Preparation process of a three-in-one shampoo and conditioner
Patent Information
- Application Number
- CN202611217850.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-08-12
- Publication Date
- 2026-09-29
AI Technical Summary
[0008]本申请主要提供一种三合一洗护用品的制备工艺方法,以解决当前茶油洗护产品水溶性差、易氧化酸败、洗后油腻贴头皮的问题
[0019]本申请的有益效果是:区别于现有技术的情况,本申请公开了一种三合一洗护用品的制备工艺方法。本申请实施例采用生物可降解的两亲性大分子作为壁材,通过80-150MPa的高压微射流均质将茶油打碎至纳米级,并在芯材中复配天然抗氧化剂,纳米级包埋使得茶油在水基洗护体系中能瞬间分散,不留浮油;复合壁材与抗氧化剂的协同作用,结合进风温度为40℃-60℃的低温喷雾干燥工艺,显著提升茶油水溶性与抗氧化稳定性,彻底避免了高温导致的茶油氧化酸败,极大延长了产品的货架期;在制备三合一组合物时,严格控制在降温至35℃以下加入酸性pH调节剂,这一冷配工艺避免了高温或碱性环境对微胶囊壁材的破坏,使得茶油微胶囊在表面活性剂体系中保持结构完整;在洗发过程中,茶油微胶囊主要发挥物理润滑作用并随水流冲走,避免了大分子油脂直接附着导致的头发扁塌和头皮油腻;而在沐浴时,借助体温与肌肤摩擦,茶油微胶囊在身体角质层缓慢破裂释放茶油活性成分,实现长效深层保湿,实现了一瓶多效。
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Figure CN122827904A_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of biomanufacturing technology for personal care products, and in particular to a preparation process for a three-in-one shampoo and conditioner. Background Technology
[0002] Camellia oil is a high-grade natural plant oil extracted from the seeds of the camellia tree. It is rich in bioactive substances such as oleic acid, linoleic acid, squalene, vitamin E, and camelliaside. Due to its chemical composition's high similarity to human sebum, camellia oil exhibits excellent skin permeability, moisturizing and water-locking abilities, and the ability to repair damaged skin barriers in personal care. For hair, camellia oil can penetrate deep into the hair cuticle to repair damaged structures; for skin, it can form a breathable natural protective film to prevent moisture loss. Therefore, the application of camellia oil in shampoos, conditioners, and body washes has extremely high nutritional value and promising market prospects.
[0003] However, adding camellia oil directly to personal care products currently faces three significant technical bottlenecks. First, poor water solubility and dispersibility. As a fat-soluble substance, camellia oil is prone to stratification, floating, or precipitation when directly added to water-based personal care systems, leading to unstable product appearance. Second, high risk of oxidative rancidity and spoilage. The unsaturated fatty acids abundant in camellia oil are easily oxidized in the air, especially in the presence of surfactants and moisture in personal care products. This oxidative rancidity accelerates dramatically, not only producing unpleasant odors but also causing nutrient loss and the formation of peroxides harmful to the skin. Third, difficulty in simultaneously addressing shampooing and bathing needs. Traditional methods of directly adding camellia oil can easily lead to flat, limp hair and increased scalp oiliness during shampooing due to residual oil. While moisturizing oils are needed during bathing, unprocessed camellia oil feels heavy and is difficult to absorb quickly.
[0004] To address these issues, microencapsulation technology has been gradually introduced into the personal care field. Microencapsulation not only protects the core material (tea oil) from environmental damage but also masks unpleasant odors and enables the sustained release of active substances. However, existing microencapsulation preparation technologies still have many shortcomings when applied to tea oil and 3-in-1 shampoo and conditioner products. On the one hand, traditional emulsification encapsulation processes often employ high-temperature homogenization or high-temperature spray drying, while squalene and vitamin E in tea oil are heat-sensitive substances. High-temperature processing easily leads to the loss of their activity, and high temperatures accelerate the oxidation reaction of tea oil. On the other hand, conventional wall materials (such as gelatin and gum arabic single systems) have poor stability and encapsulation rates in personal care systems, and in wash-off products, the release kinetics of microcapsules are difficult to control—if they rupture rapidly during shampooing, the released oil will still cause the hair to become flat; if they do not rupture, they cannot provide moisturizing effects during showering.
[0005] In addition, as consumers pursue green and gentle skin care concepts, amino acid surfactants are widely used due to their mild and non-irritating properties. However, the compound system of amino acid surfactants and oil microcapsules has poor phase stability at low temperatures, and the traditional preparation process is energy-intensive and complicated, making it difficult to achieve low-cost, large-scale industrial production while ensuring product quality.
[0006] Furthermore, current microcapsule preparation methods often employ high-temperature homogenization or conventional high-temperature spray drying. However, squalene and vitamin E in tea oil are heat-sensitive substances, and high-temperature processing easily leads to their loss of activity. Moreover, high temperatures accelerate the oxidation reaction of tea oil. Additionally, when microcapsules are incorporated into a 3-in-1 shampoo, conditioner, and body wash system, if the mixing temperature and pH of the system are not strictly controlled, the microcapsule wall material is prone to rupture or swelling under the action of surfactants, causing premature release of tea oil. This not only fails to achieve the intelligent balance between oil control in shampooing and moisturizing in body wash, but also results in decreased product water solubility and an oily, sticky scalp after washing.
[0007] Therefore, there is an urgent need for a manufacturing process for a three-in-one shampoo and conditioner that can significantly improve the water solubility and antioxidant properties of tea oil, retain the natural activity of tea oil, and perfectly balance the needs of shampooing for oil control and bathing for moisturizing. Summary of the Invention
[0008] This application mainly provides a preparation process for a three-in-one shampoo and conditioner product to solve the problems of poor water solubility, easy oxidation and rancidity, and oily residue on the scalp after washing with current tea oil shampoo and conditioner products.
[0009] To solve the above-mentioned technical problems, one technical solution adopted in this application is: to provide a preparation process for a three-in-one shampoo and conditioner product. The preparation process includes: S1: The biodegradable amphiphilic macromolecular wall material is mixed with purified water and stirred at 40℃-50℃ to obtain the aqueous phase of the wall material; S2: Cold-pressed tea oil is mixed with natural antioxidants to form an oil phase. The oil phase is slowly added to the aqueous phase of the wall material under high-speed shearing conditions to carry out coarse emulsification and obtain a primary emulsion. S3: The primary emulsion is passed into a high-pressure microfluidic homogenizing system and homogenized 2-4 times under a pressure of 80-150MPa to obtain a nanoscale microemulsion. S4: The nanoscale microemulsion is mixed with a low-temperature excipient and then spray-dried at a low temperature of 40℃-60℃ to collect the powder and obtain tea oil microcapsules. S5: The tea oil microcapsules are mixed with the surfactant system and functional additives in a preset order, and the mixture is cooled to below 35°C and an acidic pH adjuster is added to obtain a three-in-one shampoo, conditioner and body wash product.
