Fragrance with trimethylsilyl modified aerogel loaded with head perfume

Abstract

The invention provides an aromatherapy product with a trimethylsilyl modified aerogel loaded with a head perfume. According to the aromatherapy, trimethylsilyl modified aerogel is used as a carrier to at least adsorb head perfume. Wherein the head spice is at least one of leaf alcohol, ethyl cyclohexyl formate, melonal, isoamyl acetate, octanal and nonanal. According to the aromatherapy disclosed by the invention, the trimethylsilyl modified aerogel is adopted to at least load the head-aroma perfume, so that the aroma retention time of the head-aroma perfume is greatly prolonged, the overall aroma proportion of the aromatherapy is balanced, the freshness feeling is maintained, and meanwhile, the aldehyde head-aroma perfume is also protected and is not easy to oxidize and deteriorate. According to the aromatherapy, the saturation adsorption capacity of the aromatherapy can be adjusted by adjusting the density of the trimethylsilyl modified aerogel, and then release of the top-aroma perfume in the aromatherapy is adjusted, so that the optimal proportion of the overall aroma of the aromatherapy is achieved.

Description

Technical Field

[0001] The invention belongs to the technical field of aromatherapy, and in particular relates to an aromatherapy of trimethylsilyl modified aerogel loaded with top fragrance. Background Art

[0002] Top notes refer to the first impression of the aroma in a flavor or fragranced product, that is, the aroma characteristics that people can smell first. This type of fragrance usually has a high volatility and a strong diffusion power, and the fragrance lasts less than 4 hours on the fragrance evaluation paper. Top notes usually include some highly volatile organic compounds, which are mainly composed of elements such as carbon (C), hydrogen (H), oxygen (O), and nitrogen (N). The specific chemical composition will vary depending on the type of fragrance, but in general, the molecular structure of top notes is relatively simple and easy to volatilize. The aroma of top notes has a strong diffusion power, which can make the aroma of the essence brighter and more transparent, increasing people's initial liking.

[0003] The role and importance of top notes in fragrances are mainly reflected in the following aspects: 1. Give the initial fragrance impression: Top notes are the initial fragrance impression when the fragrance is smelled, usually composed of spices with good volatility. This fragrance is people's first impression of the fragrance, so it is very important. 2. Make the fragrance light, fresh and lively: Top notes have a strong fragrance diffusion power, which can make the fragrance of the fragrance appear light, fresh and lively. This characteristic makes the fragrance give people a pleasant feeling at the beginning of use. 3. Balance the fragrance: Top notes can also conceal the depressed part of the base fragrance and body fragrance, and achieve a good fragrance balance. This means that the top notes not only determine the initial fragrance of the fragrance, but also enhance the coordination and durability of the overall fragrance through interaction with other fragrances. 4. Enhance the charm of the fragrance: Commonly used top notes such as leaf alcohol, ethyl cyclohexylcarboxylate, melon aldehyde, octanal, nonanal and other advanced fatty aldehydes and citrus fragrances can change the style of the fragrance and add a new charm. This diversity and complexity makes the fragrance more attractive. Therefore, it is particularly important to control the volatility of the fragrance by using a carrier. The volatility of the top note is large, which determines the image and freshness of the fragrance; the volatility of the body note is moderate, which gives the fragrance a characteristic aroma; the base note provides a lasting aroma. Therefore, a suitable carrier is needed to slowly release and control the volatility of these spices, especially the top note, to achieve a balanced overall aroma ratio and maintain freshness.

[0004] The method of slow release of top fragrance is mainly achieved by two methods: 1. It is achieved by microencapsulation technology, which can effectively slow down the volatilization rate of fragrance, thereby extending the duration of fragrance. Specifically, microencapsulation technology includes two main preparation methods: physical method and chemical method. 2. It is achieved by synthesizing latent fragrance body. The research progress of latent fragrance molecules mainly focuses on linking fragrance molecules with specific groups by chemical bonding means to form a system that can control the breaking of chemical bonds under specific conditions to release fragrance. This latent fragrance body can effectively avoid the problem of short fragrance retention time caused by the high volatility of the fragrance itself, and meet the requirements of long-lasting fragrance retention of many fragrance products. In terms of controlling the release rate, innovation is mainly reflected in the design and optimization of chemical bonds. By selecting groups that are sensitive to acidic environments, ultraviolet rays, air or enzymes, the breaking of chemical bonds can be triggered under specific external conditions, thereby achieving precise control of the release rate of fragrance. This design not only improves the utilization rate of fragrance, but also enhances the product experience, so that the fragrance product can quickly release fragrance when needed, and remain stable when not needed, avoiding the waste and inconvenience caused by excessive volatilization.

