Flower micro-capsule cleaning granular powder, preparation method thereof and cleaning care product

Abstract

The invention discloses flower micro-capsule cleaning particle powder and a preparation method thereof. The particle powder comprises 30-40% of a carrier and forming agent, 30-45% of a surfactant, 5-15% of a conditioning and repairing agent, 5-12% of a disintegration and dissolution promoter, 3-8% of a core functional component and 1.5-3.0% of a fragrance protection micro-capsule agent. The carrier and the forming agent comprise corn starch, hydrophobic fumed silica and vitamin E; the surface active agent is prepared from sodium cocoyl isethionate, sodium methyl cocoyl taurate, coconut oil acyl propyl betaine and APG1214; the conditioning and repairing agent comprises a cationic conditioning agent, a humectant and a skin conditioning agent; the disintegration and dissolution promoter comprises polyvinylpolypyrrolidone, microcrystalline cellulose and a sodium bicarbonate-citric acid gas production pair; the core functional components comprise radiation-resistant composite enzyme powder and flower components. The product disclosed by the invention has the advantages of instant collapse when encountering water, abundant foam, lasting fragrance (not less than 36 hours), high active matter retention rate, stable color system, no chemical preservative, stable storage and the like. The invention further provides a cleaning and nursing article.

Description

Technical Field

[0001] This invention relates to the field of daily chemical cleaning products technology, and in particular to a flower microcapsule cleaning granule powder, its preparation method, and cleaning and care products. Background Technology

[0002] With the increasing demand from consumers for natural, environmentally friendly, and safe personal care products, solid cleaning products featuring flower and plant extracts (such as facial cleansing granules, shower gels, and shampoo powders) have become a market hotspot. These products are favored for their environmental friendliness, portability, and gentleness. However, existing technological solutions face a series of insurmountable technical bottlenecks in achieving a balance between product functionality, stability, and user experience, as detailed below:

[0003] First, the retention rate of natural active ingredients is low and the color is unstable. The core active ingredients in flowers, such as polyphenols and flavonoids, as well as natural pigments, are all heat-sensitive. Current technologies mostly use traditional hot air drying (e.g., above 80℃) or hot water extraction processes to treat flower raw materials, leading to significant degradation of active ingredients and oxidative fading of pigments. The total polyphenol retention rate is generally below 80%, resulting in uneven product color and large batch-to-batch color differences (ΔE>1.5), failing to meet consumers' dual expectations of "natural effectiveness" and "visual appeal."

[0004] Second, long-term storage without preservatives is difficult to achieve and relies on high-cost packaging. To ensure microbial safety, existing technologies typically employ two approaches: one is to add chemically synthesized preservatives, which contradicts the "natural" positioning and may cause skin irritation; the other is to rely on special packaging such as vacuum or nitrogen filling to isolate moisture and oxygen. This not only significantly increases production costs, but also makes the product highly susceptible to moisture absorption, clumping, and even mold growth after packaging damage, easily leading to excessive total microbial counts (>1000 CFU / g) and poor long-term storage stability.

[0005] Third, the user experience is poor, with slow dissolution and disintegration speeds. Many commercially available solid cleaning products (such as effervescent tablets) take tens of seconds to disintegrate, which can easily lead to clumping or incomplete dissolution, affecting the immediacy and richness of foam generation and significantly diminishing the user experience.

[0006] Fourth, the fragrance lacks staying power, failing to achieve simultaneous cleansing and long-lasting fragrance care. Existing products mostly use direct addition of fragrance, resulting in significant evaporation and loss of aroma during production and storage. When used, the fragrance is quickly released upon contact with water, leading to a short-lasting scent (usually <12 hours), which cannot meet consumers' demand for long-lasting body fragrance.

[0007] Fifth, the manufacturing process struggles to balance the protection of heat-sensitive ingredients with industrial-scale production. Existing solid detergent preparation processes (such as high-temperature drying and hot-melt granulation) cannot effectively protect the activity of heat-sensitive ingredients such as enzymes and flower extracts in large-scale production, resulting in a gap between the claimed efficacy and the actual effects of the final product.

