong sensory properties of LEO, its applications in the textile industry are still limited. Encapsulation and slow release technology can solve these problems. The encapsulation technology loads the active agent into the matrix at the micron or nanometer level to protect them from external damage. For textile processing, LEO microcapsules can be applied to textiles at any stage of the production process and can be processed into textile materials by adopting technologies such as coating, impregnation, and exhaustion during fiber spinning and fabric finishing processes. However, in traditional processing, the strength of the microcapsule wall material is insufficient, and its adsorption performance on the fabric surface and wash resistance are not good. Moreover, relying solely on lavender essential oil, its effects of relieving insomnia, reducing pain, and increasing physical comfort are also relatively limited. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to provide a modified silica microcapsule, a composition, and their preparation and applications

[0006] The present invention provides a modified silica microcapsule, and the modified silica microcapsule is a silica microcapsule modified by PEI.

[0007] Preferably, for the silica capsule modified by PEI, the silica microcapsule is a slow release microcapsule with lavender essential oil as the core material and silica as the shell.

[0008] Preferably, the average particle size of the silica microcapsule modified by PEI is 10 - 20 μm.

[0009] Preferably, the grafting rate of PEI in the PEI-modified silica capsules is 5%-95%.

[0010] The silica microcapsules are prepared by an emulsion method using raw materials of an aqueous phase and an oil phase; the aqueous phase includes a surfactant and water; the oil phase includes lavender essential oil and tetraethoxysilane (TEOS); the mass ratio of lavender essential oil to tetraethoxysilane (TEOS) is 1-10:1.

[0011] The mass ratio of the aqueous phase to the oil phase is (70-80):(20-50).

[0012] The present invention provides a method for preparing modified silica microcapsules, including: using a silanization reagent to first introduce aldehyde groups on the surface of the capsule wall of the silica microcapsules, and then performing a cross-linking reaction with polyethyleneimine (PEI) to obtain modified silica microcapsules.

[0013] Further, the silanization reagent is 3-aminopropyltriethoxysilane; the cross-linking reaction is a room-temperature stirring reaction for 10-15 h.

[0014] The mass ratio of the polyethyleneimine (PEI) to the aldehyde-group-functionalized silica microcapsules is 1:1-5.

[0015] Using a silanization reagent to first introduce aldehyde groups on the surface of the capsule wall of the silica microcapsules includes: dispersing the silica microcapsule dispersion, a silane coupling agent, and a solvent, reacting at 50-55 °C overnight, washing and then dispersing in methanol, and then adding glutaraldehyde and reacting at room temperature in the dark for 10-15 h. The components include: the silica microcapsule dispersion, the silane coupling agent, and glutaraldehyde, and the dosages are in a volume ratio of 5-15:2:1.25 in sequence.

[0016] The preparation of the silica microcapsules includes: using a mixed solution of a surfactant and water as the aqueous phase, mixing lavender essential oil and tetraethoxysilane as the oil phase, homogenizing and emulsifying the two after mixing to obtain an emulsion, then adjusting the pH to 3-4, stirring at 25-35 °C and 100-200 rpm for 10-24 h to obtain the silica microcapsules.

[0017] The present invention provides a modified silica microcapsule composition. By weight percentage, the components include: any one of the above-mentioned modified silica microcapsules 2-20%, coconut charcoal powder 0.1-5%, thickener 1-10%, penetrant 0.01-0.5%, defoamer 0.1-3%, cross-linking agent 1-10%, and water 51.5-95.7%.

[0018] Preferably, the average particle size of the coconut charcoal powder is 0.1-5 μm.

[0019] Preferably, the thickener is sodium polyacrylate thickener; the penetrant is penetrant JFC; the defoamer is silicone defoamer; the crosslinking agent is polyurethane crosslinking agent.

[0020] Preferably, by weight percentage, the components include: any one of the modified silica microcapsules 5-10%, coconut charcoal powder 0.5-2%, thickener 1-5%, penetrant 0.1-0.5%, defoamer 0.1-2%, crosslinking agent 3-8%, and water is added to 100%.

[0021] The present invention provides a method for preparing a modified silica microcapsule composition, including: weighing each component according to mass percentage, mixing the modified silica microcapsules, coconut charcoal powder, thickener, penetrant, defoamer, crosslinking agent and water, and stirring and mixing evenly to obtain the modified silica microcapsule composition.

[0022] The present invention provides a textile, which is a textile treated with the modified silica microcapsule composition.

[0023] The treatment includes one or several of textile post-finishing processes such as printing, dipping, padding, spraying, etc.

[0024] The present invention provides an application of the modified silica microcapsules or the textile in bedding, smart wearable products, such as three-piece sets for beds, etc.

[0025] The composition of the present invention has the functions of relieving insomnia, reducing pain and increasing physical comfort at the same time. The sustained-release composition contains silica microcapsules and coconut charcoal powder, wherein the core of the microcapsules is lavender essential oil extracted from natural plants, and the capsule wall can be well improved in crosslinking density and strength through the amino modification effect of polyethyleneimine (PEI) with high reactivity. Also, due to the sufficiently high cationic charge density on the surface of the microcapsule particles, the binding strength between the capsule and the fabric can be maximized.