[0005] However, microencapsulation technology has the following problems: 1. High preparation cost, complex process, long cycle, and difficulty in large-scale industrial production; 2. The wall material is non-degradable, highly toxic, and has poor environmental compatibility; 3. It is difficult to achieve controlled release of the capsule core at a specific time and space; 4. The loading capacity is small, and the encapsulation rate and drug loading amount need to be improved.

[0006] However, the synthesis and design of latent fragrance molecules are relatively complex and expensive, the release mechanism is generally complicated, and toxicological research needs to be further studied. Summary of the invention

[0007] To solve the problems of the prior art, a suitable carrier is needed for the sustained release of top notes. Aerogel itself is a solid material composed of a nano-scale porous structure with extremely low density and high porosity. The main characteristics of aerogel include high hydrophobicity, high specific surface area, low thermal conductivity, high porosity and good thermal insulation performance. These advantages make aerogel suitable as a sustained release carrier for fragrance molecules, especially top notes. Therefore, the present invention provides a trimethylsilyl modified aerogel loaded with top notes fragrance.

[0008] The specific technical solutions of the present invention are as follows:

[0009] The trimethylsilyl modified aerogel-loaded fragrance provided by the present invention is characterized in that the fragrance uses the trimethylsilyl modified aerogel as a carrier to adsorb at least the top fragrance.

[0010] The trimethylsilyl modified aerogel-loaded aromatherapy provided by the present invention also has the following technical characteristics, wherein the top note fragrance is at least one of leaf alcohol, ethyl cyclohexylcarboxylate, melon aldehyde, isoamyl acetate, octanal or nonanal.

[0011] The trimethylsilyl modified aerogel-loaded fragrance provided by the present invention also has the following technical features, wherein the preparation method of the trimethylsilyl modified aerogel comprises the following steps: step S1, mixing a silicon source, a solvent 1 and water for hydrolysis reaction to obtain a hydrolysis solution; step S2, adjusting the pH to make the hydrolysis solution gel, heat-drying and curing the gel to obtain a gel after heat-drying and curing; step S3, mixing the solvent 2 and the modifier evenly to obtain a modified liquid, immersing the gel after heat-drying and curing in the modified liquid, heat-drying and curing again, to obtain a gel after heat-drying and curing again; step S4, supercritical CO 2 The gel is extracted and heat-dried and cured again to obtain trimethylsilyl-modified aerogel.

[0012] The trimethylsilyl modified aerogel-loaded aromatherapy with top fragrance provided by the present invention also has the following technical features: the silicon source in step S1 is methyl orthosilicate or ethyl orthosilicate; the solvent 1 is methanol or ethanol; the temperature of the hydrolysis reaction is 50-70°C, the pH is 1.0-3.0, and the time is 6-10h; the mass ratio of the silicon source, the solvent 1 and water is 1:(4-6):(0.1-0.3).

[0013] The trimethylsilyl modified aerogel-loaded aromatherapy with top fragrance provided by the present invention also has the following technical features: wherein, in step S2, the pH is adjusted to 7.5-8.5; the temperature of the heat drying curing is 60-80° C., and the time is 6-12 hours.

[0014] The trimethylsilyl modified aerogel-loaded aromatherapy with top fragrance provided by the present invention also has the following technical features: in step S3, the solvent 2 is one or more of acetone, ethanol, n-hexane and n-heptane; the modifier is hexamethyldisilazane, trimethylchlorosilane or triphenylchlorosilane; the mass ratio of the solvent 2 to the modifier is (8-20):1; the temperature of the second heat drying and curing is 60-80°C, and the time is 6-12h.

