Double-fermentation biological enzyme solid microcapsule cleaning particles as well as preparation method and application thereof

Abstract

The invention discloses a double-fermentation biological enzyme solid microcapsule cleaning particle, which comprises an inner core layer, an effect developing layer and a protective slow-release layer from inside to outside, the inner core layer comprises 10-20% of double-fermentation biological enzyme powder, 4-8% of an anti-caking auxiliary agent, 8-15% of a disintegration accelerator, and 15-30% of a surfactant; the functional color developing layer comprises 50-80% of fruit and vegetable extract and 20-50% of medicinal and edible plant extract; the protective layer comprises 40-50% of a film-forming agent, 30-40% of a hydrophobic softening and moistening agent and 5-10% of essence; the mass ratios of the inner core layer, the efficacy developing layer and the protective layer are 60-75%, 15-25% and 5-15% respectively. The problem that in the prior art, a cleaning product is poor in portability is solved. The invention further provides a preparation method and application of the particles.

Description

Technical Field

[0001] This invention relates to the field of solid cleaning product technology, and in particular to a dual-fermentation bio-enzyme solid microcapsule cleaning particle, its preparation method, and its application. Background Technology

[0002] Cleaning products are generally in the form of pastes, such as shampoo for cleaning hair, shower gel for cleaning the body, and facial cleanser for cleaning the face. However, existing cleaning products typically contain a large amount of chemical agents, which inevitably cause chemical irritation to the cleaned areas. Although there are existing cleaning products with more natural ingredients that can reduce irritation, they require individual packaging, making them less portable (e.g., needing to carry multiple types of cleaning products when traveling). Summary of the Invention

[0003] In view of the shortcomings of the existing technology, the purpose of this invention is to provide a dual-fermentation bio-enzyme solid microcapsule cleaning granule, which solves the problem of poor portability of existing cleaning products.

[0004] To achieve the above objectives, the present invention adopts the following technical solution:

[0005] A dual-fermentation bio-enzyme solid microcapsule cleaning granule comprises, from the inside out, a core layer, an efficacy color-developing layer, and a protective sustained-release layer. The core layer comprises 10-20% dual-fermentation bio-enzyme powder, 4-8% anti-caking agent, 8-15% disintegration promoter, and 15-30% surfactant. The efficacy color-developing layer comprises 50-80% fruit and vegetable extracts and 20-50% medicinal and edible plant extracts. The protective layer comprises 40-50% film-forming agent, 30-40% hydrophobic emollient, and 5%-10% fragrance. The mass ratios of the core layer, efficacy color-developing layer, and protective layer are 60-75%, 15-25%, and 5-15%, respectively.

[0006] Furthermore, the double-fermented bio-enzyme powder is obtained from fruit and vegetable raw materials and medicinal and edible plant raw materials through fermentation.

[0007] Furthermore, the anti-caking agent comprises citric acid, crospovidone, microcrystalline cellulose and silicon dioxide in a weight ratio of (1-3):(1-3):(2-4):(0.5-1.5).

[0008] Furthermore, the disintegration promoters include mannitol, microcrystalline cellulose, and crospovidone in a weight ratio of 3:(3-6):(2-4).

[0009] A method for preparing the above-mentioned dual-fermentation bio-enzyme solid microcapsule cleaning particles is also provided, which includes the following steps:

[0010] S1, Enzymatic fermentation of double-fermented biological enzyme powder: Fruit and vegetable raw materials and medicinal and edible plant raw materials are pretreated and extracted at low temperature, mixed with compound biological enzymes, and enzymatically fermented at 37±1℃ and pH 5.0-5.5 for 72±2h.

[0011] S2, Microbial fermentation of double-fermented biological enzyme powder: The product of enzyme fermentation is inoculated with probiotics after sterilization and anaerobic fermentation is carried out at 37±1℃ and pH 5.5 for 24±1h.

[0012] S3, the product of microbial fermentation is dried at low temperature and then pulverized to obtain double-fermented biological enzyme powder.