[0026] In the present invention, the surface of silica microcapsules is modified to introduce PEI containing a large number of amino groups on the surface of the capsule wall. Polyethyleneimine (PEI) is a cationic aliphatic polymer, and its molecular structure contains a large number of primary, secondary, and tertiary amine groups. These groups can be protonated and carry positive charges in an acidic environment, thereby enhancing the adsorption of anions in water or processed fabrics. Through the modification of amino groups with high reactivity of polyethyleneimine (PEI) on the capsule wall, the crosslinking density and strength of the capsule wall can be well improved. The adsorption performance of the microcapsules can be greatly enhanced, which is better than simply adding textile adhesives. However, it is difficult for silica to directly react with PEI. In the present invention, a silanization reagent is used to first introduce highly reactive aldehyde groups on the surface of the capsule wall of the silica microcapsules. Finally, PEI is successfully modified onto the surface of the silica microcapsules through a crosslinking reaction.

[0027] A lavender essential oil sustained-release composition mentioned in the present invention further includes the addition of coconut charcoal powder. Compared with common bamboo charcoal powder, bamboo fibers are relatively thick and the structure is relatively loose, with larger pores after carbonization. In contrast, for coconut charcoal powder, the coconut shell has a hard texture and a dense fiber structure, forming small and dense pores after carbonization. Especially for coconut charcoal powder with smaller sizes even at the nanoscale level, it has better dispersibility and a larger specific surface area, is suitable for adsorbing small molecules, has stronger adsorption, can effectively remove odors, effectively release negative ions, improve the air quality around, is rich in various minerals, and various trace elements have health care effects on the human body such as activating cells and eliminating fatigue. It can emit far-infrared rays, increase the subcutaneous temperature, accelerate blood circulation, and promote metabolism. And the PEI on the surface of the silica microcapsules can improve the binding force between the coconut charcoal and the fiber.

[0028] Beneficial effects

[0029] (1) The capsule proposed in the present invention: The capsule wall is silica, and the capsule core is lavender essential oil. The capsule core, which is the plant extract lavender essential oil, has green, environmentally friendly, and safe properties and has been proven to have various pharmacological effects, including antibacterial, antioxidant, anti-inflammatory, immunomodulatory, and potential anti-cancer properties. In addition, it can also relieve pain and soothe stress. The silica capsule wall is successively modified on the surface of the silica phase change microcapsules with aldehyde groups and PEI, thereby introducing highly reactive amino groups, increasing the adhesiveness on the surface of the microcapsules, and also improving the compactness of the silica microcapsule wall material.

[0030] (2) The sustained-release composition containing capsules proposed by the present invention: The coconut charcoal powder in the composition can promote the microcirculation on the surface of the body skin, boost metabolism, enhance the body's immunity, and has health-care functions such as activating cells, helping sleep, and relieving fatigue. There are three reasons why the PEI on the surface of the silica microcapsules can improve the binding force between the coconut charcoal and the fiber: First, since PEI is rich in amino groups, it can react with the oxygen-containing functional groups (such as carboxyl groups and hydroxyl groups) on the surface of the coconut charcoal, thereby enhancing the surface activity of the coconut charcoal. PEI can also cover the surface of the coconut charcoal through physical adsorption, increasing its surface polarity and enhancing the binding force with the fiber. Second, the long-chain structure of PEI can play a "bridge" role between the coconut charcoal and the fiber, connecting the two through chemical bonds or physical adsorption, thereby enhancing the binding force. Third, PEI can also react with the functional groups (such as hydroxyl groups and carboxyl groups) on the surface of the fiber, increasing the surface activity of the fiber, and further enhancing the binding force with the coconut charcoal.

[0031] (3) The textile processed with the sustained-release composition proposed by the present invention: The polar groups such as amino groups on the surface of the modified capsules will form a strong interaction with the fabric surface. Adding a small amount of textile adhesive can further improve the washing resistance effect and ensure the wash fastness of the prepared fabric. Thereby reducing the risk of leakage during the later textile processing and improving its wash resistance on the fabric surface. Description of the Drawings

[0032] Figure 1 is the deposition percentage of the cotton fabrics processed with the lavender essential oil sustained-release compositions of Examples 1-4 prepared by the present invention and Comparative Examples 1-3 after 30 washes;

[0033] Figure 2 is the optical microscope image of the cotton fabric processed with the lavender essential oil sustained-release composition of Example 4 prepared by the present invention after 30 washes;

[0034] Figure 3 is the comparison of the application evaluation results of the three-piece bed sets processed with the lavender essential oil sustained-release compositions of Examples 1-4 prepared by the present invention and Comparative Examples 1-3 regarding comfortable sleep assistance;

[0035] Figure 4 is the comparison of the application evaluation results of the wearable products processed with the lavender essential oil sustained-release compositions of Examples 1-4 prepared by the present invention and Comparative Examples 1-3 regarding relieving body pain and fatigue;

[0036] Figure 5 is the comparison of the microcirculation before and after improvement after using the non-woven fabric processed with the lavender essential oil sustained-release composition of Example 4 prepared by the present invention for two weeks. Detailed Embodiments

[0037] The present invention will be further described below in conjunction with specific embodiments. It should be understood that these embodiments are only used to illustrate the present invention and not to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of this application.