[0015] The trimethylsilyl modified aerogel-loaded aromatherapy of top fragrance provided by the present invention also has the following technical features: wherein in step S4, supercritical CO 2 The extraction stage temperature is 50-70℃, the extraction stage pressure is 10-15MPa, the separation stage temperature is 35-60℃, the separation stage pressure is 4.5-5.5MPa, and the supercritical CO 2 The extraction time is 6-12h.

[0016] The trimethylsilyl modified aerogel-loaded aromatherapy for head fragrance provided by the present invention also has the following technical features: the density of the trimethylsilyl modified aerogel is 0.050-0.165 g / cm 3 .

[0017] The trimethylsilyl modified aerogel-loaded aromatherapy fragrance provided by the present invention also has the following technical characteristics: the adsorption is saturated adsorption.

[0018] The trimethylsilyl modified aerogel-loaded aromatherapy fragrance provided by the present invention also has the following technical features: the trimethylsilyl modified aerogel is in the form of blocks, particles or powders.

[0019] Functions and Effects of the Invention

[0020] The fragrance of top notes lasts for a short time, and aldehyde top notes are easily oxidized and deteriorated. The aromatherapy of the present invention uses trimethylsilyl modified aerogel to load at least the top notes, which greatly prolongs the fragrance of the top notes, balances the overall fragrance ratio of the aromatherapy and maintains the freshness, while also protecting the aldehyde top notes so that they are not easily oxidized and deteriorated.

[0021] The aromatherapy of the present invention can adjust the saturated adsorption capacity of the trimethylsilyl modified aerogel by adjusting its density (its saturated adsorption capacity can reach 5-20 times the weight of the aerogel), and then adjust the release of the top notes in the aromatherapy to achieve the optimal ratio of the overall aroma of the aromatherapy. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is the GC graph of Aromatherapy 28 after 0.5 h in Example 8 of the present invention.

[0023] Figure 2 It is the GC chart of essential oil 27 after 0.5h in Example 8 of the present invention.

[0024] Figure 3 This is the GC graph of Aromatherapy 28 after 1 hour in Example 8 of the present invention.

[0025] Figure 4 This is the GC chart of essential oil 27 after 1 hour in Example 8 of the present invention. DETAILED DESCRIPTION

[0026] The terms used in the present invention, unless otherwise specified, generally have the meanings that are commonly understood by those of ordinary skill in the art.

[0027] In the following examples, various processes and methods not described in detail are conventional methods well known in the art.

[0028] The reagents used in the following examples were purchased from common commercial sources, and the experimental operations and experimental conditions not specified were referred to the conventional operations and conventional conditions in the art.

[0029] The specific implementation of the present invention is described below in conjunction with embodiments and drawings.

[0030] <Example 1>

[0031] This embodiment provides a method for preparing trimethylsilyl modified aerogel, and the preparation steps are as follows:

[0032] Step S1, mixing the silicon source, solvent 1 and water for hydrolysis reaction to obtain a hydrolysis solution. The specific process is:

[0033] Tetraethyl orthosilicate, ethanol and water were mixed in a mass ratio of 1:5:0.2, and hydrolysis reaction was carried out at 60° C. and pH 2.0 for 8 hours to obtain a hydrolysis solution.

[0034] Step S2, adjusting the pH to make the hydrolyzed solution gel, and heat-drying and curing the gel to obtain a heat-drying and curing gel.

[0035] The specific process is:

[0036] The pH of the hydrolyzed solution was adjusted to 7.6, and the solution was injected into a mold to gel. After gelation, the solution was placed in a 70° C. oven for curing for 12 hours to obtain a gel block after heat curing.

[0037] Step S3, the solvent 2 and the modifier are mixed evenly to obtain a modified liquid, the gel after heat curing is immersed in the modified liquid, and heat-cured again to obtain a gel after heat curing again. The specific process is:

[0038] The solvent 2 (a mixture of acetone and ethanol, with a mixing mass ratio of 2:1) and the modifier hexamethyldisilazane are uniformly mixed in a mass ratio of 10:1 to obtain a modified solution, and the gel block after heat curing obtained in step S2 is immersed in the modified solution and placed in an oven at 70°C for curing for 12 hours to obtain a gel block after heat curing again.