[0013] S4 mixes double-fermented biological enzyme powder, anti-caking agent, disintegration promoter and surfactant in proportion to obtain core powder for later use.

[0014] S5, Mix fruit and vegetable extracts and medicinal and edible plant extracts in a certain proportion to form a coating solution for later use, which contains an O / W type emulsion;

[0015] S6, Mix the film-forming agent, hydrophobic softener and fragrance in a certain proportion to form an outer film-forming liquid for later use;

[0016] S7. Add the double-fermented biological enzyme powder to the fluidized bed granulator, spray with coating liquid, dry for 5±1 min, then spray with outer film-forming liquid, dry for 15±2 min, and collect the material on the sieve after sieving.

[0017] S8, the material on the sieve is dried until the moisture content is ≤2.5%, and then cooled to room temperature to obtain the product.

[0018] Furthermore, the probiotics include Lactobacillus plantarum, yeast, and Bacillus subtilis in a mass ratio of 3:1:1, with a probiotic inoculation amount of 2%-3%.

[0019] Furthermore, the low-temperature vacuum drying conditions in S3 are ≤60℃, vacuum degree -0.08~-0.09MPa, 8-10h, and pulverization to 100-200 mesh.

[0020] Furthermore, the inlet air temperature of the fluidized bed granulator in the S7 is 60-65℃, the fluidizing air velocity is 2.5-3.0 m / s, the material temperature is 38-42℃, the coating liquid spraying flow rate is 4-6 mL / min, and the outer film-forming liquid spraying flow rate is 3-4 mL / min.

[0021] Furthermore, S8 is dried using a fluidized bed at low temperature, with conditions of 55-60℃ for 10-15 minutes.

[0022] It also provides applications for the aforementioned dual-fermentation bio-enzyme solid microcapsule cleaning granules, including shampooing, facial cleansing, and bathing.

[0023] Compared with the prior art, the present invention has the following beneficial effects:

[0024] The product is in solid granule form, which allows for simple packaging and easier portability. It can be applied to multiple cleaning scenarios: shampoo, suitable for different hair types such as oily, dry, and sensitive scalps, and can be formulated into shampoo granules with different effects such as oil control, moisturizing, and hair darkening; facial cleanser, suitable for different skin types such as sensitive, dry, and oily skin, and can be formulated into facial cleanser granules with different effects such as gentle soothing and oil control; bath granules, suitable for different skin conditions such as dry, sensitive, and normal skin, and can be formulated into bath granules with different effects such as moisturizing, soothing, and oil control. All products can be packaged using flexible packaging materials (such as high-barrier aluminum foil bags), further enhancing portability and solving the problem of poor portability in existing cleaning products.

[0025] The raw materials can be selected from those listed in the 2025 "Catalogue of Used Cosmetic Raw Materials". At the same time, the double fermentation process can enhance the efficacy and reduce irritation.

[0026] Disintegration accelerators can control disintegration time to ≤10s, with a coefficient of variation of ≤5%, and show no significant changes or residues after storage. Detailed Implementation

[0027] The present invention will be further described in detail below through specific embodiments:

[0028] This solution provides a dual-fermentation bio-enzyme solid microcapsule cleaning granule, which, by weight, is prepared by the following steps:

[0029] S1, Enzymatic fermentation of double-fermented bio-enzyme powder: Fruit and vegetable raw materials (including cucumber, pear, oat, etc.) and medicinal and edible plant raw materials (including mint, lily, yam, etc.) are pretreated and then extracted at low temperature (≤50℃, 2-3h). They are then mixed with compound bio-enzymes (amylase:cellulase:pectinase:xylanase = 2:1:1:1, addition amount 0.5-1.5%) and enzymatically fermented at 37±1℃ and pH 5.0-5.5 for 72±2h to degrade macromolecular substances and release natural color, aroma and flavor components;

