High-temperature-resistant long-lasting slow-release double-layer microcapsule powder essence as well as preparation method and application thereof
The bilayer microcapsule powder fragrance prepared by interfacial polymerization and spray drying methods solves the problems of easy volatility and weak binding force of liquid fragrance in leather production, and achieves stability and long-lasting fragrance effect under high temperature and high pressure conditions.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-31
- Publication Date
- 2026-04-07
AI Technical Summary
Existing liquid fragrances are prone to volatilization and loss during the high-temperature and high-pressure processing of leather production, and have weak binding force with leather fibers, resulting in low fragrance utilization and short fragrance retention time, which cannot meet consumers' demand for long-lasting fragrance in leather.
High-temperature resistant, long-lasting sustained-release bilayer microcapsule powder fragrance was prepared by interfacial polymerization and spray drying. The oily fragrance was encapsulated in a bilayer, and dense microcapsules were formed using oil and water phase materials. Spray drying was then used to form powder microcapsules, which enhanced the fragrance's high-temperature and high-pressure resistance and sustained-release effect.
It achieves the stability and long-lasting fragrance of fragrance under high temperature and high pressure conditions, prolongs the fragrance retention time of leather products, solves the problems of easy volatilization and poor heat resistance of fragrance, and improves the utilization rate of fragrance.
Smart Images
Figure CN121797209A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of fragrance technology, specifically to a high-temperature resistant, long-lasting, sustained-release double-layer microcapsule powder fragrance, its preparation method, and its application. Background Technology
[0002] With social development and the improvement of people's material and living standards, more and more consumers are showing increasing interest in leather products. Due to the diversification of leather production technologies, including genuine leather, artificial leather, and synthetic leather, the chemical odor from solvents and additives in artificial leather is difficult to completely remove. Many of these products contain impurities, especially the inherent odor of organic solvents, which means the produced leather has an unpleasant smell that is unlikely to appeal to consumers. However, using fragrances to scent leather not only creates a pleasant atmosphere but also has antibacterial, deodorizing, and odor-eliminating effects. This can significantly increase the added value of leather products, improve their inherent style, and expand the application areas of leather.
[0003] Currently, the fragrance technology used in the leather industry mainly involves directly adding liquid fragrances or spraying fragrances. Specifically, this includes adding liquid fragrances directly during leather retanning, filling, and finishing processes, or spraying fragrances onto the surface of finished leather products. However, the common liquid fragrances used in existing technologies have significant technical drawbacks: Firstly, the molecular structure of common fragrances is unstable and highly volatile. During high-pressure, high-temperature processing in leather production (such as baking, embossing, and shaping, typically at 120-140℃ and 0.5-7.5 MPa), fragrance molecules evaporate and are lost rapidly, resulting in extremely low fragrance utilization. Secondly, common liquid fragrances have weak binding force with leather fibers, making it difficult to firmly adhere to the interior of the leather fibers. They easily dissipate quickly due to washing, storage, and other factors during use, resulting in a very short fragrance retention time for leather products, usually only lasting a few days to a few weeks, which cannot meet consumers' demand for long-lasting leather fragrance. Summary of the Invention
[0004] To overcome the shortcomings and deficiencies of existing technologies, the present invention aims to provide a high-temperature resistant, long-lasting, sustained-release double-layer microcapsule powder fragrance, which is prepared by interfacial polymerization and spray drying. The double-layer encapsulated powder microcapsule fragrance provides better protection for the sustained release of the fragrance and offers a longer-lasting fragrance retention effect during high-temperature and high-pressure processing, making it effective for application in mobile phone leather manufacturing.
[0005] The purpose of this invention is to provide a method for preparing a high-temperature resistant, long-lasting, sustained-release double-layer microcapsule powder flavoring. This preparation method is simple, easy to operate and control, produces high-quality products at low cost, and is conducive to industrial production.