[0039] Step S4, supercritical CO 2 The gel after extraction and heat drying is then cured to obtain trimethylsilyl modified aerogel. The specific process is as follows:

[0040] Take out the gel block after heat drying and put it into supercritical CO 2 The extraction reactor was set to an extraction stage temperature of 55°C, an extraction stage pressure of 10 MPa, a separation stage temperature of 45°C, a separation stage pressure of 5.5 MPa, and extraction for 6 hours to obtain trimethylsilyl-modified aerogel blocks.

[0041] In this embodiment, the density of the trimethylsilyl modified aerogel is adjusted by adjusting the mass ratio of the silicon source, solvent 1 and water in step S1; ethylene glycol is added in step S1 to adjust the pore size distribution of the trimethylsilyl modified aerogel, and the mass of ethylene glycol is 0.5, 1, 1.25, 1.5, 2, and 2.25 times that of the silicon source. Through adjustment, this embodiment also obtains a density range of 0.062-0.153 g / cm 3 Trimethylsilyl-modified aerogel blocks.

[0042] The present invention can adjust the density of trimethylsilyl modified aerogel to 0.050-0.165g / cm 3 , so that its saturated adsorption capacity reaches 5-20 times the weight of the aerogel. The density of trimethylsilyl modified aerogel is basically inversely proportional to its adsorption capacity.

[0043] Therefore, for aromatherapy using trimethylsilyl modified aerogel as a carrier, when the adsorption capacity of aerogel needs to be enhanced, the density of aerogel can be reduced to increase its saturated adsorption capacity. When the adsorption capacity of aerogel needs to be weakened, the density of aerogel can be increased to reduce its saturated adsorption capacity.

[0044] <Example 2>

[0045] In this example, trimethylsilyl modified aerogel blocks of different densities prepared in Example 1 were used to saturate the adsorption of geraniol to prepare aromatherapy 1-5, and the desorption / volatilization test of geraniol was carried out on the aromatherapy 1-5.

[0046] The trimethylsilyl-modified aerogel blocks of different densities prepared in Example 1 were used to carry out saturated adsorption of leaf alcohol. The trimethylsilyl-modified aerogel blocks of different densities were taken for adsorption test, and the corresponding relationship between the density of the trimethylsilyl-modified aerogel and its saturated adsorption amount was obtained, which is listed in Table 1.

[0047] The adsorption test method is: use a 30mL transparent wide-mouth glass sample bottle as a container, drop an excess of essential oil onto about 0.2-0.6g accurately weighed trimethylsilyl modified aerogel (accurate to one ten-thousandth of a gram), adsorb for 24 hours, remove the residual essential oil droplets that cannot be adsorbed with a pipette and capillary, accurately weigh the weight of essential oil adsorbed on trimethylsilyl modified aerogel (accurate to one ten-thousandth of a gram), and calculate the saturated adsorption amount. The saturated adsorption amount of trimethylsilyl modified aerogel is calculated as: saturated adsorption amount = saturated adsorption essential oil mass / 100g aerogel mass. The essential oil tested in this test is leaf alcohol.

[0048] Table 1

[0049] Aromatherapy 1 2 3 4 5 Carrier Aerogel E Aerogel A Aerogel K Aerogel J Aerogel B Ethylene glycol:ethyl orthosilicate 2 1.5 1.25 1 0.5 <![CDATA[Density (g / cm 3 )]]> 0.062 0.092 0.122 0.141 0.153 Aerogel(g) 0.3017 0.5963 0.2986 0.3748 0.5923 Saturated adsorption of leaf alcohol (g) 4.3178 6.0444 2.4486 2.3581 3.7315 Saturated adsorption capacity (g / 100g) 1431 1014 820 629 630

[0050] Further, about 2g of the above-mentioned No. 1-5 aromatherapy and 1.9184g of No. 6 leaf alcohol control sample were taken for desorption / volatilization test. The specific method is: the container containing the aromatherapy or control sample (30mL transparent large-mouth glass sample bottle) is placed in a fume hood with the mouth open, and the volatility of leaf alcohol at different times is calculated. Volatility rate = volatilized essential oil mass / saturated adsorption or total mass of added essential oil × 100%. On the 9th day, the geraniol in the No. 1-5 aromatherapy was basically volatilized (volatilization rate 96-100%). The saturated adsorption amount of the aerogel for leaf alcohol at this time was tested according to the above-mentioned adsorption test method. The saturated adsorption amount on the 10th day was obtained by 24h saturated adsorption. The results are listed in Table 2.