[0008] In summary, existing technologies cannot synergistically address a series of interconnected pain points, including high activity retention, color stability, preservative-free storage, rapid disintegration, long-lasting fragrance, and industrial feasibility. Summary of the Invention

[0009] The purpose of this invention is to provide a floral microcapsule cleaning granule powder with high retention of active ingredients, stable color, no preservatives, easy storage, rapid disintegration, and long-lasting fragrance.

[0010] To achieve the above objectives, the present invention adopts the following technical solution:

[0011] A type of floral microcapsule cleansing granule powder, by weight, comprises 30-40% carrier and forming agent, 30-45% surfactant, 5-15% conditioning and repairing agent, 5-12% disintegrant and solubilizing agent, 3-8% core active ingredient, and 1.5-3.0% fragrance microcapsule agent; the carrier and forming agent includes corn starch, hydrophobic fumed silica, and vitamin E; the surfactant includes sodium cocoyl ethanesulfonate, sodium methyl cocoyl taurate, cocoyl propyl betaine, and APG1214; the conditioning and repairing agent includes cationic conditioning agent, moisturizer, and skin conditioning agent; the disintegrant and solubilizing agent includes crospovidone, microcrystalline cellulose, and sodium bicarbonate-citric acid gas-generating pair; the core active ingredient includes radiation-resistant compound enzyme powder and floral components; the fragrance microcapsule agent includes β-cyclodextrin, γ-cyclodextrin, polyurea microcapsule fragrance, and polyquaternium-39.

[0012] Furthermore, the floral components include plant extract powder and flower fragments prepared from one of the following: rose, butterfly pea, and marigold.

[0013] Furthermore, the radiation-resistant compound enzyme powder includes protease and lipase.

[0014] Furthermore, the cationic conditioner includes one or more of behenyltrimethylammonium chloride, polyquaternium-10, and cationic guar gum.

[0015] Furthermore, the moisturizers include one or more of panthenol, trehalose, and hydrolyzed keratin.

[0016] Furthermore, skin conditioning agents include allantoin and / or dipotassium glycyrrhizate.

[0017] According to the embodiments, a method for preparing the aforementioned flower microcapsule cleaning granule powder is also provided, which includes the following steps:

[0018] S1. Mix and emulsify β-cyclodextrin, γ-cyclodextrin, polyquaternium-39 with deionized water at 50-60℃, cool to 35-40℃, add polyurea microcapsule fragrance, stir evenly, and obtain fragrance-protecting microcapsule emulsion.

[0019] S2. Mix the remaining solid components, except for the fragrance microcapsule emulsion, evenly to obtain the basic premixed powder;

[0020] S3. Put the basic premixed powder into a fluidized bed granulator and dry it at an inlet air temperature of 75-95℃ and an outlet air temperature of 40-50℃.

[0021] S4. Adjust the inlet and outlet air temperatures to 30-40℃, maintain the material temperature at 35-45℃, and spray the fragrance microcapsule emulsion obtained in step S1 into the fluidized material through an atomizing nozzle. The atomization pressure is 0.12-0.22MPa.

[0022] S5. After spraying, maintain the inlet air temperature at 30-40℃ and continue fluidized drying for 15-20 minutes until the material moisture content is ≤5.0%. The discharged material is screened to obtain spherical particles with a particle size of 0.8-1.2mm.

[0023] S6. Place the particles obtained in step S5 in a cobalt-60 irradiation field and sterilize them by irradiation with a dose of 7-8 kGy at an ambient temperature of 27-29℃, then seal and package them.

[0024] Furthermore, the sterilized granules are sealed and packaged in aluminum foil composite bags or light-proof plastic bottles.