[0006] The objective of this invention is achieved through the following technical solution: a high-temperature resistant, long-lasting, sustained-release double-layer microcapsule powder fragrance, comprising a core material and a wall material encapsulating the core material, wherein the wall material comprises 75-90 wt% and the core material comprises 10-25 wt%. The core material comprises the following raw materials in parts by weight: Oil phase: 25-35 parts oily fragrance and 0.5-6 parts diisocyanate; Aqueous phase: 10-20 parts surfactant, 2-6 parts amino resin, 0.1-2 parts pH adjuster, and 44.6-84 parts deionized water; The wall material includes starch derivatives.
[0007] This invention relates to a high-temperature resistant, long-lasting, sustained-release double-layer microcapsule powder fragrance. It uses a floral-fruity oily fragrance as the core material and a polymer material as the wall material, undergoing encapsulation and spray drying. The synthetic microcapsule fragrance is then coated again to form a double-layer microcapsule powder fragrance. This double encapsulation of the volatile fragrance not only provides a sustained-release and long-lasting fragrance effect but also alters the physical state of the fragrance, making the powder microcapsules more convenient to use. The double-layer microcapsule powder fragrance of this invention is resistant to high temperatures and pressures, is not easily broken, and can release fragrance sustainably, solving the problems of easy volatility, poor heat resistance, and difficulty in use of fragrances in leather scenting applications.
[0008] Preferably, the oily fragrance is at least one of green apple fragrance, lily fragrance, and floral fragrance.
[0009] Preferably, the diisocyanate is at least one selected from toluene diisocyanate (TDI), diphenylmethane diisocyanate (MDI), hexamethylene diisocyanate (HDI), isoflurone diisocyanate (IPDI), or phenyl diisocyanate (XDI).
[0010] Preferably, the surfactant includes at least one of a nonionic surfactant, anionic surfactant, or polymeric surfactant.
[0011] Preferably, the nonionic surfactant includes at least one of Tween 85, Tween 80, OP-9, or OP-10; the anionic surfactant includes at least one of sodium dodecyl sulfate or sodium dodecyl sulfonate; and the polymeric surfactant includes at least one of styrene-maleic anhydride copolymer, ethylene-maleic anhydride copolymer E60, or polyoxyethylene acrylate.
[0012] Preferably, the amino resin is at least one of CYMEL 385, CYMEL 325 or CYMEL 327.
[0013] Preferably, the pH adjuster is at least one of hydrochloric acid solution, acetic acid solution, citric acid solution or phosphoric acid solution.
[0014] Preferably, the pH adjuster is at least one of the following: a hydrochloric acid solution with a mass fraction of 1-30%, an acetic acid solution with a mass fraction of 1-30%, a citric acid solution with a mass fraction of 1-30%, or a phosphoric acid solution with a mass fraction of 1-30%.
[0015] This invention also provides a method for preparing a high-temperature resistant, long-lasting, sustained-release bilayer microcapsule powder fragrance, comprising the following steps: S1. According to the weight parts, add the oily fragrance and diisocyanate into the reaction device and mix evenly to obtain the oil phase for later use; S2. According to the weight proportions, add the surfactant and amino resin to the deionized water, mix thoroughly and evenly to form an aqueous phase, and set aside for later use; S3. Add the oil phase obtained in step S1 to the aqueous phase obtained in step S2, and mix them evenly under high-speed shearing to obtain a mixture for later use. S4. Add the mixture obtained in step S3 to the reaction vessel, stir it mechanically at 50-60℃ until homogeneous, and keep it at the temperature for 0.8-1.2h. Then add a pH adjuster to adjust the pH of the system to accelerate the reaction, and raise the temperature to 80-90℃ and keep it at the temperature for 1.5-2.5h to obtain the fragrance microcapsule emulsion. S5. Add deionized water to the mixing tank and heat it to 40-50℃. Then add maltodextrin and β-cyclodextrin and stir evenly. Next, add the flavor microcapsule emulsion obtained in step S4 and mix and stir for 1-3 hours to obtain a mixed emulsion. S6. The mixed emulsion obtained in step S5 is spray-dried using a spray dryer with an inlet air temperature of 150-200℃ and an outlet air temperature of 75-85℃. After the mixed emulsion is dried into powder, it is cooled to room temperature to obtain double-layer microcapsule powder fragrance.