[0051] Table 2

[0052]

[0053] First, for the control sample No. 6 (leaf alcohol without trimethylsilyl modified aerogel loading), about 2g of leaf alcohol was added to a 30mL transparent wide-mouthed glass sample bottle and evaporated at a constant rate of 2.86% per hour, and the volatilization was completed in 35 hours. After accumulation, the contact area with the air is not as large as that on the fragrance paper, so it cannot be completely evaporated within 4 hours like ordinary top note molecules, but the same container was used as the fragrance 1-5 during the test, so it can be used as a control sample.

[0054] As shown in Table 2, the density of trimethylsilyl modified aerogel in aromatherapy No. 1 to No. 5 gradually increases, and the volatilization rate of leaf alcohol in aromatherapy increases successively. The volatilization rate of leaf alcohol in aromatherapy using trimethylsilyl modified aerogel is lower than that of leaf alcohol without carrier (the volatilization rate of leaf alcohol in aromatherapy No. 5 is 12% in 3h, which is greater than that of leaf alcohol without carrier in No. 6 in 3h, because aerogel B is seriously broken into particles from blocks, and its contact area with air is larger, and its specific surface area is larger than that of leaf alcohol without carrier, so it is easier to volatilize at the beginning, but after volatilization to a certain extent, due to the adsorption and sustained release effect of aerogel, the volatilization becomes slower and slower, and the subsequent leaf alcohol volatilization rate in aromatherapy No. 5 is lower than that of leaf alcohol without carrier), indicating that trimethylsilyl modified aerogel has a sustained release effect on geraniol; the time for leaf alcohol in aromatherapy No. 1-5 to completely volatilize is much longer than 35 hours. It shows that trimethylsilyl modified aerogel has a good sustained release effect on the head fragrance molecule leaf alcohol.

[0055] On the 9th day, the geraniol in the fragrance No. 1-5 was basically volatilized (volatilization rate 96-100%), and the saturated adsorption of geraniol by trimethylsilyl modified aerogel was tested again. The saturated adsorption amount on the 10th day obtained by 24h saturated adsorption was basically consistent with the first saturated adsorption amount. This shows that the trimethylsilyl modified aerogel can be recycled and reused, which improves the utilization rate of the trimethylsilyl modified aerogel for the sustained release of geraniol molecules.

[0056] <Example 3>

[0057] In this example, trimethylsilyl-modified aerogel blocks with different densities prepared in Example 1 were used to saturate-adsorb ethyl cyclohexanecarboxylate, the top note fragrance, to prepare aromatherapy products 7 - 9, and desorption / volatilization tests of the top note ethyl cyclohexanecarboxylate were carried out on them.

[0058] The methods for saturated adsorption and desorption / volatilization tests were carried out according to the corresponding methods of Example 2. The results are listed in Table 3.

[0059] Table 3

[0060]

[0061]

[0062] First, for the control sample No. 10 (ethyl cyclohexanecarboxylate not supported by trimethylsilyl-modified aerogel), about 2 g of ethyl cyclohexanecarboxylate was added to a 30 mL transparent wide-mouth glass sample bottle and volatilized at a uniform rate of 1.25% per hour. The volatilization was completed in 80 hours. After stacking, the contact area with air was not as large as that on the perfuming paper, so it could not volatilize completely within 4 hours like ordinary top note molecules. However, the same container as that used for aromatherapy products 7 - 9 was used during the test, so it could be used as a control sample.