[0038] Example 1

[0039] Step 1: Preparation of aldehyde group-modified silica sustained-release microcapsules (SiO2-CHO):

[0040] (1) Mix 0.20 g of 30 wt% cetyltrimethylammonium chloride (CTAC) with 75 g of deionized water to prepare an aqueous phase. Add the oil phase component prepared by mixing 20 g of lavender essential oil and 5 g of tetraethoxysilane (TEOS) to this aqueous phase, and emulsify the mixed solution using a homogenizing emulsifier with a rotation speed of 9000 rpm to obtain emulsion S1.

[0041] (2) Add 0.16 g of 1 wt% sulfuric acid aqueous solution to the obtained emulsion S1 to obtain emulsion S2 with a pH adjusted to 3.8. Keep stirring at 30 °C and 200 rpm for 24 hours to obtain a sustained-release microcapsule aqueous dispersion S3 with lavender essential oil as the core material and silica as the shell.

[0042] (3) Take 10 mL of the above capsule dispersion S3, and then take 2.0 mL of 3-aminopropyltriethoxysilane and 50 mL of ethanol and add them to a 100 mL three-necked flask. React overnight at 50 °C, and then wash the product (SiO2-NH2) with absolute ethanol multiple times. Finally, disperse it in 10 mL of methanol. Subsequently, add 5.0 mL of 25% glutaraldehyde solution to the SiO2-NH2 dispersion. After reacting in the dark at 25 °C for 12 h, centrifuge the product (SiO2-CHO), and wash it with absolute ethanol and deionized water multiple times. Finally, dry the aldehyde group-modified silica sustained-release capsule (SiO2-CHO) at 25 °C to constant weight to obtain it.

[0043] Step 2: Preparation of PEI-modified silica sustained-release capsules (PEI-SiO2):

[0044] (4) Disperse 1 g of PEI in 100 mL of methanol and mix evenly; another 5 g of the above capsule powder (SiO2-CHO) is weighed and added to the PEI-methanol solution, and stirred for 12 h. Collect the prepared PEI-modified silica sustained-release capsules (PEI-SiO2), wash them and dry them to constant weight at 25 °C to obtain them. The average particle size is 12.5 um.

[0045] Step 3: Preparation of the silica slow-release composition containing coconut charcoal powder (Coconut Charcoal-PEI-SiO2):

[0046] (5) Weigh 5 g of the above-mentioned PEI-modified silica slow-release capsule powder (PEI-SiO2), add 0.5 g of coconut charcoal powder (average particle size of coconut charcoal is 200 nm), 3 g of sodium polyacrylate thickener, 0.1 g of penetrant JFC, 0.1 g of silicone defoamer, 3 g of polyurethane cross-linking agent, add water to 100 g, stir well and mix evenly. Then a lavender essential oil slow-release composition is obtained.

[0047] Example 2

[0048] Step 1: Preparation of aldehyde group-modified silica slow-release microcapsules (SiO2-CHO):

[0049] (1) Mix 0.20 g of 30 wt% cetyltrimethylammonium chloride (CTAC) evenly with 75 g of deionized water to prepare the aqueous phase. Add the oil phase component prepared by mixing 40 g of lavender essential oil and 5 g of tetraethoxysilane (TEOS) to this aqueous phase, and emulsify the mixed solution using a homogenizing emulsifier with a rotation speed of 9000 rpm to obtain emulsion S1.

[0050] (2) Add 0.16 g of 1 wt% sulfuric acid aqueous solution to the obtained emulsion S1 to obtain emulsion S2 with a pH adjusted to 3.8. Keep stirring at 30 °C and 200 rpm for 24 hours to obtain an aqueous dispersion S3 of silica slow-release capsules with lavender essential oil as the core material and silica as the shell material.

[0051] (3) Take 10 mL of the above capsule dispersion S3, then take 2.0 mL of 3-aminopropyltriethoxysilane and 50 mL of ethanol and add them to a 100 mL three-necked flask. React overnight at 50 °C, then wash the product (SiO2-NH2) with absolute ethanol multiple times, and finally disperse it in 10 mL of methanol. Subsequently, add 5.0 mL of 25% glutaraldehyde solution to the SiO2-NH2 dispersion. After reacting in the dark at 25 °C for 12 h, centrifuge the product (SiO2-CHO), and wash it with absolute ethanol and deionized water multiple times. Finally, dry the aldehyde group-modified silica slow-release capsules (SiO2-CHO) at 25 °C to constant weight to obtain them.