[0016] The high-temperature resistant, long-lasting, sustained-release double-layer microcapsule powder fragrance of this invention is prepared by interfacial polymerization. The preparation method involves emulsifying a surfactant in an aqueous phase onto the surface of fragrance oil microspheres. An amino resin in the aqueous phase diffuses into the oil phase and reacts rapidly with diisocyanate, forming a dense microcapsule within seconds, thus obtaining the core material. The second layer of the double-layer microcapsule powder fragrance is prepared by spray drying. This involves mixing starch derivative natural polymer materials, atomizing the thinner in a drying chamber, and then rapidly vaporizing the moisture upon contact with hot air, resulting in the dried double-layer microcapsule powder fragrance. This double-layer microcapsule powder fragrance is resistant to high temperatures and pressures, is not easily broken, and can release fragrance sustainably. It can be used in leather applications to mask odors and meet the need for long-lasting fragrance in daily life.
[0017] The beneficial effects of this invention are as follows: 1. The double-layer microcapsule powder fragrance prepared by the present invention is formed by double-layer coating of oily fragrance, which provides double protection for the easily volatile oily fragrance, greatly prolonging the fragrance retention time. On the other hand, it also changes the physical state of the fragrance, and the powder microcapsules are more convenient to use.
[0018] 2. The double-layer microcapsule powder fragrance prepared by this invention has the effect of high temperature and high pressure resistance, which solves the problems of easy volatility, poor heat resistance and difficulty in use of fragrance in leather fragrance application. Attached Figure Description
[0019] Figure 1 The TGA curve is shown for the double-layer microcapsule powder fragrance prepared in Example 1. Detailed Implementation
[0020] To facilitate understanding by those skilled in the art, the following description is provided in conjunction with embodiments and appendices. Figure 1 The present invention will be further described below, and the content mentioned in the embodiments is not intended to limit the present invention.
[0021] Example 1 This embodiment provides a high-temperature resistant, long-lasting, sustained-release bilayer microcapsule powder fragrance, including a core material and a wall material encapsulating the core material; The core material comprises the following raw materials in parts by weight: Oil phase: 30 parts oily fragrance and 3 parts diisocyanate; Aqueous phase: 10 parts surfactant, 5.4 parts amino resin, 1.4 parts pH adjuster, and 50.2 parts deionized water; The wall material comprises 35 parts of starch derivative, wherein the starch derivative is a mixture of maltodextrin and β-cyclodextrin in a mass ratio of 6:1.
[0022] Furthermore, the oily fragrance is green apple fragrance. The diisocyanate is phthalimide diisocyanate. The surfactant is styrene-maleic anhydride copolymer 520. The amino resin is CYMEL 385. The pH adjuster is a 50% acetic acid solution.
[0023] A method for preparing a high-temperature resistant, long-lasting, sustained-release bilayer microcapsule powder fragrance includes the following steps: S1. Add 30g of green apple flavoring (oil-based) and 3g of phthalimide diisocyanate to the reaction apparatus and mix well to obtain the oil phase for later use. S2. According to the weight parts, add 10g of surfactant with a mass fraction of 20% and 5.4g of amino resin to 50.2g of deionized water, mix thoroughly and evenly to form an aqueous phase, and set aside for later use; S3. Add the oil phase obtained in step S1 to the aqueous phase obtained in step S2, and mix under high-speed shear at 3000 rpm / min for 5 min to obtain a mixture for later use. S4. Add the mixture obtained in step S3 to the reaction vessel, mechanically stir it at 300 rpm / min at 55°C until homogeneous, and keep it at the temperature for 1 hour. Then add 1.4 g of 50% acetic acid solution to adjust the pH of the system and accelerate the reaction, and raise the temperature to 82°C and keep it at the temperature for 2 hours to obtain the fragrance microcapsule emulsion. S5. Add 150g of deionized water to the mixing tank and heat it to 45℃. Then add 30g of maltodextrin and 5g of β-cyclodextrin and stir evenly. Next, add 65g of the flavor microcapsule emulsion obtained in step S4 and mix and stir for 2 hours to obtain a mixed emulsion. S6. The mixed emulsion obtained in step S5 is spray-dried using a spray dryer with an inlet air temperature of 180°C and an outlet air temperature of 80°C. The liquid needs to be slowly stirred during spraying to ensure that the liquid is a homogeneous system. After the mixed emulsion is dried into powder, it is cooled to room temperature to obtain double-layer microcapsule powder fragrance.