[0010] In some embodiments, step S1 includes: S11: Dissolve the modified cyclodextrin in the purified water in the first part, and stir at 300-500 rpm for 15-25 minutes at 40℃-45℃ until completely dissolved; S12: Disperse natural phospholipids in the purified water of the second part and perform hydration and swelling. The hydration temperature is 40℃-50℃ and the swelling time is 20-40 minutes. S13: Combine the solution obtained in S11 with the dispersion obtained in S12, and stir in a homogenizer at 4000-6000 rpm for 3-8 minutes to form a uniform aqueous phase of the wall material.
[0011] In some embodiments, in step S11, the modified cyclodextrin is one of hydroxypropyl-β-cyclodextrin or octyl-β-cyclodextrin; in step S12, the natural phospholipid is soybean lecithin or hydrogenated phospholipid. The mass ratio of the modified cyclodextrin to the natural phospholipid is 2:1-3:1, and the total mass of the two accounts for 15%-20% of the total mass of the aqueous phase of the wall material.
[0012] In some embodiments, step S2 includes: S21: Preheat cold-pressed tea oil to 30℃-40℃, add 0.5%-1.5% of natural antioxidants by weight of tea oil, and stir until completely dissolved to form the oil phase; S22: Preheat the aqueous phase of the wall material to 35℃-45℃, place it in a high-shear emulsification tank, and set the shear speed to 8000-12000 rpm; S23: While maintaining shearing, the oil phase is added to the aqueous phase of the wall material at a uniform rate by atomization spraying. After the addition is completed, shearing continues for 10-20 minutes to obtain a primary emulsion with a particle size of 1-5μm.
[0013] In some embodiments, in step S21, the natural antioxidant is a composite antioxidant composed of rosemary extract, tea polyphenols and vitamin E in a mass ratio of 1:1:2.
[0014] In some embodiments, step S3 includes: S31: Before the primary emulsion is fed into the reaction chamber of the micro-jet homogenizer by a high-pressure plunger pump, it is pre-cooled to control the material inlet temperature at 20℃-25℃. S32: In the Y-shaped interactive collision chamber of the micro-jet homogenizer, the first-stage homogenization pressure is set to 100-120MPa, and the second-stage homogenization pressure is set to 80-90MPa for continuous cyclic homogenization. S33: After homogenization, the material is quickly cooled to 10℃-15℃ through a plate heat exchanger to obtain a nanoscale microemulsion with an average particle size of 50-200nm and a polydispersity index of 0.2-0.3.
[0015] In some embodiments, step S4 includes: S41: Dissolve the low-temperature excipient in purified water to prepare an excipient aqueous solution with a mass concentration of 20%-30%, and mix it evenly with the nanoscale microemulsion at a volume ratio of 1:0.8-1:1.2; S42: The mixture is fed into a low-temperature spray drying tower, with the inlet air temperature set at 45℃-55℃, the outlet air temperature at 30℃-35℃, and the atomization pressure at 0.2-0.3MPa; S43: The powder is collected by a cyclone separator at the bottom of the tower and sieved through a 40-60 mesh vibrating screen to obtain tea oil microcapsules with a moisture content of 1%-3%.
[0016] In some embodiments, in step S41, the low-temperature excipient is a mixture of maltodextrin and gum arabic in a mass ratio of 2:1 to 4:1.
[0017] In some embodiments, step S5 includes: S51: Dissolve the amino acid-based surfactant in deionized water, heat to 38℃-42℃ and stir to dissolve, then add humectant and thickener, and stir until completely transparent; S52: When the system cools down to 32℃-35℃, add the tea oil microcapsules and disperse them evenly by low-speed shearing and stirring to avoid damaging the microcapsule structure. S53: Add a 5%-15% citric acid aqueous solution to adjust the pH of the system to 5.0-5.5. Finally, add preservatives and fragrances, and the product is ready to be dispensed as a three-in-one shampoo and conditioner.
[0018] In some embodiments, in step S51, the amino acid-based surfactant is a combination of sodium cocoyl glutamate and sodium lauroyl hydroxymethyl sulfonate; in step S52, the rotational speed of the low-speed shearing is 300-500 rpm.
[0019] The beneficial effects of this application are as follows: Unlike existing technologies, this application discloses a preparation process for a three-in-one shampoo and conditioner. In this application, biodegradable amphiphilic macromolecules are used as the wall material. Tea oil is broken down to the nanoscale through high-pressure micro-jet homogenization at 80-150 MPa, and natural antioxidants are compounded into the core material. This nanoscale encapsulation allows the tea oil to disperse instantly in water-based shampoo and conditioner systems without leaving any floating oil. The synergistic effect of the composite wall material and antioxidants, combined with a low-temperature spray drying process with an inlet air temperature of 40℃-60℃, significantly improves the water solubility and antioxidant stability of the tea oil, completely avoiding oxidation and rancidity caused by high temperatures, and greatly extending the product's shelf life. This process is crucial for the preparation of the three-in-one product. When assembling the product, the addition of acidic pH adjusters is strictly controlled to be below 35°C. This cold-mixing process avoids damage to the microcapsule wall material caused by high temperature or alkaline environment, allowing the tea oil microcapsules to maintain structural integrity in the surfactant system. During shampooing, the tea oil microcapsules mainly play a physical lubricating role and are washed away with water, avoiding the direct adhesion of large molecule oils that cause flat hair and oily scalp. During bathing, with the help of body temperature and friction with the skin, the tea oil microcapsules slowly break down in the stratum corneum of the body, releasing the active ingredients of tea oil, achieving long-lasting deep moisturizing, thus realizing multiple effects in one bottle. Attached Figure Description
[0020] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort, wherein: Figure 1 This is a schematic flow chart of an embodiment of the preparation process provided in this application; Figure 2 This is a schematic flowchart of an embodiment of step S1 in the preparation process provided in this application; Figure 3 This is a schematic flowchart of an embodiment of step S2 in the preparation process provided in this application; Figure 4 This is a schematic flowchart of an embodiment of step S3 in the preparation process provided in this application; Figure 5 This is a schematic flowchart of an embodiment of step S4 in the preparation process provided in this application; Figure 6 This is a schematic flowchart of an embodiment of step S5 in the preparation process provided in this application. Detailed Implementation
[0021] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of this application, and not all of the embodiments. Based on the embodiments of this application, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of this application.
[0022] The terms "first," "second," and "third" used in the embodiments of this application are for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined as "first," "second," or "third" may explicitly or implicitly include at least one of that feature. In the description of this application, "multiple" means at least two, such as two, three, etc., unless otherwise explicitly specified. Furthermore, the terms "comprising" and "having," and any variations thereof, are intended to cover non-exclusive inclusion. For example, a process, method, system, product, or device that includes a series of steps or units is not limited to the listed steps or units, but may optionally include steps or units not listed, or may optionally include other steps or units inherent to these processes, methods, products, or devices.
[0023] In this document, the term "embodiment" means that a particular feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of this application. The appearance of this phrase in various places throughout the specification does not necessarily refer to the same embodiment, nor is it a mutually exclusive, independent, or alternative embodiment. It will be explicitly and implicitly understood by those skilled in the art that the embodiments described herein can be combined with other embodiments.