[0052] Step 2: Preparation of PEI-modified silica slow-release capsules (PEI-SiO2):

[0053] (4) Disperse 1 g of PEI in 100 mL of methanol and mix evenly. Weigh another 5 g of the above capsule powder (SiO2-CHO), add it to the PEI-methanol solution, stir for 12 h, collect the prepared PEI-modified silica sustained-release capsules (PEI-SiO2), wash them and dry them to constant weight at 25 °C to obtain the product. The average particle size is 14.5 μm.

[0054] Step 3: Preparation of the silica sustained-release composition containing coconut charcoal powder (coconut charcoal-PEI-SiO2):

[0055] (5) Weigh 5 g of the above PEI-modified silica sustained-release capsule powder (PEI-SiO2), add 0.5 g of coconut charcoal powder (the particle size of the coconut charcoal powder is 200 nm), 3 g of sodium polyacrylate thickener, 0.1 g of penetrant JFC, 0.1 g of silicone defoamer, 3 g of polyurethane crosslinking agent, add water to 100 g, stir well and mix evenly to obtain a lavender essential oil sustained-release composition.

[0056] Example 3

[0057] Step 1: Preparation of aldehyde group-modified silica sustained-release microcapsules (SiO2-CHO):

[0058] (1) Mix 0.20 g of 30 wt% cetyltrimethylammonium chloride (CTAC) evenly with 75 g of deionized water to prepare the aqueous phase. Add the oil phase component prepared by mixing 40 g of lavender essential oil and 5 g of tetraethoxysilane (TEOS) to this aqueous phase, and emulsify the mixed solution using a homogenizing emulsifier with a rotation speed of 9000 rpm to obtain emulsion S1.

[0059] (2) Add 0.16 g of 1 wt% sulfuric acid aqueous solution to the obtained emulsion S1 to obtain emulsion S2 with a pH adjusted to 3.8. Keep stirring at 30 °C and 200 rpm for 24 h to obtain an aqueous dispersion S3 of silica sustained-release capsules with lavender essential oil as the core material and silica as the shell material.

[0060] (3) Take 10 mL of the above capsule dispersion S3, and then take 2.0 mL of 3-aminopropyltriethoxysilane and 50 mL of ethanol and add them to a 100 mL three-necked flask. React overnight at 50 °C, wash the product (SiO2-NH2) with absolute ethanol multiple times, and finally disperse it in 10 mL of methanol. Subsequently, add 5.0 mL of 25% glutaraldehyde solution to the SiO2-NH2 dispersion. After reacting in the dark at 25 °C for 12 h, centrifuge the product (SiO2-CHO), and wash it with absolute ethanol and deionized water multiple times. Finally, dry the aldehyde group-modified silica sustained-release capsules (SiO2-CHO) to constant weight at 25 °C to obtain the product.

[0061] Step 2: Preparation of PEI-modified silica sustained-release capsules (PEI-SiO2):

[0062] (4) Disperse 2 g of PEI in 100 mL of methanol and mix evenly. Weigh another 5 g of the above capsule powder (SiO2-CHO) and add it to the PEI-methanol solution. Stir for 12 h, collect the prepared PEI-modified silica sustained-release capsules (PEI-SiO2), wash them, and dry them at 25 °C to constant weight. The average particle size is 15.2 μm.

[0063] Step 3: Preparation of silica sustained-release composition containing coconut charcoal powder (coconut charcoal-PEI-SiO2):

[0064] (5) Weigh 5 g of the above PEI-modified silica sustained-release capsule powder (PEI-SiO2), add 0.5 g of coconut charcoal powder (the average particle size of coconut charcoal powder is 200 nm), 3 g of sodium polyacrylate thickener, 0.1 g of penetrant JFC, 0.1 g of silicone defoamer, 3 g of polyurethane crosslinking agent, and add water to 100 g. Stir well and mix evenly to obtain a lavender essential oil sustained-release composition.

[0065] Example 4

[0066] Step 1: Preparation of aldehyde group-modified silica sustained-release microcapsules (SiO2-CHO):

[0067] (1) Mix 0.20 g of 30 wt% cetyltrimethylammonium chloride (CTAC) evenly with 75 g of deionized water to prepare the aqueous phase. Add the oil phase component prepared by mixing 40 g of lavender essential oil and 5 g of tetraethoxysilane (TEOS) to this aqueous phase, and emulsify the mixed solution using a homogenizing emulsifier with a rotation speed of 9000 rpm to obtain emulsion S1.

[0068] (2) Add 0.16 g of 1 wt% sulfuric acid aqueous solution to the obtained emulsion S1 to obtain emulsion S2 with a pH adjusted to 3.8. Keep stirring at 30 °C and 200 rpm for 24 h to obtain an aqueous dispersion S3 of silica sustained-release capsules with lavender essential oil as the core material and silica as the shell material.