[0025] According to an embodiment, a cleaning and care product is also provided, which includes a facial cleanser, a bath product, or a shampoo product containing the aforementioned flower microcapsule cleaning particle powder.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] 1) High activity retention and color stability: The compound flower treatment process combined with vitamin E antioxidant properties ensures that the total polyphenol retention rate of flowers is ≥91%, the product color difference ΔE<1.0, and the color difference change ΔE after accelerated testing is also low. · <0.5;

[0028] 2) Achieve long-term preservation without preservatives: The three-level system of "low moisture content pretreatment of raw materials + precise water control in granulation + irradiation sterilization" reduces the water activity of the product to Aw<0.6. After 6 months of accelerated testing, the total number of microorganisms is still <10CFU / g, without the need for chemical preservatives and special packaging.

[0029] 3) Excellent user experience: The disintegration and solubilization system works synergistically to make the particles disintegrate instantly in less than 3 seconds after contact with water, producing rich and delicate foam without any lumps or residue;

[0030] 4) Breakthrough fragrance longevity: Through a triple mechanism of physical encapsulation, microcapsule sustained release, and cationic adsorption, the fragrance is effectively released for ≥36 hours, far exceeding existing products;

[0031] 5) Safe and environmentally friendly: All ingredients are compliant, free of chemical preservatives and synthetic dyes, with low skin irritation and a green production process;

[0032] 6) Strong industrial feasibility: precise process parameters, simplified steps, high compatibility with existing industrial equipment, high production efficiency, and easy industrialization. Detailed Implementation

[0033] The present invention will be further described in detail below through specific embodiments:

[0034] This solution provides a floral microcapsule cleansing granule powder, comprising 30-40% carrier and forming agent, 30-45% surfactant, 5-15% conditioning and repairing agent, 5-12% disintegrant and solubilizer, 3-8% core active ingredient, and 1.5-3.0% fragrance microcapsule agent; the carrier and forming agent includes corn starch, hydrophobic fumed silica, and vitamin E; the surfactant includes sodium cocoyl ethanesulfonate, sodium methyl cocoyl taurate, cocoyl propyl betaine, and APG1214; the conditioning and repairing agent includes cationic conditioning agents (one or more of behenyltrimethylammonium chloride, polyquaternium-10, and cationic guar gum), moisturizers (one or more of panthenol, trehalose, and hydrolyzed keratin), and skin conditioning agents (allantoin and / or dipotassium glycyrrhizate). The disintegration and solubilizing agents include cross-linked povidone, microcrystalline cellulose, and sodium bicarbonate-citric acid gas-producing pair; the core active ingredients include radiation-resistant compound enzyme powder (composed of protease and lipase in a 1:1 ratio, with an enzyme activity retention rate ≥85% after irradiation with 7-8 kGy cobalt-60 γ rays), floral components (floral components include plant extract powder and flower fragments prepared from one of rose, butterfly pea, and marigold as raw materials, wherein the water content of the plant extract powder is 4.5-4.9%, the water content of the flower fragments is 2.5-2.9%, and the particle size is 20-40 mesh); the fragrance microcapsule agents include β-cyclodextrin, γ-cyclodextrin, polyurea microcapsule fragrance (including one of polyurea microcapsule rose fragrance, polyurea microcapsule butterfly pea fragrance, and polyurea microcapsule marigold fragrance) and polyquaternium-39. It is prepared by the following method:

[0035] Fragrance-protecting microcapsule emulsion preparation: Mix β-cyclodextrin, γ-cyclodextrin, polyquaternium-39 with deionized water at 50-60℃, emulsify at high speed to form a homogeneous emulsion, cool to 35-40℃, add polyurea microcapsule fragrance, gently stir and disperse, and set aside; the amount of deionized water is 3-5 times the total weight of the above four components to ensure uniform dispersion of microcapsules and avoid aggregation;

[0036] Solid raw material premixing: The carrier, molding agent, surfactant, conditioning and repairing agent, disintegrating and solubilizing agent, radiation-resistant enzyme powder, and flower components are sequentially added to a three-dimensional motion mixer and mixed for 20 minutes to obtain the basic premixed powder;

[0037] Integrated fluidized bed low-temperature spray granulation:

[0038] a) Preheating and drying: The basic premixed powder is put into a fluidized bed granulator with an inlet air temperature of 75-95℃ and an outlet air temperature of 40-50℃. Fluidized preheating and drying removes excess moisture from the raw materials and prevents subsequent spray agglomeration.