[0024] To address the problems of poor water solubility, easy oxidation and rancidity, oily and sticky scalp after shampooing, and loss of activity and high energy consumption caused by high-temperature processing in existing 3-in-1 shampoo, conditioner, and body wash products using tea oil, this application provides a technical solution for preparing 3-in-1 shampoo and conditioner products by microemulsifying tea oil with a biodegradable wall material and then cold-blending at low temperatures. This technical solution achieves nanoscale encapsulation of tea oil at low temperatures throughout the entire process, through a process route of "amphiphilic macromolecular compounding - high-pressure microfluidic nano-sizing - low-temperature spray drying and curing - low-temperature cold-blending composite." This endows the microcapsules with differentiated release characteristics in shampooing and body wash scenarios. Furthermore, the process is compact, low-carbon, and energy-saving, completely eliminating the use of traditional high-temperature homogenization and strong chemical solvents.
[0025] Specifically, see Figure 1 , Figure 1 This is a schematic flow chart of an embodiment of the preparation process method provided in this application. The preparation process method for a three-in-one personal care product provided in this application includes: Step S1: Mix the biodegradable amphiphilic macromolecular wall material with purified water, and swell and stir at 40℃-50℃ to obtain the aqueous phase of the wall material.
[0026] Camellia oil is rich in unsaturated fatty acids, primarily oleic acid. While these components possess high skin affinity and repairing effects, their strong hydrophobicity prevents them from being stably dispersed directly in water-based shampoos and body washes. Microencapsulation technology is the core solution to this problem, and the selection and pretreatment of the wall material directly determine the encapsulation rate, stability, and subsequent release behavior of the microcapsules in rinse-off products. This embodiment abandons traditional synthetic polymer wall materials and selects biodegradable amphiphilic macromolecules as the wall material, which is both safe and environmentally friendly, and can effectively encapsulate the camellia oil by utilizing its hydrophilic ends and hydrophobic cavities.
[0027] In some embodiments, see Figure 2 , Figure 2 This is a schematic flowchart of an embodiment of step S1 in the preparation process provided in this application. Step S1 includes: Step S11: Dissolve the modified cyclodextrin in the purified water of the first part, and stir at 300-500 rpm for 15-25 minutes at 40℃-45℃ until completely dissolved; Step S12: Disperse the natural phospholipids in the purified water of the second part and perform hydration and swelling. The hydration temperature is 40℃-50℃ and the swelling time is 20-40 minutes. Step S13: Combine the solution obtained in S11 with the dispersion obtained in S12, and stir in a homogenizer at 4000-6000 rpm for 3-8 minutes to form a uniform aqueous phase of the wall material.
[0028] Specifically, in step S11, modified cyclodextrin is selected as the first wall material component. Cyclodextrin (CD) is a cyclic oligosaccharide produced by the action of glucosyltransferase on starch. Its unique external hydrophilic and internal hydrophobic truncated cone-shaped cylindrical structure allows it to encapsulate small molecule fat-soluble components (such as squalene and vitamin E) in tea oil into its cavity through hydrophobic interactions.
[0029] However, natural cyclodextrins (such as β-cyclodextrin) have low solubility in water, approximately 1.85%, which is insufficient to meet the requirements for high-concentration tea oil encapsulation. Therefore, this embodiment uses modified cyclodextrin, specifically one of hydroxypropyl-β-cyclodextrin (HP-β-CD) or octyl-β-cyclodextrin (O-β-CD). HP-β-CD, by introducing a hydroxypropyl group, disrupts the hydrogen bond network within the cyclodextrin molecule, causing its solubility in water to jump to over 60%; while the octyl group introduced in O-β-CD not only increases water solubility but also further enhances the affinity of its hydrophobic cavity for long-chain fatty acids (the main component of tea oil).
[0030] Stirring at a low speed of 300-500 rpm for 15-25 minutes at 40℃-45℃ ensures that the modified cyclodextrin dissolves fully in the purified water in the first part without generating bubbles. If the temperature is below 40℃, the dissolution rate of cyclodextrin is too slow and takes too long; if the temperature is above 45℃, although dissolution is accelerated, it can easily lead to the thermal destruction of the structure of the subsequently added natural phospholipids. Maintaining the stirring speed at 300-500 rpm, using a paddle or anchor stirrer, creates laminar flow and avoids the entrainment of large amounts of air, which can generate stable bubbles. The presence of bubbles will seriously affect the continuity of the fluid and the stability of the pressure during subsequent high-pressure microjet homogenization.
[0031] In step S12, natural phospholipids are selected as the second wall material component, specifically soybean lecithin or hydrogenated phospholipids. Natural phospholipids are amphoteric surfactants with a molecular structure containing hydrophilic phosphate groups and hydrophilic choline groups, as well as two hydrophobic fatty acid chains. In water, phospholipids can spontaneously form a liposome bilayer structure. Their hydrophobic tails can tightly bind to the surface of tea oil droplets, while their hydrophilic heads extend into the aqueous phase, thus forming a dense physical barrier on the surface of the tea oil droplets. The natural phospholipids are dispersed in the second part of purified water for hydration and swelling. The hydration temperature is set at 40℃-50℃, which is higher than the phase transition temperature of phospholipids, which is typically between 15-35℃. Above the phase transition temperature, the acyl chains of the phospholipids move more, transforming from a tightly packed gel state to a more fluid liquid crystal state. At this point, water molecules can easily penetrate the space between the phospholipid bilayers, causing them to swell rapidly and peel off into single or multilayer vesicles. If the hydration temperature is below 40℃, the phospholipids will not hydrate sufficiently, easily forming large insoluble masses or gel clusters, affecting the subsequent embedding effect; if the temperature is above 50℃, excessive swelling may lead to local structural disintegration. The swelling time should be 20-40 minutes to ensure that the phospholipids are fully hydrated and form a uniform blank liposome suspension.
[0032] In step S13, the cyclodextrin solution obtained in S11 and the phospholipid dispersion obtained in S12 are combined and stirred in a homogenizer at 4000-6000 rpm for 3-8 minutes to form a homogeneous aqueous wall material phase. The purpose of this step is to uniformly mix the cyclodextrin solution with inclusion capacity and the phospholipid vesicle solution with film-forming capacity to construct a composite wall material system with dual synergistic inclusion and film-forming properties. The moderate shear speed of 4000-6000 rpm can break down the large multilayer vesicle structure of phospholipids, making them smaller and more uniform single-chamber vesicles, while allowing cyclodextrin molecules to be uniformly dispersed around the vesicles, preparing for synergistic encapsulation upon subsequent contact with tea oil.
[0033] In some embodiments, in step S11, the modified cyclodextrin is one of hydroxypropyl-β-cyclodextrin or octyl-β-cyclodextrin; in step S12, the natural phospholipid is soybean lecithin or hydrogenated phospholipid; the mass ratio of the modified cyclodextrin to the natural phospholipid is 2:1-3:1, and the total mass of the two accounts for 15%-20% of the total mass of the aqueous phase of the wall material.