[0024] Example 2 This embodiment provides a high-temperature resistant, long-lasting, sustained-release bilayer microcapsule powder fragrance, including a core material and a wall material encapsulating the core material; The core material comprises the following raw materials in parts by weight: Oil phase: 60 parts oily fragrance and 6 parts diisocyanate; Aqueous phase: 10 parts surfactant, 5.4 parts amino resin, 1.4 parts pH adjuster, and 50.2 parts deionized water; The wall material comprises 35 parts of starch derivative, wherein the starch derivative is a mixture of maltodextrin and β-cyclodextrin in a mass ratio of 6:1.
[0025] Furthermore, the oily fragrance is green apple fragrance. The diisocyanate is a mixture of terephthalic diisocyanate and hexamethylene diisocyanate in a molar ratio of 1:1. The surfactant is styrene-maleic anhydride copolymer 520. The amino resin is CYMEL 385. The pH adjuster is a 50% acetic acid solution.
[0026] A method for preparing a high-temperature resistant, long-lasting, sustained-release bilayer microcapsule powder fragrance includes the following steps: S1. Add 60g of green apple flavoring (oil-based) and 6g of diisocyanate to the reaction apparatus and mix well to obtain the oil phase for later use; S2. According to the weight parts, add 10g of surfactant with a mass fraction of 20% and 5.4g of amino resin to 50.2g of deionized water, mix thoroughly and evenly to form an aqueous phase, and set aside for later use; S3. Add the oil phase obtained in step S1 to the aqueous phase obtained in step S2, and mix under high-speed shear at 3000 rpm / min for 5 min to obtain a mixture for later use. S4. Add the mixture obtained in step S3 to the reaction vessel, mechanically stir it at 300 rpm / min at 55°C until homogeneous, and keep it at the temperature for 1 hour. Then add 1.4 g of 50% acetic acid solution to adjust the pH of the system and accelerate the reaction, and raise the temperature to 82°C and keep it at the temperature for 2 hours to obtain the fragrance microcapsule emulsion. S5. Add 150g of deionized water to the mixing tank and heat it to 45℃. Then add 30g of maltodextrin and 5g of β-cyclodextrin and stir evenly. Next, add 65g of the flavor microcapsule emulsion obtained in step S4 and mix and stir for 2 hours to obtain a mixed emulsion. S6. The mixed emulsion obtained in step S5 is spray-dried using a spray dryer with an inlet air temperature of 180°C and an outlet air temperature of 80°C. The liquid needs to be slowly stirred during spraying to ensure that the liquid is a homogeneous system. After the mixed emulsion is dried into powder, it is cooled to room temperature to obtain double-layer microcapsule powder fragrance.
[0027] Example 3 The process of splicing and covering leather for mobile phone case back covers includes the following steps: material slitting → die-cutting → adhesive application to cut surfaces → sequential single-color splicing → assembly splicing → binding → hot pressing → precision cutting → hot pressing and bonding. The leather undergoes two high-temperature and high-pressure processes: hot pressing and hot pressing bonding, at temperatures of 120℃-150℃ and pressures of 0.5-7.5Mpa.
