Fluorosiloxane hydrophobic modified blended fragrance product and preparation method thereof

Abstract

The invention discloses a preparation method of a fluorosiloxane hydrophobic modified blended fragrant product, which comprises the following steps: 1) mixing fragrant powder in proportion, soaking the mixed fragrant powder in a fluorosiloxane solution, filtering and drying the fragrant powder; (2) grinding and sieving the modified spice powder, mixing with the sticky powder and the water according to a certain ratio, repeatedly plastifying into uniform mud by using an open mill, and fermenting the mud for later use; (3) pressing the fermented fragrant mud into sheets through an open mill, compacting the sheets in a mold, drawing the mold, and scraping off redundant parts; (4) putting the demolded blended fragrant product in a dark, dry and ventilated place for drying in the shade; and 5) grinding, polishing and oiling to obtain the hydrophobic modified blended perfume. According to the invention, a low-surface-energy fluorine element is introduced into the surface of the blended incense by utilizing a chemical coupling reaction between the fluorosiloxane / coupling agent and the incense powder, so that the hydrophobicity of the blended incense is improved, the hydrophobic effect of the blended incense is remarkably improved, the problem that the blended incense is sticky and greasy in hand feeling caused by an additive type hydrophobic agent is avoided, and the service life of the blended incense is prolonged. The method is suitable for moisture-proof and mildew-proof treatment of high-value synthetic aromatic beads.

Description

Technical Field

[0001] The present invention belongs to the technical field of compound incense processing, and particularly relates to a fluorosiloxane hydrophobic modified compound incense product and a preparation method thereof. Background Art

[0002] Compound incense products include compound incense beads, compound incense tablets, compound incense thumb rings, compound incense ornaments, etc. These compound incense products have similar raw materials and processes. Besides being fragrant and wonderful objects that can be worn and played with, they can also have effects such as calming the mind, regulating qi in the middle energizer, and health care and nourishment. They have gradually become popular since the Ming and Qing dynasties. "The Book of Incense" records various incense formulas, and many current incense culture enthusiasts are also keen on researching and making compound incense products for wearing and playing with.

[0003] However, the current compound incense products basically follow the ancient incense formulas and processes. The main innovations mainly focus on changing the incense formulas, as well as the components and contents of the incense powder. For example, a traditional Chinese medicine health care compound incense bead and its preparation method disclosed in Patent CN107960709A, or adding fashionable design elements to the appearance of the compound incense product; such as the compound incense bead pendant disclosed in Patent CN305574192S. However, since compound incense products are mainly used for wearing and playing with, they are inevitably in contact with water during activities such as washing hands and exercising in daily life. And the incense powder that makes up the compound incense product will dissolve when encountering water, which to a certain extent restricts the popularization and use of compound incense products.

[0004] To address the problem that compound incense products dissolve when encountering water, the current main method is to improve their hydrophobicity. For example, Patent No. CN119587498A discloses a waterproof traditional Chinese medicine compound incense bead and its preparation method. By adding fluorinated surfactants such as perfluorobutylethyl octadecylcarbamate, it can significantly improve the hydrophobic performance of the compound incense bead compared to paraffin wax, etc. However, as an additive hydrophobic agent, although it migrates to the surface to form a protective layer during the process of making the compound incense bead, thus achieving a hydrophobic effect, it is also easy to transfer to the human hand when playing with it, bringing a sticky and unpleasant touch. For people with sensitive skin, there is a possibility of irritation, which affects the popularization and use of compound incense products. Summary of the Invention

[0005] The present invention aims to at least partly solve one of the technical problems in the related technologies. Therefore, the main purpose of the present invention is to provide a fluorosiloxane hydrophobic modified compound incense product with good hydrophobicity and no sticky feeling and a preparation method thereof.