[0039] b) Low-temperature spray coating: Adjust the inlet and outlet air temperature to 30-40℃ and maintain the material temperature at 35-45℃. Spray the fragrance microcapsule emulsion evenly into the fluidized material through a pressure atomizing nozzle (atomizing pressure 0.12-0.22MPa) so that the microcapsules are firmly attached to the surface of the particles.

[0040] c) Curing and drying: After spraying, maintain the inlet air temperature at 30-40℃ and continue fluidized drying for 15-20 minutes until the material moisture content is ≤5.0%. After discharge and sieving, spherical particles with a particle size of 0.8-1.2mm are obtained to ensure particle formability and microcapsule adhesion.

[0041] Irradiation terminal sterilization: The sieved particles are placed in a cobalt-60 irradiation field at an ambient temperature of 27-29℃ and irradiated with 7-8kGy gamma rays for 14-16 minutes to completely inactivate microorganisms without destroying the activity of the active ingredients, thus ensuring preservation-free storage.

[0042] Sealed packaging: In a clean environment, use aluminum foil composite bags or light-proof plastic bottles for sealed packaging to avoid the effects of light and moisture and ensure the long-term stability of the product.

[0043] Example 1

[0044] Corn starch 30.0%, hydrophobic fumed silica 2.0%, vitamin E 0.3%; sodium cocoyl ethanesulfonate 12.0%, sodium methyl cocoyl taurate 12.0%, cocoyl propyl betaine 8.0%, APG121 48.0%; behenyltrimethylammonium chloride 2.0%, polyquaternium-10 3.0%, cationic guar gum 2.0% (total cationic conditioning agent 7.0%), panthenol 0.5%, hydrolyzed keratin 0.5%, trehalose 0.5% (total moisturizer 1.5%), allantoin 0.3%. Dipotassium glycyrrhizate 0.2% (0.5% of total skin conditioning agent); crospovidone 3.0%, microcrystalline cellulose 4.0%, sodium bicarbonate 1.5%, citric acid 1.5%; radiation-resistant compound enzyme powder 1.0% (protease + lipase 1:1 compound, enzyme activity retention rate ≥85% after 7-8kGy cobalt-60 γ-ray irradiation), rose plant extract powder 3.0%, rose fragments (40 mesh) 4.5%; β-cyclodextrin 1.0%, γ-cyclodextrin 0.5%, polyurea microcapsule rose fragrance 0.4%, polyquaternium-39 0.2%.

[0045] 2. Preparation steps:

[0046] a) Flower pretreatment: Fresh roses were washed, crushed, and then quick-frozen in liquid nitrogen at -40℃ and freeze-dried under vacuum of <10Pa for 10 hours; the freeze-dried material was enzymatically hydrolyzed at 50℃ for 2.5 hours in a pH 6.2 buffer system, followed by hot water extraction at 85℃ for 1.5 hours; solid-liquid separation was performed, and the product was spray-dried in liquid phase to obtain rose extract powder (moisture content 4.7%), and then crushed and sieved in solid phase to obtain rose fragments (moisture content 2.7%, 40 mesh).

[0047] b) Preparation of Fragrance Microcapsule Emulsion: β-Cyclodextrin, γ-Cyclodextrin, polyquaternium-39 and 8 parts of 55°C deionized water are mixed, emulsified by high-speed shearing, cooled to 35°C and polyurea microcapsule rose fragrance is added, and gently stirred for later use; the amount of deionized water is 3-5 times the total weight of the above four components.