[0028] This embodiment provides the application of the above-mentioned high-temperature resistant, long-lasting, slow-release double-layer microcapsule powder fragrance in mobile phone leather: the application method includes the following steps: take the double-layer microcapsule powder fragrance, add it to the acrylic ester glue, stir and mix evenly, apply the glue evenly to the cut surface of the leather, and then cure it in hot pressing.
[0029] Performance testing (1) Thermogravimetric analysis (TGA) was performed on the green apple double-layer microcapsule powder flavoring and green apple flavoring (liquid) prepared in Example 1. The results are as follows: Figure 1 As shown: Depend on Figure 1It can be seen that the liquid fragrance (red curve) rapidly loses weight to near zero before reaching approximately 200℃, indicating that it will evaporate and be lost in large quantities during the high-temperature process (120-150℃) of leather processing. In contrast, the weight loss rate of the double-layer microcapsule fragrance (blue curve) is significantly slower, only beginning to show significant weight loss at around 250℃, indicating that it has stronger tolerance to high temperatures and can effectively resist the high temperatures in leather production, reducing heat loss of the fragrance. Moreover, the slow weight loss stage of the curve corresponds to the slow release process of the fragrance: the liquid fragrance has almost no slow release process and evaporates completely in a short time; the weight loss curve of the double-layer microcapsule fragrance is flatter, indicating that its wall material can effectively encapsulate the fragrance, achieving slow release and thus prolonging the fragrance retention time of leather products.
[0030] (2) Fragrance retention effect test Experimental group: Take 0.5g of green apple double-layer microcapsule powder fragrance prepared in Example 1, add it to 10g of YH-818 acrylate adhesive, stir and mix evenly, apply the adhesive evenly to the cut surface of the leather, and then heat-press to cure.
[0031] Control group 1: Take 0.5g of green apple fragrance (liquid) and add it to 10g of YH-818 acrylic glue. Stir and mix evenly. Apply the glue evenly to the cut surface of the leather and then heat-press to cure.
[0032] Control group 2: Take 0.5g of green apple flavoring embedded in maltodextrin powder, add it to 10g of YH-818 acrylate adhesive, stir and mix evenly, apply the adhesive evenly to the cut surface of the leather, and then heat-press to cure. The preparation method of green apple flavoring encapsulated in maltodextrin powder includes the following steps: S1. Add 150g of deionized water to the mixing tank and heat it to 45℃. Then add 30g of maltodextrin and 5g of β-cyclodextrin and stir evenly. Next, add 30g of green apple flavor (oil-based) and mix for 2 hours to obtain a mixed emulsion. S2. The mixed emulsion obtained above is spray-dried using a spray dryer with an inlet air temperature of 180°C and an outlet air temperature of 80°C. After the mixed emulsion is dried into powder, it is cooled to room temperature to obtain double-layer microcapsule powder fragrance.
[0033] Control group 3 (blank control group): Take 10.5g of YH-818 acrylic glue, apply it evenly to the cut surface of the leather, and then heat-press to cure.
[0034] The four sets of shaped leather phone cases were then placed for 12 hours, 24 hours, 36 hours, 72 hours, and 128 hours, and their fragrances were compared. The results are shown in Table 1. Table 1
[0035] It can be seen that the double-layer microcapsule powder fragrance prepared by the present invention is formed by double-layer coating of oily fragrance, which provides double protection for the easily volatile oily fragrance and greatly prolongs the fragrance retention time.
[0036] The above embodiments are preferred implementations of the present invention. In addition, the present invention can be implemented in other ways. Any obvious substitutions without departing from the concept of the present invention are within the protection scope of the present invention.
Claims
1. A high-temperature resistant, long-lasting, sustained-release, double-layered microcapsule powder fragrance, characterized in that: Includes a core material and a wall material enclosing the core material, wherein the wall material comprises 75-90 wt% and the core material comprises 10-25 wt%. The core material comprises the following raw materials in parts by weight: Oil phase: 25-35 parts oily fragrance and 0.5-6 parts diisocyanate; Aqueous phase: 10-20 parts surfactant, 2-6 parts amino resin, 0.1-2 parts pH adjuster, and 44.6-84 parts deionized water; The wall material includes starch derivatives.