[0006] The object of the present invention is achieved by the following technical solutions:

[0007] A preparation method of a fluorosiloxane hydrophobic modified compound incense product, comprising the following steps:

[0008] 1) Mix the incense powder in proportion and soak it in a fluorosiloxane solution, filter and dry the incense powder to obtain modified incense powder;

[0009] 2) Grind the modified incense powder, sieve it, then mix it proportionally with adhesive powder and water, and repeatedly knead it until it becomes a uniform mud shape by an open mill. Wrap it with plastic wrap and let it rest in a cool place for later use;

[0010] 3) Press the rested incense mud into sheets by an open mill, put it into a mold and compact it, then remove the mold and scrape off the excess part;

[0011] 4) Place the demolded combined incense product in a dark, dry and ventilated place to dry in the shade;

[0012] 5) Polish, buff and oil the dried combined incense product to obtain a hydrophobic modified combined incense product.

[0013] In some specific embodiments, the incense powder described in step 1) is at least one of jasmine pollen, osmanthus powder, Hainan agarwood powder, mint powder, rose roselle pollen, agastache powder, sandalwood powder, and dalbergia odorifera powder.

[0014] In some specific embodiments, the fluorosiloxane solution described in step 1) is obtained by stirring and hydrolyzing 20 - 40% by volume of heptadecafluorodecyltrimethoxysilane, 1 - 2% of aminopropyltriethoxysilane, and 60 - 80% of 50 wt% alcohol at room temperature for 2 - 6 h.

[0015] In some specific embodiments, the soaking time described in step 1) is 12 - 24 h.

[0016] In some specific embodiments, the drying process parameters described in step 1) are: the drying temperature is 80 - 100 °C, and the drying time is 2 - 4 h.

[0017] In some specific embodiments, the mass ratio of the adhesive powder, incense powder and water described in step 2) is 1:(2 - 3):(3 - 4).

[0018] In some specific embodiments, the mesh number of the sieving described in step 2) is 50 - 120 meshes.

[0019] As the same inventive concept, the present application also provides a fluorosiloxane hydrophobic modified combined incense product.

[0020] Compared with the prior art, the present invention has at least the following advantages:

[0021] The preparation method of the fluorosiloxane hydrophobic modified combined incense product provided by the present invention introduces low surface energy fluorine elements onto the surface of the combined incense product by utilizing the chemical coupling reaction of fluorosiloxane / coupling agent and incense powder, thereby improving the hydrophobicity of the combined incense product, significantly improving its hydrophobic effect, and avoiding the problem of sticky feel of the combined incense product caused by additive hydrophobic agents, and is applicable to the moisture-proof and mildew-proof treatment of high-value combined incense beads. Description of the Drawings

[0022] To more clearly illustrate the specific embodiments of the present invention, the following will briefly introduce the drawings required for use in the description of the specific embodiments or the prior art.

[0023] Figure 1 Physical diagram of the water contact angle and hydrophobic effect of the combined incense product of Example 2 (bottom) and Comparative Example 2 (top) of the present invention;

[0024] Figure 2 Physical diagram of the effect of the combined incense product of Example 2 (right) and Comparative Example 2 (left) of the present invention after being soaked in water for 1 h;

[0025] Figure 3 Physical diagram of the surface greasiness effect of the combined incense product of the embodiment (right) and Comparative Example 3 (left) of the present invention. Specific embodiments

[0026] The present invention will be further described in detail below in conjunction with the drawings and embodiments. The following embodiments are only descriptive and not restrictive, and the protection scope of the present invention cannot be limited thereby.

[0027] When expressing a certain quantity, concentration or other value or parameter in the form of a range, a preferred range, or a preferred upper and lower limit of a value, it should be understood that any range obtained by combining any upper limit of the range or a preferred value with any lower limit of the range or a preferred value is specifically disclosed, regardless of whether the range is specifically disclosed. Unless otherwise indicated, the numerical range values listed herein include the endpoints of the range and all integers and fractions within the range.