[0048] c) Premixing: All solid ingredients except for the fragrance microcapsule emulsion and rose petals are put into a three-dimensional motion mixer and mixed for 20 minutes (first 15 minutes, then add the rose petals and mix for another 5 minutes) to obtain the basic premixed powder;

[0049] d) Low-temperature spray granulation: The basic premixed powder is fed into a fluidized bed, preheated and dried with air inlet at 85°C and air outlet at 45°C; the inlet / outlet air temperature is adjusted to 35°C, the material temperature is maintained at 40°C, and the fragrance microcapsule emulsion is sprayed in at an atomization pressure of 0.18MPa; after spraying, drying is continued at 35°C for 18 minutes, and 0.8-1.2mm spherical particles (moisture content 4.6%) are obtained by sieving.

[0050] e) Irradiation sterilization: Irradiate with 7.5 kGy cobalt-60 γ rays for 15 minutes at 28°C;

[0051] f) Sealed packaging: Sealed packaging in aluminum foil composite bags under a Class 10,000 clean environment.

[0052] 3. Product Performance: Pink, uniform spherical granules; disintegrates in 2.8 seconds upon contact with water; total polyphenol retention rate is 91.3%; initial fragrance lasts 38.5 hours; ΔE=0.78; after 6 months of accelerated treatment at 40℃ and 75% RH, the total polyphenol retention rate is 82.1%; ΔE · =0.35, fragrance lasts for 31.7 hours, total microbial count <10 CFU / g, no clumping, no moisture absorption, and skin irritation score of 0.

[0053] Example 2

[0054] 1. Formulation composition: Same as in Example 1, except that the rose raw material is replaced with butterfly pea flower, and the polyurea microcapsule rose fragrance is replaced with polyurea microcapsule butterfly pea flower fragrance;

[0055] 2. Preparation steps: Same as in Example 1, with adjustments: flower pretreatment -38℃ liquid nitrogen quick-freezing, 48℃ enzymatic hydrolysis, 88℃ water extraction, freeze-drying for 9 hours to obtain butterfly pea flower plant extract powder (moisture content 4.6%) and butterfly pea flower fragments (30 mesh, moisture content 2.6%); during spraying, the material temperature is 33℃, the inlet / outlet air temperature is 33℃, the atomization pressure is 0.17MPa, and the drying time is 17 minutes.

[0056] 3. Product Performance: Sky blue granules, disintegration time 2.7 seconds, total polyphenol retention rate 91.0%, initial fragrance duration 37.8 hours, ΔE=0.84; after 6 months of accelerated treatment at 40℃ and 75% RH, the total polyphenol retention rate is 81.5%, ΔE... · =0.32, fragrance lasts for 30.9 hours, total microbial count <10 CFU / g, no clumping, no moisture absorption, and skin irritation score of 0.

[0057] Example 3

[0058] 1. Formula composition: Same as in Example 1, except that the rose raw material is replaced with calendula, and the polyurea microcapsule rose fragrance is replaced with polyurea microcapsule calendula fragrance;

[0059] 2. Preparation steps: Same as in Example 1, with adjustments: flower pretreatment -32℃ liquid nitrogen quick-freezing, 88℃ water extraction, freeze-drying for 11 hours to obtain calendula plant extract powder (moisture content 4.8%) and calendula fragments (20 mesh, moisture content 2.8%); during spraying, the material temperature was 37℃, the inlet / outlet air temperature was 37℃, the atomization pressure was 0.19MPa, and the drying time was 19 minutes;

[0060] 3. Product Performance: Golden yellow granules, disintegration time 2.9 seconds, total polyphenol retention rate 91.5%, initial fragrance duration 38.2 hours, ΔE=0.95; after 6 months of accelerated treatment at 40℃ and 75% RH, the total polyphenol retention rate is 82.7%, ΔE... · =0.38, fragrance lasts for 32.3 hours, total microbial count <10 CFU / g, no clumping, no moisture absorption, and skin irritation score of 0.