[0063] As can be seen from Table 3, the density of the trimethylsilyl-modified aerogel in aromatherapy products from No. 7 to No. 9 gradually decreases, and the saturated adsorption amount increases in turn. The volatilization rate of ethyl cyclohexanecarboxylate in the aromatherapy products with trimethylsilyl-modified aerogel is lower than that of ethyl cyclohexanecarboxylate without a carrier, indicating that the trimethylsilyl-modified aerogel has a slow-release effect on the top note ethyl cyclohexanecarboxylate. The time for the complete volatilization of ethyl cyclohexanecarboxylate in aromatherapy products 7 - 9 is much longer than 80 hours, indicating that the trimethylsilyl-modified aerogel has a good slow-release effect on the top note molecule ethyl cyclohexanecarboxylate.

[0064] <Example 4>

[0065] In this example, trimethylsilyl-modified aerogel blocks with different densities prepared in Example 1 were used to saturate-adsorb melonal, the top note fragrance, to prepare aromatherapy products 11 - 13, and desorption / volatilization tests of the top note melonal were carried out on them.

[0066] The methods for saturated adsorption and desorption / volatilization tests were carried out according to the corresponding methods of Example 2. The results are listed in Table 4.

[0067] Table 4

[0068]

[0069]

[0070] First, for control sample No. 14 (melon aldehyde without trimethylsilyl modified aerogel loading), about 2g of melon aldehyde was added to a 30mL transparent wide-mouthed glass sample bottle and evaporated at a constant rate of 1.4% per hour, and the volatilization was completed in 72 hours. After accumulation, the contact area with the air is not as large as that on the fragrance paper, so it cannot be completely evaporated within 4 hours like ordinary top note molecules, but the same container was used as the fragrance 11-13 during the test, so it can be used as a control sample.

[0071] As shown in Table 4, the density of trimethylsilyl modified aerogel in aromatherapy No. 11 to No. 13 gradually decreases, and the saturated adsorption amount increases successively. The volatilization rate of melon aldehyde in aromatherapy using trimethylsilyl modified aerogel is lower than that of melon aldehyde without carrier, indicating that trimethylsilyl modified aerogel has a sustained release effect on the first fragrance melon aldehyde. After 5 days, the melon aldehyde in aromatherapy No. 11-13 volatilized only about 50%, and the time for the melon aldehyde in aromatherapy No. 11-13 to completely volatilize was much longer than 72 hours, indicating that trimethylsilyl modified aerogel has a good sustained release effect on the first fragrance molecule melon aldehyde.

[0072] <Example 5>

[0073] In this example, trimethylsilyl modified aerogel blocks of different densities prepared in Example 1 were used to saturate adsorb isoamyl ethyl acetate to prepare aromatherapy 15-17, and desorption / volatilization tests of isoamyl ethyl acetate were performed on them.

[0074] The saturated adsorption and desorption / volatilization test methods were carried out according to the corresponding methods of Example 2. The results are listed in Table 5.

[0075] Table 5

[0076]

[0077]

[0078] First, for control sample No. 18 (isoamyl acetate without trimethylsilyl modified aerogel loading), about 2g of isoamyl acetate was added to a 30mL transparent wide-mouthed glass sample bottle and evaporated at a constant rate of 2.5% per hour, and the volatilization was completed in 40 hours. After accumulation, the contact area with the air is not as large as that on the fragrance paper, so it cannot be completely evaporated within 4 hours like ordinary top note molecules, but the same container was used as the fragrance 15-17 during the test, so it can be used as a control sample.

[0079] As shown in Table 5, the density of trimethylsilyl modified aerogel in aromatherapy No. 15 to No. 17 gradually decreases, and the saturated adsorption amount increases successively. The volatilization rate of isoamyl acetate in aromatherapy using trimethylsilyl modified aerogel is lower than that of isoamyl acetate without carrier, indicating that trimethylsilyl modified aerogel has a sustained release effect on isoamyl acetate of head fragrance. It took 2 days for the isoamyl acetate in aromatherapy No. 15-17 to completely volatilize, which also shows that trimethylsilyl modified aerogel has a sustained release effect on isoamyl acetate of head fragrance molecule.