[0069] (3) Take 10 mL of the above capsule dispersion S3, then take 2.0 mL of 3-aminopropyltriethoxysilane and 50 mL of ethanol and add them to a 100 mL three-necked flask. After reacting at 50°C overnight, wash the product (SiO2-NH2) with anhydrous ethanol for multiple times, and finally disperse it in 10 mL of methanol. Subsequently, add 5.0 mL of 25% glutaraldehyde solution to the SiO2-NH2 dispersion. After reacting at 25°C in the dark for 12 hours, centrifuge the product (SiO2-CHO) and wash it with anhydrous ethanol and deionized water for multiple times. Finally, dry the aldehyde-modified silica sustained-release capsule (SiO2-CHO) at 25°C to constant weight to obtain.

[0070] Step 2: Preparation of PEI-modified silica sustained-release capsules (PEI-SiO2):

[0071] (4) Disperse 1 g of PEI in 100 mL of methanol and mix well; weigh 5 g of the above capsule powder (SiO2-CHO) and add it to the PEI-methanol solution, stir for 12 h, collect the prepared PEI-modified silica sustained-release capsules (PEI-SiO2), wash and dry at 25°C to constant weight. The average particle size is 14.5 μm.

[0072] Step 3: Preparation of silica sustained-release composition containing coconut charcoal powder (coconut charcoal-PEI-SiO2):

[0073] (5) Weigh 5 g of the above-mentioned PEI-modified silica sustained-release capsule powder (PEI-SiO2), add 1 g of coconut charcoal powder (the average particle size of coconut charcoal powder is 200 nm), 3 g of sodium polyacrylate thickener, 0.1 g of penetrant JFC, 0.1 g of silicone defoamer, 3 g of polyurethane crosslinker, add water to 100 g, stir well, and mix evenly. A lavender essential oil sustained-release composition is obtained.

[0074] Comparative Example 1

[0075] Step 1: Preparation of aldehyde-modified silica sustained-release microcapsules (SiO2-CHO):

[0076] (1) 0.20 g of 30 wt% hexadecyltrimethylammonium chloride (CTAC) was uniformly mixed with 75 g of deionized water to prepare an aqueous phase. An oil phase component prepared by mixing 10 g of lavender essential oil and 5 g of tetraethoxysilane (TEOS) was added to the aqueous phase, and the mixed solution was emulsified using a homogenizer at a rotation speed of 9000 rpm to obtain an emulsion S1.

[0077] (2) 0.16 g of 1 wt % aqueous sulfuric acid solution was added to the obtained emulsion S1 to obtain an emulsion S2 with a pH adjusted to 3.8, and the mixture was stirred at 30° C. and 200 rpm for 24 hours to obtain an aqueous dispersion S3 of silica sustained-release capsules containing lavender essential oil as a core material and silica as a shell.

[0078] (3) Take 10 mL of the above capsule dispersion S3, take 2.0 mL of 3-aminopropyltriethoxysilane and 50 mL of ethanol and add them to a 100 mL three-necked flask. After reacting at 50°C overnight, wash the product (SiO2-NH2) with anhydrous ethanol for several times and finally disperse it in 10 mL of methanol. Subsequently, add 5.0 mL of 25% glutaraldehyde solution to the SiO2-NH2 dispersion. After reacting at 25°C in the dark for 12 hours, centrifuge the product (SiO 2- CHO), washed with anhydrous ethanol and deionized water for multiple times. Finally, the aldehyde-modified silica sustained-release capsule (SiO2-CHO) was dried at 25°C to constant weight.

[0079] Step 2: Preparation of PEI-modified silica sustained-release capsules (PEI-SiO2):

[0080] (4) Disperse 1 g of PEI in 100 mL of methanol and mix well; weigh 5 g of the above capsule powder (SiO2-CHO) and add it to the PEI-methanol solution, stir for 12 h, collect the prepared PEI-modified silica sustained-release capsules (PEI-SiO2), wash and dry at 25°C to constant weight. The average particle size is 10.5 μm.

[0081] Step 3: Preparation of silica sustained-release composition containing coconut charcoal powder (coconut charcoal-PEI-SiO2):

[0082] (5) Weigh 5 g of the above-mentioned PEI-modified silica sustained-release capsule powder (PEI-SiO2), add 0.5 g of coconut charcoal powder (the average particle size of coconut charcoal powder is 200 nm), 3 g of sodium polyacrylate thickener, 0.1 g of penetrant JFC, 0.1 g of silicone defoamer, 3 g of polyurethane crosslinker, add water to 100 g, stir well, and mix evenly. A lavender essential oil sustained-release composition is obtained.

[0083] Comparative Example 2

[0084] Step 1: Preparation of aldehyde-modified silica sustained-release microcapsules (SiO2-CHO):

[0085] (1) 0.20 g of 30 wt% hexadecyltrimethylammonium chloride (CTAC) was uniformly mixed with 75 g of deionized water to prepare an aqueous phase. An oil phase component prepared by mixing 20 g of lavender essential oil and 5 g of tetraethoxysilane (TEOS) was added to the aqueous phase, and the mixed solution was emulsified using a homogenizer at a rotation speed of 9000 rpm to obtain an emulsion S1.