[0028] Unless otherwise specified, all percentages, parts, ratios, etc. in this article are by weight.

[0029] The materials, methods and embodiments in this article are all exemplary and should not be construed as restrictive unless otherwise specified.

[0030] In the following embodiments, the incense powder used is at least one of jasmine pollen, osmanthus powder, Hainan agarwood powder, mint powder, rose roxburghii tratt pollen, agastache powder, sandalwood powder, and dalbergia odorifera powder. In this application, jasmine pollen (Jasmine Pillow Cold Jade) is taken as an example, and its formula is as follows: in parts by weight, it includes 6.5 parts of jasmine pollen, 1 part of osmanthus powder, 0.5 part of Hainan agarwood, 1 part of mint, 2 parts of rose roxburghii tratt pollen, 0.2 part of agastache. Jasmine pollen is fresh and elegant, which can soothe the mind. When used in combination with osmanthus powder and rose roxburghii tratt pollen, it emits a fragrance. Adding mint, agarwood, and agastache can improve concentration and clear the head.

[0031] In the following embodiments, the water contact angle of the combined incense product is measured according to GB / T 30693-2014.

[0032] Example 1

[0033] This example provides a preparation method of a fluorosiloxane hydrophobic modified compound incense product, which comprises the following steps:

[0034] 1) Mix 20% by volume of heptadecafluorodecyltrimethoxysilane, 1% of aminopropyltriethoxysilane and 79% of 50wt% alcohol by mass and stir for 4 h to prepare a fluorosiloxane solution;

[0035] 2) Immerse the incense powder mixed according to the formula of Jasmine Pillow Cold Jade in the fluorosiloxane solution for 12 h, filter, and dry at 80 °C for 4 h;

[0036] 2) Grind the dried incense powder through a 100-mesh sieve, take the mass ratio of adhesive powder: incense powder: water as 1:3:3, mix them, and repeatedly knead them into a uniform mud shape by an open mill, wrap them with plastic wrap and place them in a cool place to wake up the mud for standby;

[0037] 3) Press the woken incense mud into a sheet by an open mill, put it into a mold and compact it, take out the mold, and scrape off the excess part;

[0038] 4) Place the demolded compound incense product in a dark, dry and ventilated place for air drying;

[0039] 5) Grind, polish and oil the air-dried compound incense product to obtain a hydrophobic modified compound incense product; test its water contact angle to be 108°.

[0040] Example 2

[0041] This example provides a preparation method of a fluorosiloxane hydrophobic modified compound incense product, which comprises the following steps:

[0042] 1) Mix 40% by volume of heptadecafluorodecyltrimethoxysilane, 2% of aminopropyltriethoxysilane and 70% of 50wt% alcohol by mass and stir for 4 h to prepare a fluorosiloxane solution;

[0043] 2) Immerse the incense powder mixed according to the formula of Jasmine Pillow Cold Jade in the fluorosiloxane solution for 12 h, filter, and dry at 80 °C for 4 h;

[0044] 2) Grind the dried incense powder through a 100-mesh sieve, take the mass ratio of adhesive powder: incense powder: water as 1:3:3, mix them, and repeatedly knead them into a uniform mud shape by an open mill, wrap them with plastic wrap and place them in a cool place to wake up the mud for standby;

[0045] 3) Press the woken incense mud into a sheet by an open mill, put it into a mold and compact it, take out the mold, and scrape off the excess part;

[0046] 4) Place the demolded compound incense product in a dark, dry and ventilated place for air drying;

[0047] 5) Grind, polish, and oil the dried natural incense product to obtain a hydrophobic modified natural incense product; measure its water contact angle as shown in the Figure 1 lower left, which is 120°, and the actual hydrophobic effect of the natural incense product is as shown in the Figure 1 lower right.