[0061] The particles obtained in the above embodiments can be used as additives in various product types, including facial cleansers, bath products, or shampoos.

[0062] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all such modifications or substitutions should be covered within the scope of the claims of the present invention.

Claims

1. A floral microcapsule cleaning granule powder, characterized by, by weight, The product comprises 30-40% carrier and molding agent, 30-45% surfactant, 5-15% conditioning and repairing agent, 5-12% disintegrant and prosolventizing agent, 3-8% core active ingredient, and 1.5-3.0% fragrance microcapsule. The carrier and molding agent includes corn starch, hydrophobic fumed silica, and vitamin E. The surfactants include sodium cocoyl ethanesulfonate, sodium methyl cocoyl taurate, cocoyl propyl betaine, and APG1214. The conditioning and repairing agents include cationic conditioning agents, moisturizers, and skin conditioning agents. The disintegrant and prosolventizing agents include crospovidone, microcrystalline cellulose, and sodium bicarbonate-citric acid gas-generating pair. The core active ingredient includes radiation-resistant complex enzyme powder and floral components. The fragrance microcapsule includes β-cyclodextrin, γ-cyclodextrin, polyurea microcapsule fragrance, and polyquaternium-39.

2. The flower microcapsule cleaning granule powder as described in claim 1, characterized in that, The floral components include plant extract powder and flower fragments prepared from one of the following: rose, butterfly pea, and marigold.

3. The flower microcapsule cleaning granule powder as described in claim 1, characterized in that, Radiation-resistant compound enzyme powder includes protease and lipase.

4. The flower microcapsule cleaning granule powder as described in claim 1, characterized in that, Cationic conditioners include one or more of behenyltrimethylammonium chloride, polyquaternium-10, and cationic guar gum.

5. The flower microcapsule cleaning granule powder as described in claim 1, characterized in that, Moisturizers include one or more of panthenol, trehalose, and hydrolyzed keratin.

6. The flower microcapsule cleaning granule powder as described in claim 1, characterized in that, Skin conditioning agents include allantoin and / or dipotassium glycyrrhizate.

7. The method for preparing flower microcapsule cleaning granules as described in any one of claims 1-6, characterized in that, Includes the following steps: S1. Mix and emulsify β-cyclodextrin, γ-cyclodextrin, polyquaternium-39 with deionized water at 50-60℃, cool to 35-40℃, add polyurea microcapsule fragrance, stir evenly, and obtain fragrance-protecting microcapsule emulsion. S2. Mix the remaining solid components in claim 1 evenly to obtain the basic premixed powder; S3. Put the basic premixed powder into a fluidized bed granulator and dry it at an inlet air temperature of 75-95℃ and an outlet air temperature of 40-50℃. S4. Adjust the inlet and outlet air temperatures to 30-40℃, maintain the material temperature at 35-45℃, and spray the fragrance microcapsule emulsion obtained in step S1 into the fluidized material through an atomizing nozzle. The atomization pressure is 0.12-0.22MPa. S5. After spraying, maintain the inlet air temperature at 30-40℃ and continue fluidized drying for 15-20 minutes until the material moisture content is ≤5.0%. The discharged material is screened to obtain spherical particles with a particle size of 0.8-1.2mm. S6. Place the particles obtained in step S5 in a cobalt-60 irradiation field and sterilize them by irradiation with a dose of 7-8 kGy at an ambient temperature of 27-29℃, then seal and package them.

8. The preparation method according to claim 7, characterized in that, After sterilization, the granules are sealed in aluminum foil composite bags or light-proof plastic bottles.

9. A cleaning and care product, characterized in that, It contains floral microcapsule cleaning particles as described in any one of claims 1-6.

10. The cleaning and care product as described in claim 9, characterized in that, This includes facial cleansers, bath products, and shampoos.