[0034] Extensive experimental verification has shown that when the mass ratio of modified cyclodextrin to natural phospholipids is controlled between 2:1 and 3:1, the system exhibits the best tea oil encapsulation efficiency and long-term stability. If the proportion of modified cyclodextrin is too low, such as a mass ratio of modified cyclodextrin to natural phospholipids <2:1, the system mainly relies on phospholipid film formation. Although the emulsifying ability is strong, the microcapsule shell formed is prone to rupture in alkaline or strong surfactant environments (such as shampoo), leading to tea oil leakage. If the proportion of modified cyclodextrin is too high, such as a mass ratio of modified cyclodextrin to natural phospholipids >3:1, although the inclusion ability is strong, cyclodextrin molecules are prone to self-polymerization through hydrogen bonds, resulting in a sharp increase in system viscosity and even gelation. This leads to excessive homogenization resistance in subsequent high-pressure microjets and may even block microchannels.
[0035] Furthermore, the total mass of the two components should account for 15%-20% of the total mass of the aqueous phase of the wall material. This is a good range that balances high-concentration encapsulation with suitable flowability. If the total mass is less than 15%, the wall material is insufficient to completely encapsulate the tea oil, leading to an increase in free oil droplets and exposed oil droplets on the surface of the microcapsules, making the product highly susceptible to oxidation and rancidity. If the total mass is greater than 20%, the viscosity of the system increases exponentially. Although the encapsulation rate is high, atomization is difficult during subsequent spray drying, easily forming large particles or even preventing powder from being extruded.
[0036] By precisely controlling the wall material concentration and compounding ratio within this range, a balance between encapsulation rate and process feasibility was achieved.
[0037] Step S2: Cold-pressed tea oil is mixed with natural antioxidants to form an oil phase. Under high-speed shearing conditions, the oil phase is slowly added to the aqueous phase of the wall material to carry out coarse emulsification and obtain a primary emulsion.
[0038] Cold-pressed tea oil is extracted from tea seeds using physical cold-pressing technology, with the entire processing temperature below 60℃, thus preserving the natural active ingredients such as squalene, vitamin E, and sterols to the greatest extent. However, these active ingredients, rich in unsaturated double bonds, are highly susceptible to free radical chain oxidation reactions upon contact with air, light, and moisture. To construct the first line of antioxidant protection before emulsification and encapsulation, this application introduces natural antioxidants into the oil phase preparation stage for premixing and compounding.
[0039] In some embodiments, see Figure 3 , Figure 3 This is a schematic flowchart of an embodiment of step S2 in the preparation process provided in this application. Step S2 includes: Step S21: Preheat the cold-pressed tea oil to 30℃-40℃, add 0.5%-1.5% of natural antioxidants by weight of the tea oil, and stir until completely dissolved to form the oil phase; Step S22: Preheat the aqueous phase of the wall material to 35℃-45℃, place it in a high-shear emulsification tank, and set the shear speed to 8000-12000 rpm; Step S23: While maintaining shearing, the oil phase is added to the aqueous phase of the wall material at a uniform rate by atomization spraying. After the addition is complete, shearing continues for 10-20 minutes to obtain a primary emulsion with a particle size of 1-5μm.
[0040] Specifically, in step S21, the cold-pressed tea oil is preheated to 30℃-40℃. The purpose of preheating is twofold: first, to moderately reduce the viscosity of the tea oil and improve its fluidity, allowing it to be more quickly torn into tiny droplets by shear force when the aqueous phase is added subsequently; second, to accelerate the dissolution and diffusion of natural antioxidants in the oil phase. However, the preheating temperature is strictly limited to below 40℃. If the temperature exceeds 40℃, although the viscosity further decreases, the heat-sensitive vitamin E and sterol components in the tea oil begin to show signs of degradation, and excessively high temperatures will reduce the interfacial tension gradient at the oil-water interface during subsequent emulsification, which is detrimental to emulsion stability. Conversely, if the temperature is below 30℃, the viscosity of the tea oil is high, requiring more mechanical energy to be consumed during subsequent high-speed shearing, and it is prone to localized uneven concentration and clumping.
[0041] Furthermore, in step S21, the natural antioxidant is a composite antioxidant composed of rosemary extract, tea polyphenols, and vitamin E in a mass ratio of 1:1:2. This specific ratio of composite antioxidant is tailored to the oxidation mechanism of tea oil in water-based cleansing systems. The main components of rosemary extract are carrageenan and carrageenanol. Rosemary extract has a strong singlet oxygen quenching ability, acting as the first line of defense to block the photo-oxidation process. Tea polyphenols are highly water-soluble but, due to their amphiphilic nature, can accumulate at the oil-water interface, effectively scavenging free radicals in the aqueous phase. Vitamin E is a classic oil-soluble chain inhibitor, penetrating deep into the oil phase to block the chain growth of carbon-centered free radicals. The three components, combined in a 1:1:2 ratio, not only form a comprehensive three-dimensional antioxidant network in the water and oil phases and at the interface, but also, due to the regenerative synergistic effect of tea polyphenols and rosemary extract on vitamin E, the antioxidant durability is increased several times. If only a single antioxidant is used, even if the amount added is increased to 3%, it is still difficult to prevent tea oil from becoming rancid and deteriorating within 3 months in the high moisture content and surfactant solubilization environment of the washing and care products.
[0042] In step S22, the aqueous phase of the wall material is preheated to 35℃-45℃. Preheating optimizes the liquid crystal flowability of phospholipid molecules in the wall material, facilitating their rapid migration to the newly formed oil-water interface and the formation of a dense protective film during shearing. The shearing speed of the high-shear emulsification tank is set to 8000-12000 rpm. This high-speed range is a key mechanical condition for breaking the macroscopic oil-water layer and forming a micron-sized primary emulsion. At such high linear velocities, the fluid generates strong turbulence and centrifugal force, tearing the oil phase into droplets. If the speed is below 8000 rpm, the shear energy is insufficient to overcome the cohesive force of the tea oil, resulting in coarse and unevenly distributed primary emulsion particles, severely increasing the load on the subsequent high-pressure micro-jet homogenizer, and even causing blockage of the high-pressure homogenization chamber. If the speed is above 12000 rpm, although the particle size decreases, the large amount of mechanical heat generated by the intense friction between the rotor and the fluid will cause the local temperature to rise sharply by more than 50℃, which not only damages the phospholipid wall material structure but also accelerates the degradation of heat-sensitive components in the tea oil.