[0030] S2, Microbial fermentation of double-fermented biological enzyme powder: After the product of enzyme fermentation is sterilized at 121℃ for 30 min, it is cooled to below 40℃ and inoculated with probiotics (Lactobacillus plantarum: yeast: Bacillus subtilis = 3:1:1, inoculation amount 2%-3%), and anaerobic fermentation is carried out at 37±1℃ and pH 5.5 for 24±1 h to selectively enrich active ingredients;

[0031] S3. The product of microbial fermentation is dried under low temperature and vacuum (≤60℃, vacuum degree -0.08~-0.09MPa, 8-10h) and then pulverized to 100-200 mesh to obtain double-fermented bio-enzyme powder. The biotin content of the obtained double-fermented bio-enzyme powder is 0.45-0.55 mg / g, the water content is 2.0%-2.5%, and the water solubility is ≥99%.

[0032] S4 mixes 10-20% double-fermented bio-enzyme powder, 4-8% anti-caking agent, 8-15% disintegration promoter, and 15-30% surfactant in a mixer (18±2 r / min, 30±5 min, ≤30℃) to obtain core powder for later use. The anti-caking agent is a compound of citric acid, crospovidone, microcrystalline cellulose, and silica in a weight ratio of (1-3):(1-3):(2-4):(0.5-1.5) (all are ingredients listed in the 2025 catalog, with citric acid catalog number 01024, crospovidone catalog number 02115, microcrystalline cellulose catalog number 02116, and silica catalog number 04001), which differs from the single anti-caking agent in the existing technology. Achieving dual anti-caking through chemical and physical methods: Citric acid chelates metal ions and adjusts pH; cross-linked povidone provides a porous framework, balancing anti-caking and disintegration; microcrystalline cellulose enhances particle rigidity and synergistically promotes disintegration; silica provides physical isolation and reduces friction, preventing particle adhesion; the disintegrant is a compound of mannitol, microcrystalline cellulose, and cross-linked povidone in a weight ratio of 3:3-6:2-4 (all ingredients listed in the 2025 catalog), which differs from single disintegrants in existing technologies and has a synergistic mechanism: mannitol enhances hydrophilicity and accelerates water penetration; microcrystalline cellulose provides water channels and enhances dispersibility; cross-linked povidone swells rapidly upon contact with water (swelling rate ≥300%), generating capillary action to promote rapid particle disintegration, ensuring a disintegration time ≤10 seconds and stable performance after storage;

[0033] S5, Mix fruit and vegetable extracts and medicinal and edible plant extracts in a certain proportion to form a coating solution for later use. The solution contains an O / W type emulsion with a solid content of 35-40% and a D90≤5μm.

[0034] S6, Mix the film-forming agent, hydrophobic softener and fragrance in a certain proportion to form an outer film-forming liquid for later use, with a solid content of 40%-45%;

[0035] S7. Add the double-fermented biological enzyme powder into the fluidized bed granulator. The inlet air temperature is 60-65℃, the fluidizing air velocity is 2.5-3.0 m / s, and the material temperature is 38-42℃. First, spray the coating liquid (4-6 mL / min), dry for 5±1 min, then spray the outer film-forming liquid (3-4 mL / min), dry for 15±2 min, and collect the material on the sieve after sieving (20-50 mesh sieve).

[0036] S8, sieve-based fluidized bed low-temperature drying (55-60℃, 10-15 minutes) until moisture content ≤2.5%, cooled to room temperature to obtain product. The product can also be sterilized by cobalt-60 irradiation (12-18kGy, ≤30℃), with a total bacterial count ≤50 CFU / g, and sealed in high-barrier aluminum foil bags.

[0037] The resulting product (double-fermented bio-enzyme solid microcapsule cleansing granules) has a three-layer core-shell spherical structure, consisting of an inner core layer, an efficacy color-developing layer, and a protective sustained-release layer from the inside out. The granules have a moisture content of ≤2.5%, a particle size distribution of 20-50 mesh (1-3 mm), and a disintegration time of ≤10 seconds in cold water at 25℃. Specifically:

[0038] Core layer (60-75% by weight): The core components are biotin enzyme powder derived from fruits, vegetables and medicinal plants (10-20%, prepared by double fermentation), quaternary synergistic anti-caking agent (4-8%), disintegration promoting system (8-15%, mannitol 3-5%, microcrystalline cellulose 3-6%, cross-linked polyvinylpyrrolidone (PVPP) 2-4%), and basic surfactant system (15-30%). The surfactant system can be adjusted according to the product application, and the three components of the disintegration system work together to ensure rapid disintegration.