[0086] (2) 0.16 g of 1 wt % aqueous sulfuric acid solution was added to the obtained emulsion S1 to obtain an emulsion S2 with a pH adjusted to 3.8, and the mixture was stirred at 30° C. and 200 rpm for 24 hours to obtain an aqueous dispersion S3 of silica sustained-release capsules containing lavender essential oil as a core material and silica as a shell.

[0087] (3) Take 10 mL of the above capsule dispersion S3, then take 2.0 mL of 3-aminopropyltriethoxysilane and 50 mL of ethanol and add them to a 100 mL three-necked flask. After reacting at 50°C overnight, wash the product (SiO2-NH2) with anhydrous ethanol for multiple times, and finally disperse it in 10 mL of methanol. Subsequently, add 5.0 mL of 25% glutaraldehyde solution to the SiO2-NH2 dispersion. After reacting at 25°C in the dark for 12 hours, centrifuge the product (SiO2-CHO) and wash it with anhydrous ethanol and deionized water for multiple times. Finally, dry the aldehyde-modified silica sustained-release capsules (SiO2-CHO) at 25°C to constant weight to obtain unmodified silica sustained-release capsules with an average particle size of 9.5 um.

[0088] Step 2: Preparation of silica sustained-release composition containing coconut charcoal powder (coconut charcoal-SiO2):

[0089] (4) Weigh 5 g of the above-mentioned silica sustained-release capsule powder (SiO2) not modified by PEI, add 0.5 g of coconut charcoal powder (the average particle size of coconut charcoal powder is 200 nm), 3 g of sodium polyacrylate thickener, 0.1 g of penetrant JFC, 0.1 g of silicone defoamer, 3 g of polyurethane crosslinker, add water to 100 g, stir well, and mix evenly. A lavender essential oil sustained-release composition is obtained.

[0090] Comparative Example 3

[0091] Step 1: Preparation of aldehyde-modified silica sustained-release microcapsules (SiO2-CHO):

[0092] (1) 0.20 g of 30 wt% hexadecyltrimethylammonium chloride (CTAC) was uniformly mixed with 75 g of deionized water to prepare an aqueous phase. An oil phase component prepared by mixing 20 g of lavender essential oil and 5 g of tetraethoxysilane (TEOS) was added to the aqueous phase, and the mixed solution was emulsified using a homogenizer at a rotation speed of 9000 rpm to obtain an emulsion S1.

[0093] (2) 0.16 g of 1 wt % aqueous sulfuric acid solution was added to the obtained emulsion S1 to obtain an emulsion S2 with a pH adjusted to 3.8, and the mixture was stirred at 30° C. and 200 rpm for 24 hours to obtain an aqueous dispersion S3 of silica sustained-release capsules containing lavender essential oil as a core material and silica as a shell.

[0094] (3) Take 10 mL of the above capsule dispersion S3, then take 2.0 mL of 3-aminopropyltriethoxysilane and 50 mL of ethanol and add them to a 100 mL three-necked flask. After reacting at 50°C overnight, wash the product (SiO2-NH2) with anhydrous ethanol for multiple times, and finally disperse it in 10 mL of methanol. Subsequently, add 5.0 mL of 25% glutaraldehyde solution to the SiO2-NH2 dispersion. After reacting at 25°C in the dark for 12 hours, centrifuge the product (SiO2-CHO) and wash it with anhydrous ethanol and deionized water for multiple times. Finally, dry the aldehyde-modified silica sustained-release capsule (SiO2-CHO) at 25°C to constant weight to obtain.

[0095] Step 2: Preparation of PEI-modified silica sustained-release capsules (PEI-SiO2):

[0096] (4) Disperse 1 g of PEI in 100 mL of methanol and mix well; weigh 5 g of the above capsule powder (SiO2-CHO) and add it to the PEI-methanol solution, stir for 12 h, collect the prepared PEI-modified silica sustained-release capsules (PEI-SiO2), wash and dry at 25°C to constant weight. The average particle size is 12.5 μm.

[0097] Step 3: Preparation of silica sustained-release composition without coconut charcoal powder (PEI-SiO2):

[0098] (5) Weigh 5.5 g of the above-mentioned PEI-modified silica sustained-release capsule powder (PEI-SiO2), without adding coconut charcoal powder, 3 g of sodium polyacrylate thickener, 0.1 g of penetrant JFC, 0.1 g of silicone defoamer, 3 g of polyurethane crosslinker, add water to 100 g, stir well, and mix evenly. A lavender essential oil sustained-release composition is obtained.