[0043] In step S23, the oil phase is added uniformly to the aqueous phase of the wall material using an atomized spray method. Traditional oil-pouring methods cause a large amount of oil phase to come into instantaneous contact with a localized aqueous phase, resulting in the aqueous phase being instantly encapsulated by the oil phase and generating a large number of free oil droplets. Atomized spraying, however, allows the oil phase to be uniformly distributed on the surface of the aqueous phase in the form of extremely fine droplets. Under continuous shearing at 8000-12000 rpm, these fine oil droplets are rapidly entrained into the fluid and further torn apart. After the addition is complete, shearing continues for 10-20 minutes to allow the wall material molecules (cyclodextrin and phospholipids) to fully self-assemble and arrange on the oil droplet surface, achieving a dynamically balanced emulsion state, ultimately producing a primary emulsion with a particle size of 1-5 μm. Controlling the primary emulsion particle size to 1-5 μm ensures the uniformity of subsequent microjets for homogeneous feeding and prevents excessively large particles from causing localized stress concentration and mechanical wear in the homogeneous microchannels.
[0044] Extensive experimental verification has shown that if the initial emulsion particle size is greater than 5 μm, subsequent microjets require pressures exceeding 180 MPa to achieve nanoscale performance, leading to increased equipment wear and uncontrolled thermal runaway. Conversely, if the initial emulsion particle size is less than 1 μm, it not only places stringent demands on high-shear equipment but also results in severe unstable agglomeration even before high-pressure homogenization. Therefore, 1-5 μm represents an optimal particle size range that balances downstream process feasibility with system stability.
[0045] Step S3: Pass the primary emulsion into a high-pressure microfluidic homogenizing system and homogenize it 2-4 times under a pressure of 80-150MPa to obtain a nanoscale microemulsion.
[0046] Unlike traditional high-pressure valve homogenizers that rely on the physical impact between the valve seat and the impact ring, microjet homogenizers use high-pressure pumps to force fluid into fixed microchannels at the micrometer level. The fluid is accelerated to extremely high speeds within the channels, and then undergoes violent collisions, cavitation effects, and high-frequency shearing within the Y-shaped interactive collision chamber. This multidimensional and complex mechanical action can instantly pulverize micrometer-sized droplets to the nanometer level.
[0047] In some embodiments, see Figure 4 , Figure 4 This is a schematic flowchart of an embodiment of step S3 in the preparation process provided in this application. Step S3 includes: S31: Before the primary emulsion is fed into the reaction chamber of the micro-jet homogenizer through a high-pressure plunger pump, it is pre-cooled to control the material inlet temperature at 20℃-25℃. S32: In the Y-shaped interactive collision chamber of the micro-jet homogenizer, the first-stage homogenization pressure is set to 100-120MPa, and the second-stage homogenization pressure is set to 80-90MPa for continuous cyclic homogenization. S33: After homogenization, the material is quickly cooled to 10℃-15℃ through a plate heat exchanger to obtain a nanoscale microemulsion with an average particle size of 50-200nm and a polydispersity index of 0.2-0.3.
[0048] Specifically, in step S31, the high-pressure homogenization process is essentially a conversion of mechanical energy into thermal energy. When the fluid passes through a microchannel with an extremely high pressure differential, intense internal friction and cavitation collapse release enormous amounts of heat. Without temperature intervention, a single homogenization cycle can cause the material temperature to soar to over 40°C-60°C, which is fatal for tea oil rich in unsaturated fatty acids. The high temperature not only directly leads to the large-scale decomposition of vitamin E and squalene, but also triggers the thermal degradation phase transition of the phospholipid wall material, completely destroying the emulsion stability.
[0049] Therefore, in this embodiment, the material is pre-cooled before entering the reaction chamber of the microfluidic homogenizer, controlling the material inlet temperature to be between 20°C and 25°C. This temperature range is derived through precise thermodynamic calculations: assuming a temperature rise of approximately 30°C per cycle, an inlet temperature of 20°C to 25°C ensures that the outlet temperature remains below the safe critical line of 50°C to 55°C. Furthermore, temperatures above 20°C maintain good fluidity of phospholipid molecules in the aqueous phase of the wall material, preventing the phospholipids from transitioning to a gel state due to excessively low temperatures and clogging the pipes.
[0050] Furthermore, in step S31, pre-cooling is achieved by circulating 5℃-10℃ cooling water through a jacketed material tank, and a 1-10μm pore size filter is installed on the pipeline before the material enters the reaction chamber for filtration and impurity removal. The 5℃-10℃ cooling water continuously removes accumulated heat during dynamic feeding, maintaining a constant inlet temperature. The 1-10μm filter is a necessary protective measure for the delicate diamond / ceramic microchannels of the microfluidic device. Since the primary emulsion may contain incompletely dissolved cyclodextrin agglomerates or external impurity particles, if these impurities larger than the microchannel diameter enter the high-pressure zone, they will directly cause irreversible physical blockage or even rupture of the microchannels. A 1-10μm filtration precision effectively intercepts all potentially destructive impurities without generating excessive pipeline resistance that could affect the high-pressure pump's suction efficiency.
[0051] In step S32, within the Y-shaped interactive collision chamber of the microfluidic homogenizer, the fluid is split into two streams, which collide at high speed at their confluence. The first-stage homogenization pressure is set to 100-120 MPa, and the second-stage homogenization pressure is set to 80-90 MPa, for continuous cyclic homogenization. The first-stage homogenization pressure is mainly used to provide the primary energy for pulverizing the droplets; a pressure of 100-120 MPa is sufficient to allow the droplets to withstand enormous tearing stress and cavitation effects within a very short residence time. The second-stage homogenization pressure is slightly lower, and its main function is to prevent the high-kinetic-energy nanodroplets formed in the first stage from re-aggregating due to a sudden pressure drop upon exiting the chamber, i.e., to provide a back pressure effect.
[0052] Furthermore, in step S32, the microchannel diameter of the Y-shaped interactive collision chamber is 50-100 micrometers, and the homogenization cycle is specifically 3-4 times. The microchannel diameter directly determines the maximum velocity and shear force that the fluid can achieve. A diameter of 50-100 micrometers is the optimal size for balancing the pulverizing effect and the equipment lifespan. If the microchannel is less than 50 micrometers, although the increased flow rate can generate stronger pulverizing force, it is easily blocked by large particles or scale in high-concentration emulsions, and the requirements for the seals of the high-pressure pump are extremely stringent, leading to a surge in equipment failure rate. If the microchannel is greater than 100 micrometers, the flow rate is significantly reduced, and the cavitation effect and shear force generated under the same pressure are insufficient to break the surface tension of the tea oil droplets, resulting in the particle size remaining at the micrometer level after homogenization.
[0053] The homogenization cycle is 3-4 times because droplet refinement is an energy accumulation process. After the first cycle, large droplets are broken down into medium-sized droplets, but the particle size distribution is relatively wide and the polydispersity index is high. After the second and third cycles, energy is further applied to the more stubborn large droplets, and the particle size distribution narrows rapidly. By the fourth cycle, the system basically reaches the balance point between energy and particle size. If the cycle is continued for more than 5 times, not only will the particle size no longer decrease significantly, but it will also increase the energy consumption of the equipment and bring the risk of temperature rise runaway.