[0080] <Example 6>

[0081] In this example, trimethylsilyl modified aerogel blocks of different densities prepared in Example 1 were used to saturately adsorb caprylic aldehyde to prepare aromatherapy 19-21, and the desorption / volatilization test of caprylic aldehyde was carried out on the aerogels.

[0082] The saturated adsorption and desorption / volatilization test methods were carried out according to the corresponding methods of Example 2. The results are listed in Table 6.

[0083] Table 6

[0084]

[0085]

[0086] First, for the control sample No. 22 (octanal without trimethylsilyl modified aerogel loading), about 2g of octanal was added to a 30mL transparent wide-mouthed glass sample bottle and evaporated at a constant rate of 0.49% per hour. After accumulation, the contact area with the air is not as large as that on the fragrance paper, so it cannot be completely evaporated within 4 hours like ordinary top note molecules, but the same container was used as the fragrance 19-21 during the test, so it can be used as a control sample.

[0087] It can be seen from Table 6 that the density of trimethylsilyl modified aerogel in aromatherapy No. 19 to No. 21 gradually decreases, and the saturated adsorption capacity increases successively. The volatility of octanal in aromatherapy using trimethylsilyl modified aerogel is lower than that of octanal without carrier, indicating that trimethylsilyl modified aerogel has a sustained release effect on octanal.

[0088] <Example 7>

[0089] In this example, trimethylsilyl modified aerogel blocks of different densities prepared in Example 1 were used to saturately adsorb nonanal to prepare aromatherapy 23-25, and desorption / volatilization tests of nonanal were performed on them.

[0090] The saturated adsorption and desorption / volatilization test methods were carried out according to the corresponding methods of Example 2. The results are listed in Table 7.

[0091] Table 7

[0092]

[0093] First, for the control sample No. 26 (nonanal without trimethylsilyl modified aerogel loading), about 2g of nonanal was added to a 30mL transparent wide-mouthed glass sample bottle and volatilized at a constant rate of 0.13% per hour. After accumulation, the contact area with the air is not as large as that on the fragrance paper, so it cannot be completely volatilized within 4 hours like ordinary top note molecules, but the same container was used as the fragrance 23-25 ​​during the test, so it can be used as a control sample.

[0094] It can be seen from Table 7 that the density of trimethylsilyl modified aerogel in aromatherapy No. 23 to No. 25 gradually decreases, and the saturated adsorption capacity increases successively. The volatility of nonanal in aromatherapy using trimethylsilyl modified aerogel is lower than that of nonanal without carrier, indicating that trimethylsilyl modified aerogel has a sustained release effect on nonanal.

[0095] <Example 8>

[0096] In this embodiment, leaf alcohol, citral and 2-methylundecane were mixed in a mass ratio of 1:1:1 to obtain essential oil 27, and trimethylsilyl-modified aerogel was used to saturate adsorb the essential oil 27, with a saturated adsorption amount (670 g / 100 g) to obtain aromatherapy 28. The sustained release effect of trimethylsilyl-modified aerogel on the head fragrance molecule leaf alcohol in aromatherapy 28 was tested by a third-party test (Beijing Zhongke Optical Analysis Science and Technology Institute).

[0097] The test method is as follows: take 1g of aromatherapy 28 and 1g of essential oil 27 as the control sample, heat them to 70℃ for rotary evaporation under 0.1mbar oil pump vacuum, and weigh them to calculate the desorption rate after 0.5h.

[0098] Desorption rate = (mass of aromatherapy or essential oil before desorption - mass of aromatherapy or essential oil after desorption) / mass of aromatherapy or essential oil before desorption × 100%.

[0099] The test results are: after 0.5h, the desorption rate of aromatherapy 28 is 8.82%; the desorption rate of essential oil 27 is 12.98%. At the same time, samples were taken for GC analysis. The GC graph of aromatherapy 28 is as follows: Figure 1 As shown, the GC profile of essential oil 27 is as follows Figure 2 shown.

[0100] From the desorption rate, it can be concluded that the essential oil 27 (12.98%) is greater than the aromatherapy 28 (8.82%), indicating that the carrier trimethylsilyl modified aerogel has a sustained release effect. Figure 1 , 2 By comparison, the proportion of geraniol in essential oil 27 (26.23%) is less than that in aromatherapy 28 (26.92%), indicating that trimethylsilyl-modified aerogel has a sustained-release effect on geraniol.