[0039] The efficacy color layer (15-25% by weight): composed of 80-90% natural fruit and vegetable extracts and medicinal and edible plant extracts listed in the 2025 Cosmetics Catalogue, along with their homologous natural pigments and fragrance substances, achieving a four-in-one integration of "color, fragrance, efficacy, and raw materials." The specific correspondences are as follows (all ingredients are listed in the 2025 catalogue):

[0040] Red: Strawberry extract (60%-70%, fruits and vegetables) + Goji berry extract (30-40%, medicinal and edible), Fragrance: Strawberry fruit aroma + Goji berry fragrance, Efficacy: Brightening and soothing, gentle nourishment, The final product disintegration time is 7.3 seconds;

[0041] Pink: Peach extract (50-60%, fruit and vegetable) + Jujube extract (40-50%, medicinal and edible), Fragrance: Peach and jujube scent, Efficacy: Moisturizing and skin-softening, soothing and repairing, The final product disintegration time is 6.9 seconds;

[0042] Purple: Grape extract (65-75%, fruits and vegetables) + mulberry extract (25-35%, medicinal and edible), Fragrance: Grape fruit aroma + mulberry aroma, Efficacy: Antioxidant, soothing and stabilizing, The final product disintegration time is 9.1s;

[0043] Yellow: Citrus extract (70-80%, fruits and vegetables) + ginger extract (20-30%, medicinal and edible), Fragrance: Citrus + ginger, Efficacy: Oil control and refreshing, gentle and warming, the final product disintegrates in 7.5 seconds;

[0044] Coffee color: coffee extract (60-70%, fruits and vegetables) + poria extract (30-40%, medicinal and edible), fragrance: coffee scent + poria scent, efficacy: oil control, exfoliation, soothing and nourishing, the final product disintegration time is 8.1s;

[0045] Black: Black rice extract (55-65%, fruits and vegetables) + black sesame extract (35-45%, medicinal and edible), Fragrance: Rice aroma + sesame aroma, Efficacy: Gentle cleansing, moisturizing and hair darkening, The final product disintegration time is 5.9s;

[0046] White: Lily extract (50-60%, medicinal and edible) + pear extract (40-50%, fruit and vegetable); Fragrance: Lily scent + pear scent; Efficacy: Soothes sensitivity, moisturizes and calms; The final product disintegrates in 6.5 seconds.

[0047] Beige: Oat extract (60-70%, fruits and vegetables) + yam extract (30-40%, medicinal and edible), fragrance: wheat and yam aroma, effects: gentle moisturizing, soothing and repairing, the final product disintegration time is 7.8 seconds;

[0048] Green: Cucumber extract (70-80%, fruits and vegetables) + peppermint extract (20-30%, medicinal and edible), Fragrance: Cucumber scent + peppermint scent, Efficacy: Oil control and hydration, soothing and relieving itching, The final product disintegration time is 9.4s;

[0049] Blue: Butterfly pea extract (60-70%, fruits and vegetables) + chrysanthemum extract (30-40%, medicinal and edible), fragrance: bean fragrance + chrysanthemum fragrance, efficacy: soothing and moisturizing, antioxidant, the final product disintegration time is 10.1s.

[0050] Protective layer (5-15% by weight): Composed of film-forming agent (40-50%), hydrophobic softener (30-40%) and raw material homologous fragrance encapsulated by β-cyclodextrin (5-10%), which blocks moisture and oxygen, protects the double fermentation components and natural color and fragrance, achieves slow release of fragrance, and does not affect disintegration performance.