[0054] In step S33, after homogenization, the material is rapidly cooled to 10℃-15℃ using a plate heat exchanger to obtain a nanoscale microemulsion with an average particle size of 50-200 nm and a polydispersity index of 0.2-0.3. Rapid cooling is necessary to freeze the newly formed nanoscale interfacial film. Because nanoscale droplets possess extremely high surface free energy, maintaining high temperatures can easily lead to Brownian collisions between droplets, resulting in aggregation and demulsification. Cooling to 10℃-15℃ reduces the kinetic energy of water molecules, increases the rigidity of the interfacial film, and significantly improves the thermodynamic stability of the microemulsion.
[0055] Furthermore, the preparation of nanoscale microemulsions with an average particle size of 50-200 nm and a polydispersity index (PDI) of 0.2-0.3 has significant application advantages. On the one hand, the particle size range of 50-200 nm is much smaller than the wavelength of visible light (400-700 nm). According to the Rayleigh scattering principle, this microemulsion scatters light very weakly, exhibiting a transparent or bluish translucent state. This allows tea oil to be added in large quantities to a transparent and clear shampoo and body wash gel system without affecting the product's appearance. On the other hand, the specific surface area of nanoscale droplets increases geometrically, which not only allows tea oil to be instantly and evenly distributed with the water flow during rinsing, avoiding localized oiliness, but also increases its contact area with the scalp and body stratum corneum, facilitating the targeted release of subsequent microcapsules.
[0056] A polydispersity index (PDI) between 0.2 and 0.3 indicates a narrow and uniform particle size distribution in the emulsion. If the PDI is greater than 0.3, it indicates a mixture of small and large droplets in the system. During long-term settling, due to the Ostwald ripening effect, the small droplets dissolve and deposit on the large droplets, causing the emulsion to rapidly separate. Forcing a PDI below 0.2 requires extremely high homogenization pressure and frequency, which is very costly in industrial production and severely damages the activity of the tea oil.
[0057] Step S4: After mixing the nano-scale microemulsion with the low-temperature excipient, the mixture is spray-dried at a low temperature of 40℃-60℃ to collect the powder and obtain tea oil microcapsules.
[0058] Although the nanoscale microemulsion prepared by high-pressure microjets exhibits extremely high kinetic stability, it is still essentially a thermodynamically unstable system and contains a large amount of water, making it unsuitable for long-term storage or addition as a dry powder to washing and care formulations. It must undergo drying and curing treatment to remove the moisture, allowing the wall material to form an irreversible, solid, dense protective film on the oil droplet surface.
[0059] Traditional spray drying typically employs high-temperature air intake of 150℃-220℃ to achieve rapid evaporation and high powder yield. However, for tea oil microemulsions rich in heat-sensitive active substances, the instantaneous high-temperature treatment can cause the phospholipid film on the surface of the nanodroplets to rupture or undergo a phase transition. The inclusion structure of cyclodextrin can also collapse due to rapid moisture loss, resulting in the tea oil inside being directly exposed to high temperatures. This can instantly trigger severe oxidative rancidity and damage to the active ingredients. At the same time, the high temperature can cause the surface of the microcapsule particles to melt and agglomerate, forming non-flowing dead powder.
[0060] Therefore, this embodiment adopts a process route that combines low-temperature spray drying with specific excipients.
[0061] In some embodiments, see Figure 5 , Figure 5 This is a schematic flowchart of an embodiment of step S4 in the preparation process provided in this application. Step S4 includes: S41: Dissolve the low-temperature excipient in purified water to prepare an excipient aqueous solution with a mass concentration of 20%-30%, and mix it evenly with the nanoscale microemulsion at a volume ratio of 1:0.8-1:1.2; S42: The mixture is fed into a low-temperature spray drying tower, with the inlet air temperature set at 45℃-55℃, the outlet air temperature at 30℃-35℃, and the atomization pressure at 0.2-0.3MPa; S43: The powder is collected by a cyclone separator at the bottom of the tower and sieved through a 40-60 mesh vibrating screen to obtain tea oil microcapsules with a moisture content of 1%-3%.
[0062] Specifically, in step S41, a low-temperature excipient is introduced. Because nanodroplets constructed solely from cyclodextrin and phospholipids lack sufficient skeletal support during water evaporation, they are highly susceptible to shell breakage during drying shrinkage. The low-temperature excipient is a mixture of maltodextrin and gum arabic in a mass ratio of 2:1 to 4:1. Maltodextrin possesses excellent water solubility and low viscosity, enabling it to rapidly occupy space during water evaporation and form a robust glassy carbohydrate skeleton. Gum arabic, as a natural plant gum, contains a large amount of arabinogalactan, which not only forms a thick and dense film on the oil droplet surface but also exhibits excellent emulsifying and stabilizing properties. The 2:1 to 4:1 ratio of the two ensures film strength during drying while avoiding the problem of excessive viscosity and difficulty in atomization caused by excessive gum arabic.
[0063] The mass concentration of the excipient aqueous solution is controlled between 20% and 30%. If the concentration is below 20%, the excipient is insufficient to form a continuous skeleton, and the powder is easily brittle after drying, resulting in a decrease in encapsulation efficiency. If the concentration is above 30%, the viscosity of the mixture increases dramatically, easily clogging the nozzles of the spray drying tower, and moisture diffusion is difficult at low temperatures, leading to excessive moisture content in the powder. A volume ratio of 1:0.8 to 1:1.2 ensures a perfect match between the active ingredients and excipients in the microemulsion, balancing the oil loading rate and physical strength of the final microcapsules.
[0064] In step S42, the mixture is fed into a low-temperature spray drying tower, with the inlet air temperature set at 45℃-55℃. This temperature range is much lower than that of traditional processes, but slightly higher than the boiling point of water. Because the microemulsion is atomized into extremely small droplets with a very large surface area, the moisture on the droplet surface evaporates within milliseconds in the flowing hot air, forming a dry outer shell. As the shell forms, the resistance to the outward diffusion of internal moisture increases. At this point, the outlet air temperature is maintained at 30℃-35℃. The outlet air temperature essentially reflects the intensity of evaporation within the tower. If the outlet air temperature is too low, it indicates that the moisture has not completely evaporated, and the powder is prone to sticking to the walls and clumping; if the outlet air temperature is too high, it means that the material has been overheated. The atomization pressure is set to 0.2-0.3 MPa to ensure that the mixture is torn into uniform, extremely fine droplets by the centrifugal atomizer, increasing the evaporation efficiency at low temperatures, but without excessive pressure that would cause the droplets to be too small and be directly carried away by the exhaust air, resulting in losses.
[0065] Furthermore, in step S42, a cold air dehumidification device is installed inside the low-temperature spray drying tower to control the relative humidity of the incoming air at 20%-30% to prevent the material from sticking to the walls of the drying tower. Because the incoming air temperature drops to 45℃-55℃, the saturated moisture content of the hot air is much lower than that at 150℃. If the ambient air humidity is high and directly heated before being sent into the tower, although the air can provide heat when it comes into contact with the droplets, its relative humidity is already close to saturation, and it cannot continue to absorb the evaporated water vapor, causing the droplets to remain moist for a long time, adhering to the tower wall and ultimately leading to drying failure. By using the cold air dehumidification device, the ambient air is first cooled and dehumidified to a relative humidity of 20%-30%, and then heated to the incoming air temperature. At this point, the moisture absorption capacity of the hot air is greatly improved, achieving efficient dehydration and drying even at low temperatures. This completely solves the industrial pain points of low-temperature spray drying, such as easy wall adhesion and low powder collection rate, making the entire low-temperature process feasible for mass production.