[0101] Then the desorption was continued. After 1 hour, the desorption rate of aromatherapy 28 was 15.9%; the desorption rate of essential oil 27 was 24.11%. At the same time, samples were taken for GC analysis. The GC graph of aromatherapy 28 is shown in Figure 3 As shown, the GC profile of essential oil 27 is as follows Figure 4 shown.

[0102] From the desorption rate, it can be concluded that the essential oil 27 (24.11%) is greater than the aromatherapy 28 (15.9%), indicating that the carrier trimethylsilyl modified aerogel has a sustained release effect. Figure 3 , 4 By comparison, the proportion of geraniol in essential oil 27 (15.97%) is less than that in aromatherapy 28 (20.42%), indicating that trimethylsilyl-modified aerogel has an obvious sustained-release effect on geraniol.

[0103] The above is a detailed description of the embodiments, which is convenient for those skilled in the art to correctly understand and use the present invention. Any improvements or modifications to the technical solutions obtained by those skilled in the art based on the present invention on the basis of the prior art, without innovative work, only through analysis, analogy or limited enumeration, etc., should be within the scope of protection determined by the claims.

Claims

1. A trimethylsilyl modified aerogel loaded with top fragrance aromatherapy, characterized in that: The aromatherapy uses trimethylsilyl modified aerogel as a carrier to absorb at least the top fragrance.

2. The aromatherapy according to claim 1, characterized in that: in, The top fragrance is at least one of leaf alcohol, ethyl cyclohexylcarboxylate, melonal, isoamyl acetate, octanal or nonanal.

3. The aromatherapy according to claim 1, It is characterized in that The preparation method of the trimethylsilyl modified aerogel comprises the following steps: Step S1, mixing a silicon source, a solvent 1 and water to perform a hydrolysis reaction to obtain a hydrolysis solution; Step S2, adjusting the pH to make the hydrolysis solution gel, and heat-drying and curing the gel to obtain a heat-drying and curing gel; Step S3, uniformly mixing the solvent 2 and the modifier to obtain a modified liquid, immersing the heat-cured gel in the modified liquid, and heat-curing again to obtain a heat-cured gel; Step S4, extracting the gel after heat drying and curing again with supercritical CO2 to obtain the trimethylsilyl modified aerogel.

4. The aromatherapy according to claim 3, characterized in that: in, The silicon source in step S1 is methyl orthosilicate or ethyl orthosilicate; The solvent 1 is methanol or ethanol; The hydrolysis reaction temperature is 50-70°C, the pH is 1.0-3.0, and the time is 6-10h; The mass ratio of the silicon source, the solvent 1 and the water is 1:(4-6):(0.1-0.3).

5. The aromatherapy according to claim 3, characterized in that: in, The step S2 wherein the pH is adjusted to 7.5-8.5; The temperature of the heat baking curing is 60-80°C and the time is 6-12h.

6. The aromatherapy according to claim 3, characterized in that: in, In step S3, the solvent 2 is one or more of acetone, ethanol, n-hexane and n-heptane; The modifier is hexamethyldisilazane, trimethylchlorosilane or triphenylchlorosilane; The mass ratio of the solvent 2 to the modifier is (8-20):1; The temperature of the second heat drying and curing is 60-80°C and the time is 6-12h.

7. The aromatherapy according to claim 3, characterized in that: in, The extraction stage temperature of the supercritical CO2 extraction in step S4 is 50-70°C, the extraction stage pressure is 10-15MPa, the separation stage temperature is 35-60°C, the separation stage pressure is 4.5-5.5MPa, and the supercritical CO2 extraction time is 6-12h.

8. The aromatherapy according to claim 1, characterized in that: in, The density of the trimethylsilyl modified aerogel is 0.050-0.165 g / cm 3 .

9. The aromatherapy according to claim 1, characterized in that: in, The adsorption is saturated adsorption.

10. The aromatherapy according to claim 1, characterized in that: in, The trimethylsilyl modified aerogel is in the form of blocks, particles or powders.

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