[0048] Example 3

[0049] This example provides a method for preparing a fluorosiloxane hydrophobic modified natural incense product, which includes the following steps:

[0050] 1) Mix 40% (by volume) of heptadecafluorodecyltrimethoxysilane, 2% of aminopropyltriethoxysilane, and 70% of 50 wt% alcohol and stir for 4 h to prepare a fluorosiloxane solution;

[0051] 2) Immerse the incense powder mixed according to the formula of Jasmine Pillow Cold Jade in the fluorosiloxane solution for 24 h, filter, and dry at 80 °C for 4 h;

[0052] 2) Grind the dried incense powder through a 100-mesh sieve, take the mixture of adhesive powder: incense powder: water with a mass ratio of 1:3:3, and repeatedly knead it into a uniform mud shape with an open mill, wrap it with plastic wrap and place it in a cool place to let the mud rest for later use;

[0053] 3) Press the rested incense mud into sheets with an open mill, put it into a mold and compact it, remove the mold, and scrape off the excess part;

[0054] 4) Place the demolded natural incense product in a dark, dry, and ventilated place to dry in the air;

[0055] 5) Grind, polish, and oil the dried natural incense product to obtain a hydrophobic modified natural incense product; its water contact angle is 121°.

[0056] Comparative Example 1

[0057] This comparative example provides a method for preparing a fluorosiloxane hydrophobic modified natural incense product, which includes the following steps:

[0058] The method for preparing the natural incense product provided in this comparative example is basically the same as that in Example 2, except that the prepared siloxane solution does not contain aminopropyltriethoxysilane. Measure the water contact angle of the prepared natural incense product to be 98°.

[0059] Comparative Example 2

[0060] This comparative example provides a method for preparing a fluorosiloxane hydrophobic modified natural incense product, which includes the following steps:

[0061] The method for preparing the natural incense product provided in this comparative example is basically the same as that in Example 2, except that it does not include steps 1) and 2). Measure the water contact angle of the prepared natural incense product as shown in theFigure 1 As shown in the upper left, it is 62°, and the actual hydrophobic effect of the combined incense product is as attached Figure 1 As shown in the upper right.

[0062] Comparative Example 3

[0063] This comparative example provides a method for preparing a fluorosiloxane hydrophobic modified combined incense product, which includes the following steps:

[0064] 1) 100 g of incense powder prepared according to the proportion of the Jasmine Pillow Cold Jade Incense Recipe is mixed evenly with 20 g of perfluorobutylethyl octadecylcarbamate (additive hydrophobic agent);

[0065] 2) Grind through a 100-mesh sieve. At the same time, take the mass ratio of adhesive powder: incense powder: water as 1:3:3 and mix them. Then, knead them repeatedly with an open mill until they become a uniform mud shape. Wrap them with plastic wrap and place them in a cool place to let the mud rest for later use;

[0066] 3) Press the rested incense mud into sheets with an open mill, put them into a mold and compact them, remove the mold, and scrape off the excess part;

[0067] 4) Place the demolded combined incense product in a dark, dry, and ventilated place to air-dry;

[0068] 5) Grind and polish the air-dried combined incense product, and then place it in an oven and bake it at 60 °C for 12 hours to obtain a waterproof Chinese herbal medicine combined incense bead, whose water contact angle is 118°.

[0069] To sum up, after the incense powder is modified with a fluorosiloxane solution, the hydrophobic effect of the combined incense product is greatly improved. Compared with the combined incense product without fluorosiloxane modification (Comparative Example 2), the water contact angle of the combined incense bead prepared in Example 2 increases from 62° to 120°, achieving a good hydrophobic effect. To better compare the hydrophobic effects of combined incense products, the combined incense products prepared in Example 2 and Comparative Example 2 are placed in water and soaked for 1 h. The results are as attached Figure 2 As shown, the combined incense product of Comparative Example 2 gradually dissolves, and the water body changes color significantly, while the combined incense product of Example 2 remains basically unchanged and the water body does not change color. This result intuitively proves the excellent hydrophobic effect of the combined incense product of Example 2.