[0066] In step S43, the powder is collected under negative pressure by a cyclone separator at the bottom of the tower. Having undergone thorough dehumidification and drying with cold air, the powder is in the form of free-flowing fine particles. It is then sieved through a 40-60 mesh vibrating sieve to remove a few large particle aggregates that may have resulted from uneven atomization, ultimately yielding tea oil microcapsules with a moisture content of 1%-3%. Moisture content is a key indicator determining the long-term stability of the microcapsules. If the moisture content exceeds 3%, the wall materials inside the microcapsules, such as maltodextrin, are in a rubbery state below the glass transition temperature, with relatively active molecular motion, allowing oxygen to easily penetrate, and the tea oil will begin to oxidize and become rancid within a few weeks. Forcibly reducing the moisture content to below 1% would require extending the heating time or significantly increasing the air temperature, which would be counterproductive. Therefore, a moisture content of 1%-3% ensures that the microcapsules remain in a brittle glassy state, preventing oxygen penetration, while avoiding energy waste and the risk of thermal damage caused by excessive drying.
[0067] Step S5: Mix the tea oil microcapsules with the surfactant system and functional additives in a preset order, cool to below 35°C and add an acidic pH adjuster to obtain a three-in-one shampoo, conditioner and body wash product.
[0068] The core contradiction of 3-in-1 products lies in the fact that shampoo needs strong degreasing power and oil control for a voluminous feel, while body wash needs moisturizing and lubrication to prevent moisture loss. Traditional processes often fail to address both aspects. This embodiment, through a specific surfactant compound system, a strict order of ingredient addition, and a low-temperature cold-mixing process, endows microcapsules with differentiated mechanisms of action in different areas (hair and skin).
[0069] In some embodiments, see Figure 6 , Figure 6 This is a schematic flowchart of an embodiment of step S5 in the preparation process provided in this application. Step S5 includes: Step S51: Dissolve the amino acid-based surfactant in deionized water, heat to 38℃-42℃ and stir to dissolve, then add humectant and thickener, and stir until completely transparent; Step S52: When the system cools down to 32℃-35℃, add the tea oil microcapsules and disperse them evenly by low-speed shearing and stirring to avoid damaging the microcapsule structure; Step S53: Add a citric acid aqueous solution with a mass concentration of 5%-15% to adjust the pH value of the system to 5.0-5.5. Finally, add preservatives and fragrances, and the product is ready to be discharged as a three-in-one shampoo and conditioner.
[0070] Specifically, in step S51, the amino acid-based surfactant is a combination of sodium cocoyl glutamate and sodium lauroyl methanesulfonate. Amino acid surfactants are prized for their extreme mildness and excellent biodegradability; however, single amino acid surfactants often suffer from insufficient foaming and weak degreasing power, making it difficult to provide a refreshing feeling when rinsing. This embodiment uses a combination of sodium cocoyl glutamate and sodium lauroyl methanesulfonate. Sodium cocoyl glutamate is slightly acidic, has good foaming power, and is gentle on the scalp; sodium lauroyl methanesulfonate has strong cleaning power and can produce rich, dense foam. The latter not only compensates for the former's insufficient cleaning power but also forms a smooth, keratin-like film on the scalp and hair surface. Both are dissolved in deionized water and heated to 38℃-42℃ while stirring to dissolve. Heating is necessary because thickeners are difficult to hydrate and disperse quickly at room temperature, easily forming white clumps with a wet exterior and a dry interior. Heating to 38℃-42℃ can accelerate the hydration and swelling process of polymeric thickeners, allowing the system to quickly form a transparent and uniform gel matrix. However, the temperature is strictly limited to below 42℃. If this temperature is exceeded, the molecular chains of some natural thickeners may break, leading to a decrease in the final system viscosity. Furthermore, excessively high temperatures can generate thermal stress when microcapsules are added.
[0071] In step S52, when the system cools to 32℃-35℃, tea oil microcapsules are added, and low-speed shear stirring is used to disperse them evenly. The core of this step lies in "cooling" and "low speed". Cooling to 32℃-35℃ is because the tea oil microcapsule wall material prepared above contains natural phospholipids and maltodextrin. Natural phospholipids have a specific phase transition temperature, generally exhibiting a partial liquid crystal transition region around 35℃. If added to the surfactant solution at a high temperature above 38℃, the solubilizing effect of the surfactant micelles will strongly insert into the phospholipid bilayer, causing the microcapsule wall material structure to swell or even rupture, resulting in premature release of tea oil and its floating precipitation in the system. After cooling to 32℃-35℃, the phospholipid wall material is in a relatively rigid gel state, which can effectively resist the penetration and damage of surfactants. At the same time, low-speed shear stirring at 300-500 rpm must be used. This is because although the microcapsules are reinforced by low-temperature spray drying, they can still be mechanically pulverized under high shear force. Low-speed stirring can utilize the suspending force of the gel matrix to suspend the microcapsules evenly, while also preserving the core-shell structure of the microcapsules, laying the physical foundation for their intelligent release during subsequent shampooing and bathing.
[0072] In step S53, a 5%-15% citric acid aqueous solution is added to adjust the pH of the system to 5.0-5.5. Finally, preservatives and fragrances are added, and the product is discharged to obtain a three-in-one shampoo and conditioner. pH adjustment in a three-in-one shampoo and conditioner system is not only a requirement for gentleness but also crucial for microecological balance and efficacy. The natural slightly acidic pH of the scalp and body skin is typically between 4.5 and 5.5. Adjusting the system pH to 5.0-5.5 creates a slightly acidic environment that effectively inhibits the abnormal growth of Malassezia scalp, the core colony causing dandruff and itching. It also protects the filaggrin in the stratum corneum from damage, maintaining the skin's moisture barrier. Furthermore, the slightly acidic environment allows the amino acid surfactant molecules to be in their optimal ionization state, resulting in the densest and most stable foam. Finally, preservatives and fragrances are added and stirred at a low temperature to prevent fragrance evaporation or preservative decomposition due to high temperatures.
[0073] Thus, the three-in-one shampoo and conditioner produced has the following effects: during shampooing, the microcapsules experience less mechanical friction and are washed away with the water flow, allowing the amino acid surfactants to exert a refreshing, oil-controlling, and dandruff-removing effect without leaving the scalp oily; while during showering, the microcapsules rupture under the rubbing of a bath sponge and the heating of body temperature, releasing nano-level tea oil for deep moisturizing and repair, perfectly meeting the dual needs of oil control in shampooing and moisturizing in showering.