[0099] Comparative Example 4

[0100] Step 1: Preparation of aldehyde-modified silica sustained-release microcapsules (SiO2-CHO):

[0101] (1) Mix 0.20 g of 30 wt% cetyltrimethylammonium chloride (CTAC) evenly with 75 g of deionized water to prepare the aqueous phase. Add the oil phase component prepared by mixing 20 g of lavender essential oil and 5 g of tetraethoxysilane (TEOS) to this aqueous phase, and emulsify the mixed solution using a homogenizing emulsifier with a rotation speed of 9000 rpm to obtain emulsion S1.

[0102] (2) Add 0.16 g of 1 wt% sulfuric acid aqueous solution to the obtained emulsion S1 to obtain emulsion S2 with a pH adjusted to 3.8. Keep it at 30 °C and stir at 200 rpm for 24 hours to obtain an aqueous dispersion S3 of silica sustained-release capsules with lavender essential oil as the core material and silica as the shell.

[0103] (3) Take 10 mL of the above capsule dispersion S3, and then take 2.0 mL of 3-aminopropyltriethoxysilane and 50 mL of ethanol and add them to a 100 mL three-necked flask. React overnight at 50 °C, and then wash the product (SiO2-NH2) with absolute ethanol multiple times. Finally, disperse it in 10 mL of methanol. Subsequently, add 5.0 mL of 25% glutaraldehyde solution to the SiO2-NH2 dispersion. After reacting in the dark at 25 °C for 12 h, centrifuge the product (SiO2-CHO), and wash it with absolute ethanol and deionized water multiple times. Finally, dry the aldehyde group-modified silica sustained-release capsule (SiO2-CHO) at 25 °C to constant weight to obtain it.

[0104] Step 2: Preparation of PEI-modified silica sustained-release capsules (PEI-SiO2):

[0105] (4) Disperse 1 g of PEI evenly in 100 mL of methanol; separately weigh 5 g of the above capsule powder (SiO2-CHO), add it to the PEI-methanol solution, stir for 12 h, collect the prepared PEI-modified silica sustained-release capsules (PEI-SiO2), wash them and dry them to constant weight at 25 °C to obtain them. The average particle size is 12.5 um.

[0106] Step 3: Preparation of silica sustained-release composition without coconut charcoal powder (PEI-SiO2):

[0107] (5) Weigh 5 g of the above PEI-modified silica sustained-release capsule powder (PEI-SiO2), add 0.5 g of bamboo charcoal powder, 3 g of sodium polyacrylate thickener, 0.1 g of penetrant JFC, 0.1 g of silicone defoamer, 3 g of polyurethane crosslinking agent, add water to 100 g, and stir well to mix evenly. Then a lavender essential oil sustained-release composition is obtained.

[0108] Application Example 1

[0109] In the textile post - finishing process, the raw cotton fabric of the three - piece bedding set undergoes functional finishing of this auxiliary agent through the padding process. The specific process is as follows: Immerse the raw cotton fabric into the finishing solution of the lavender essential oil sustained - release composition prepared in advance, where the addition amount of the lavender essential oil sustained - release composition is 3%, ensuring that the fabric fully absorbs it; then perform a one - dip - one - roll operation, that is, after the fabric is impregnated, it is immediately squeezed by the roller to make the finishing solution evenly penetrate and remove the excess liquid. Next, the fabric is dried at 80 degrees, and finally baked at 130 degrees for 90 seconds. Thus obtained.

[0110] Application Example 2

[0111] In the textile post - finishing process, the raw cotton fabric of the wearable product undergoes functional finishing through the printing and coating process. The specific process is as follows: Uniformly blend the functional auxiliary agent into the printing paste at an addition amount of 3%, inject the prepared paste into the paste tank of the printing machine. When the raw fabric passes through the printing machine, the printing roller precisely transfers the paste onto the fabric surface to form a preset pattern (continuous hexagon). Ensure that the functional components are evenly distributed. Subsequently, the fabric undergoes pre - drying treatment at 80 degrees to initially fix the functional layer, and then the functional auxiliary agent is fully combined with the fibers through high - temperature baking at 130 degrees. Thus obtained.

[0112] Experimental evaluation results of each application example

[0113] Select 105 volunteers aged 20 - 60 years old, especially those with poor sleep quality can be selected as volunteers for this product. Randomly divide them into 7 groups (including a blank control group using unprocessed three - piece bedding sets). For the corresponding three - piece bedding products processed from Examples 1 - 4, Comparative Examples 1 - 3, and the blank control, continuously use them for one week, with a frequency of once a day, and do not use other products during this period. Subjectively score the improvement of sleep and comfort in helping sleep on a scale of 0 - 10 points, with the highest score of 10 points (obvious effect in improving sleep), the median value of 5 points (general effect in improving sleep), and the lowest score of 0 points (no effect in improving sleep), and take the average value.