[0070] It can be seen from the comparison between Example 2 and Comparative Example 1 that the alkalinity of aminopropyltriethoxysilane itself is beneficial to the hydrolysis process of heptadecafluorodecyltrimethoxysilane, thereby promoting the modification of the incense powder. The addition of aminopropyltriethoxysilane can significantly enhance the hydrophobic modification effect of fluorosiloxane.

[0071] It can be seen from the comparison between Example 2 and Example 3 that if the soaking time of the incense powder in fluorosiloxane is further increased, it is beneficial to the graft modification of fluorine elements on the surface of the incense powder, and can further improve the hydrophobic modification effect of the combined incense product, but the cost performance is not high.

[0072] Meanwhile, by placing the combined incense products of Example 2 and Comparative Example 3 in an oven and heating them at 40 °C for 15 minutes, then taking them out and placing them on shredded paper and lifting them up, as Figure 3 shown, it can be clearly seen that Example 2 basically does not adhere to the shredded paper, indicating that the combined incense product prepared in Example 2 has no sticky feeling caused by the added hydrophobic agent during playing and wearing, effectively avoiding irritation to the human skin.

[0073] The above examples are only used to illustrate the technical solutions of the present invention, rather than limiting it; although the present invention has been described in detail with reference to the foregoing examples, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing examples, or perform equivalent replacements on some or all of the technical features; and these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the various embodiments of the present invention, and they should all be covered by the scope of the claims and the description of the present invention.

Claims

1. A preparation method of a fluorosiloxane hydrophobic modified perfume, characterized in that, It includes the following steps: 1) Mix the incense powder in proportion and soak it in the fluorosiloxane solution, filter and dry the incense powder to obtain the modified incense powder; 2) Grind and sieve the modified incense powder, then mix it with the adhesive powder and water in proportion, and repeatedly knead it with an open mill until it becomes a uniform mud shape, wrap it with plastic wrap and place it in a cool place to let the mud rest for later use; 3) Press the rested incense mud into sheets with an open mill, put it into a mold and compact it, take out the mold, and scrape off the excess part; 4) Place the de-molded combined incense product in a dark, dry and ventilated place to dry in the shade; 5) Polish, buff and oil the dried combined incense product to obtain the hydrophobic modified combined incense product.

2. The preparation method of the fluorosiloxane-hydrophobically modified fragrance product according to claim 1, wherein The incense powder described in step 1) is at least one of jasmine pollen, osmanthus powder, Hainan agarwood powder, mint powder, rose roselle pollen, agastache powder, sandalwood powder, and dalbergia odorifera powder.

3. The preparation method of the fluorosiloxane hydrophobic modified perfume according to claim 1 or 2, characterized in that, The fluorosiloxane solution described in step 1) is obtained by stirring and hydrolyzing 20-40% by volume of heptadecafluorodecyltrimethoxysilane, 1-2% of aminopropyltriethoxysilane and 60-80% of 50wt% alcohol at room temperature for 2-6h.

4. The preparation method of the fluorosiloxane hydrophobic modified incense product according to claim 1, characterized in that, The soaking time described in step 1) is 12-24h.

5. The preparation method of the fluorosiloxane hydrophobic modified perfume according to claim 4, wherein, The drying process parameters described in step 1) are: the drying temperature is 80-100°C, and the drying time is 2-4h.

6. The preparation method of the fluorosiloxane hydrophobic modified perfume according to claim 5, characterized in that, The mass ratio of the adhesive powder, incense powder and water described in step 2) is 1:(2-3):(3-4).

7. The preparation method of the fluorosiloxane-hydrophobically modified perfume product according to claim 6, characterized in that, The mesh number of the sieving described in step 2) is 50-120 mesh.

8. A fluorosiloxane hydrophobic modified combined incense product prepared by the preparation method according to any one of claims 1-7.

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