[0074] This application utilizes biodegradable amphiphilic macromolecules as the composite wall material. High-pressure microfluidic homogenization breaks down tea oil to the nanoscale, and a composite antioxidant of rosemary extract, tea polyphenols, and vitamin E is incorporated into the core material. This nanoscale encapsulation allows the tea oil to disperse instantly in water-based cleansing systems without leaving any floating oil. The synergistic effect of the composite wall material and antioxidants, combined with a low-temperature spray drying process, significantly improves the water solubility and antioxidant stability of the tea oil, preventing oxidative rancidity caused by high temperatures and greatly extending the product's shelf life.
[0075] The tea oil microcapsules prepared in this application maintain their structural integrity within the surfactant system. During shampooing, the microcapsules primarily function as physical lubricants and are washed away with water, preventing the hair from becoming flat and the scalp from becoming oily due to the direct adhesion of large-molecule oils. During bathing, the microcapsules slowly rupture in the stratum corneum of the body through friction with body temperature, releasing the active ingredients of tea oil and achieving long-lasting deep moisturizing. This achieves multiple benefits in one bottle, effectively removing dandruff, controlling oil, moisturizing, and preventing dryness and itching.
[0076] The preparation process of this application adopts a technical route that combines low-temperature cold mixing and low-temperature spray drying. The highest temperature throughout the process does not exceed 60°C. Compared with traditional high-temperature homogenization and spraying processes, this significantly reduces heat energy consumption and thoroughly protects the heat-sensitive active substances such as vitamin E and squalene in tea oil from damage, thereby improving the bioavailability and efficacy of the product.
[0077] The above description is merely an embodiment of this application and does not limit the patent scope of this application. Any equivalent structural or procedural transformations made using the content of this application's specification and drawings, or direct or indirect applications in other related technical fields, are similarly included within the patent protection scope of this application.
Claims
1. A preparation process for a three-in-one shampoo and conditioner product, characterized in that, include: S1: The biodegradable amphiphilic macromolecular wall material is mixed with purified water and stirred at 40℃-50℃ to obtain the aqueous phase of the wall material; S2: Cold-pressed tea oil is mixed with natural antioxidants to form an oil phase. The oil phase is slowly added to the aqueous phase of the wall material under high-speed shearing conditions to carry out coarse emulsification and obtain a primary emulsion. S3: The primary emulsion is passed into a high-pressure microfluidic homogenizing system and homogenized 2-4 times under a pressure of 80-150MPa to obtain a nanoscale microemulsion. S4: The nanoscale microemulsion is mixed with a low-temperature excipient and then spray-dried at a low temperature of 40℃-60℃. The powder is collected to obtain tea oil microcapsules. S5: Mix the tea oil microcapsules with the surfactant system and functional additives in a preset order, cool to below 35°C and add an acidic pH adjuster to obtain a three-in-one shampoo, conditioner and body wash product.
2. The preparation process according to claim 1, characterized in that, Step S1 includes: S11: Dissolve the modified cyclodextrin in the purified water in the first part, and stir at 300-500 rpm for 15-25 minutes at 40℃-45℃ until completely dissolved; S12: Disperse natural phospholipids in the purified water of the second part and perform hydration and swelling. The hydration temperature is 40℃-50℃ and the swelling time is 20-40 minutes. S13: Combine the solution obtained in S11 with the dispersion obtained in S12, and stir in a homogenizer at 4000-6000 rpm for 3-8 minutes to form a uniform aqueous phase of the wall material.
3. The preparation process according to claim 2, characterized in that, In step S11, the modified cyclodextrin is one of hydroxypropyl-β-cyclodextrin or octyl-β-cyclodextrin; in step S12, the natural phospholipid is soybean lecithin or hydrogenated phospholipid. The mass ratio of the modified cyclodextrin to the natural phospholipid is 2:1-3:1, and the total mass of the two accounts for 15%-20% of the total mass of the aqueous phase of the wall material.
4. The preparation process according to claim 1, characterized in that, Step S2 includes: S21: Preheat cold-pressed tea oil to 30℃-40℃, add 0.5%-1.5% of natural antioxidants by weight of tea oil, and stir until completely dissolved to form the oil phase; S22: Preheat the aqueous phase of the wall material to 35℃-45℃, place it in a high-shear emulsification tank, and set the shear speed to 8000-12000 rpm; S23: While maintaining shearing, the oil phase is added to the aqueous phase of the wall material at a uniform rate by atomization spraying. After the addition is completed, shearing continues for 10-20 minutes to obtain a primary emulsion with a particle size of 1-5μm.
5. The preparation process according to claim 4, characterized in that, In step S21, the natural antioxidant is a composite antioxidant composed of rosemary extract, tea polyphenols, and vitamin E in a mass ratio of 1:1:
2.
6. The preparation process according to claim 1, characterized in that, Step S3 includes: S31: Before the primary emulsion is fed into the reaction chamber of the micro-jet homogenizer by a high-pressure plunger pump, it is pre-cooled to control the material inlet temperature at 20℃-25℃. S32: In the Y-shaped interactive collision chamber of the micro-jet homogenizer, the first-stage homogenization pressure is set to 100-120MPa, and the second-stage homogenization pressure is set to 80-90MPa for continuous cyclic homogenization. S33: After homogenization, the material is quickly cooled to 10℃-15℃ through a plate heat exchanger to obtain a nanoscale microemulsion with an average particle size of 50-200nm and a polydispersity index of 0.2-0.
3.
7. The preparation process according to claim 1, characterized in that, Step S4 includes: S41: Dissolve the low-temperature excipient in purified water to prepare an excipient aqueous solution with a mass concentration of 20%-30%, and mix it evenly with the nanoscale microemulsion at a volume ratio of 1:0.8-1:1.2; S42: The mixture is fed into a low-temperature spray drying tower, with the inlet air temperature set at 45℃-55℃, the outlet air temperature at 30℃-35℃, and the atomization pressure at 0.2-0.3MPa; S43: The powder is collected by a cyclone separator at the bottom of the tower and sieved through a 40-60 mesh vibrating screen to obtain tea oil microcapsules with a moisture content of 1%-3%.
8. The preparation process according to claim 7, characterized in that, In step S41, the low-temperature excipient is a mixture of maltodextrin and gum arabic in a mass ratio of 2:1 to 4:
1.
9. The preparation process according to claim 1, characterized in that, Step S5 includes: S51: Dissolve the amino acid-based surfactant in deionized water, heat to 38℃-42℃ and stir to dissolve, then add humectant and thickener, and stir until completely transparent; S52: When the system cools down to 32℃-35℃, add the tea oil microcapsules and disperse them evenly by low-speed shearing and stirring to avoid damaging the microcapsule structure. S53: Add a 5%-15% citric acid aqueous solution to adjust the pH of the system to 5.0-5.
5. Finally, add preservatives and fragrances, and the product is ready to be dispensed as a three-in-one shampoo and conditioner.
10. The preparation process according to claim 9, characterized in that, In step S51, the amino acid-based surfactant is a combination of sodium cocoyl glutamate and sodium lauroyl hydroxymethyl sulfonate; in step S52, the rotational speed of the low-speed shearing is 300-500 rpm.