[0114] Select 105 volunteers aged 20 - 60 years old, especially those with slow metabolism, poor microcirculation, joint pain or discomfort can be selected as volunteers for this product. Randomly divide them into 7 groups (including a blank control group using unprocessed wearable products). For the corresponding cotton wearable products processed from Examples 1 - 4, Comparative Examples 1 - 3, and the blank control, continuously use them for two weeks, and do not use other products during this period. Subjectively score the relief of body pain and fatigue on a scale of 0 - 10 points, with the highest score of 10 points (obvious effect in relieving body pain and fatigue), the median value of 5 points (general effect in relieving body pain and fatigue), and the lowest score of 0 points (no effect in relieving body pain and fatigue), and take the average value.

[0115] As Figure 1This figure shows the deposition percentage of the lavender essential oil sustained-release composition on the raw cotton fabric of the three-piece bedding sets processed in Examples 1-4 and Comparative Examples 1-3 after 30 washes. The higher the deposition percentage, the better the adhesion and wash resistance of the composition on the fabric. As can be seen from the figure, the deposition percentages of Examples 1-4 are significantly higher than those of Comparative Examples 1-3, indicating that the composition of silica microcapsules modified with PEI and coconut charcoal powder has better wash resistance.

[0116] As Figure 2 This figure shows the optical microscope image of the raw cotton fabric of the three-piece bedding sets processed in Example 4 after 30 washes. As can be seen from the figure, there are still many microcapsules remaining on the fabric surface after 30 washes, indicating that the composition has strong adhesion and good wash resistance on the fabric.

[0117] As Figure 3 This figure shows the application evaluation results of the three-piece bedding sets processed in Examples 1-4 and Comparative Examples 1-3 in terms of comfortable sleep assistance. The evaluation uses a subjective score of 0-10, and the higher the score, the better the sleep assistance effect. As can be seen from the figure, the scores of Examples 1-4 are significantly higher than those of Comparative Examples 1-3, indicating that the composition of silica microcapsules modified with PEI and coconut charcoal powder has a better effect in sleep assistance.

[0118] As Figure 4 This figure shows the application evaluation results of the wearable products processed in Examples 1-4 and Comparative Examples 1-3 in terms of alleviating body pain and fatigue. The evaluation uses a subjective score of 0-10, and the higher the score, the better the effect of alleviating pain and fatigue. As can be seen from the figure, the scores of Examples 1-4 are significantly higher than those of Comparative Examples 1-3, indicating that the composition has a better effect in alleviating body pain and fatigue.

[0119] As Figure 5 This figure shows the comparison of the effect of improving microcirculation before and after two weeks of use of the cotton fabric of the wearable product treated with the lavender essential oil sustained-release composition processed in Example 4. As can be seen from the figure, after two weeks of use, the microcirculation has been significantly improved, indicating that the composition has the effect of promoting microcirculation and improving metabolism.

Claims

1. A modified silica microcapsule, characterized in that: The modified silica microcapsules are PEI-modified silica microcapsules.

2. The modified silica microcapsule according to claim 1, characterized in that: The PEI-modified silica microcapsules are microcapsules with lavender essential oil as the core material and silica as the shell; The average particle size of the PEI-modified silica microcapsules is 10-20 μm.

3. The modified silica microcapsule according to claim 1, characterized in that: The grafting rate of PEI in the PEI-modified silica microcapsules is 5%-95%; the silica microcapsules are prepared by an emulsion method using raw materials containing an aqueous phase and an oil phase; wherein the aqueous phase includes a surfactant and water; the oil phase includes lavender essential oil and tetraethoxysilane TEOS; wherein The mass ratio of lavender essential oil to tetraethoxysilane TEOS is 1-10:

1.

4. A method for preparing modified silica microcapsules, comprising: Aldehyde groups are first introduced into the capsule wall surface of silica microcapsules by using a silanization agent, and then cross-linked with polyethyleneimine PEI to obtain modified silica microcapsules.

5. A modified silica microcapsule composition, characterized in that: By weight percentage, the components include: 2-20% of the modified silicon dioxide microcapsule according to any one of claims 1-3, 0.1-5% of coconut charcoal powder, 1-10% of a thickener, 0.01-0.5% of a penetrant, 0.1-3% of a defoamer, 1-10% of a crosslinking agent, and 51.5-95.7% of water.

6. The composition according to claim 5, characterized in that The coconut charcoal powder has an average particle size of 0.1-5 μm.

7. The composition according to claim 5, characterized in that The thickener is a sodium polyacrylate thickener; the penetrant is a penetrant JFC; the defoamer is a silicone defoamer; and the crosslinker is a polyurethane crosslinker.

8. A method for preparing a modified silica microcapsule composition, comprising: Weigh each component according to mass percentage, mix the modified silicon dioxide microcapsule, coconut charcoal powder, thickener, penetrant, defoamer, crosslinking agent and water, stir and mix well to obtain a modified silicon dioxide microcapsule composition.

9. A textile, characterized in that: The textile is a textile treated with the modified silica microcapsule composition according to claim 5.

10. Use of the modified silica microcapsule according to claim 1 or the textile according to claim 9 in bedding and smart wearable products.

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