2. The high-temperature resistant, long-lasting, sustained-release double-layer microcapsule powder fragrance according to claim 1, characterized in that: The oily fragrance is at least one of green apple fragrance, lily fragrance, and floral fragrance.
3. The high-temperature resistant, long-lasting, sustained-release double-layer microcapsule powder fragrance according to claim 1, characterized in that: The diisocyanate is at least one of toluene diisocyanate, diphenylmethane diisocyanate, hexamethylene diisocyanate, isoflurone diisocyanate, or phenyldimethyl diisocyanate.
4. The high-temperature resistant, long-lasting, sustained-release double-layer microcapsule powder fragrance according to claim 1, characterized in that: The surfactant includes at least one of nonionic surfactants, anionic surfactants, or polymeric surfactants.
5. The high-temperature resistant, long-lasting, sustained-release double-layer microcapsule powder fragrance according to claim 1, characterized in that: The nonionic surfactant includes at least one of Tween 85, Tween 80, OP-9, or OP-10; the anionic surfactant includes at least one of sodium dodecyl sulfate or sodium dodecyl sulfonate; and the polymeric surfactant includes at least one of styrene-maleic anhydride copolymer, ethylene-maleic anhydride copolymer E60, or polyoxyethylene acrylate.
6. The high-temperature resistant, long-lasting, sustained-release bilayer microcapsule powder fragrance according to claim 1, characterized in that: The pH adjuster is at least one of hydrochloric acid solution, acetic acid solution, citric acid solution or phosphoric acid solution.
7. The high-temperature resistant, long-lasting, sustained-release bilayer microcapsule powder fragrance according to claim 1, characterized in that: The starch derivative includes at least one of maltodextrin or β-cyclodextrin.
8. A method for preparing a high-temperature resistant, long-lasting, sustained-release bilayer microcapsule powder fragrance as described in any one of claims 1-7, characterized in that: Includes the following steps: S1. According to the weight parts, add the oily fragrance and diisocyanate into the reaction device and mix evenly to obtain the oil phase for later use; S2. According to the weight proportions, add the surfactant and amino resin to the deionized water, mix thoroughly and evenly to form an aqueous phase, and set aside for later use; S3. Add the oil phase obtained in step S1 to the aqueous phase obtained in step S2, and mix them evenly under high-speed shearing to obtain a mixture for later use. S4. Add the mixture obtained in step S3 to the reaction vessel, stir it mechanically at 50-60℃ until homogeneous, and keep it at the temperature for 0.8-1.2h. Then add a pH adjuster to adjust the pH of the system to accelerate the reaction, and raise the temperature to 80-90℃ and keep it at the temperature for 1.5-2.5h to obtain the fragrance microcapsule emulsion. S5. Add deionized water to the mixing tank and heat it to 40-50℃. Then add maltodextrin and β-cyclodextrin and stir evenly. Next, add the flavor microcapsule emulsion obtained in step S4 and mix and stir for 1-3 hours to obtain a mixed emulsion. S6. The mixed emulsion obtained in step S5 is spray-dried using a spray dryer with an inlet air temperature of 150-200℃ and an outlet air temperature of 75-85℃. After the mixed emulsion is dried into powder, it is cooled to room temperature to obtain double-layer microcapsule powder fragrance.
9. The method for preparing the high-temperature resistant, long-lasting, sustained-release bilayer microcapsule powder fragrance according to claim 8, characterized in that: In step S4, the stirring speed is 300-1000 rpm / min.
10. The application of the high-temperature resistant, long-lasting, sustained-release double-layer microcapsule powder fragrance according to any one of claims 1-7, or the double-layer microcapsule powder fragrance prepared by the method according to claim 7, in mobile phone leather.