[0051] In the three-layer core-shell structure of this invention, the efficacy color layer combines extracts of fruits, vegetables, and medicinal and edible plants listed in the 2025 Cosmetics Catalogue with homologous natural pigments and fragrance substances to achieve a four-in-one integration of "color-fragrance-efficacy-raw materials". The outer layer adopts a combination of "film-forming agent + hydrophobic emollient + β-cyclodextrin encapsulating fragrance", which can not only achieve water and oxygen barrier, but also achieve fragrance slow release without affecting disintegration performance. The thickness of the three-layer structure is precisely matched to ensure that the outer layer protection and core disintegration are synergistically compatible.

[0052] In this invention:

[0053] Double fermentation increases the bioavailability of active ingredients by more than 80% compared to non-fermentation technology (detection method: high performance liquid chromatography (HPLC) as per the "Guideline for Testing Active Ingredients in Cosmetics" (QB / T 4964-2016), using an Agilent 1260 HPLC instrument, with unfermented plant materials from the same batch as a blank control, calculating the in vitro transdermal absorption efficiency of active ingredients (biotin, polyphenols, etc.)). Efficacy indicators are improved by more than 50% compared to existing single fermentation technology; the irritation score is 0 (detection method: patch test using 30 healthy subjects according to the "Guideline for Skin Irritation Testing of Cosmetics" (GB / T 16886.10), with a scoring standard of 0-4 points). Suitable for sensitive skin, with color, fragrance, and efficacy derived from the same source, it eliminates synthetic additives, ensuring natural safety.

[0054] The quadruple anti-caking stabilization system, after accelerated stability testing (40℃ / RH75%), showed no sticking or discoloration for 3 months, with an aroma retention rate of ≥90%, a dual fermentation component retention rate of ≥85%, and a shelf life of ≥24 months, which is more than 100% longer than existing technologies, thus addressing the shortcomings of poor stability in existing technologies.

[0055] The synergistic disintegration system stabilizes the disintegration time at ≤10 seconds, with a coefficient of variation of ≤5%, and shows no significant changes or residues after storage (testing method: according to the "Test Method for Disintegration Time of Cosmetic Solid Products", using 25℃ distilled water, stirring rate of 50r / min, and recording the time for complete particle disintegration (no visible residue)). This meets the core requirements for commercialization and addresses the disintegration shortcomings of existing products.

[0056] The particle sphericity is ≥0.85, the angle of repose is <35°, the filling loss rate is ≤1%, and it is suitable for various packaging. The one-step coating process improves efficiency by more than 40%, shortens the new product development cycle by more than 50%, and can flexibly produce multiple categories of products, which is superior to the production efficiency of existing multi-step coating processes.

[0057] All raw materials comply with the 2025 "Catalogue of Used Cosmetic Raw Materials", and the key raw materials are clearly included in the catalogue (citric acid 01024, crospovidone 02115, etc.), which can be quickly registered; the solid form reduces carbon emissions and plastic usage by 70%, reduces the overall cost by 30%, the raw materials are renewable, which is in line with industry trends and solves the problems of insufficient compliance and poor environmental performance of existing raw materials.

[0058] 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 dual-fermentation bio-enzyme solid microcapsule cleaning granule, characterized by, by weight, It includes a core layer, an efficacy color-developing layer, and a protective sustained-release layer, which are arranged from the inside out. The core layer includes 10-20% double-fermented bio-enzyme powder, 4-8% anti-caking agent, 8-15% disintegration promoter, and 15-30% surfactant. The efficacy color layer includes 50-80% fruit and vegetable extracts and 20-50% medicinal and edible plant extracts. The protective layer consists of 40-50% film-forming agent, 30-40% hydrophobic softener and 5%-10% fragrance; The mass ratios of the core layer, the functional color development layer, and the protective layer are 60-75%, 15-25%, and 5-15%, respectively.

2. The dual-fermentation bio-enzyme solid microcapsule cleaning granules as described in claim 1, characterized in that, Double-fermented bio-enzyme powder is obtained from fruit and vegetable raw materials and medicinal and edible plant raw materials through fermentation.

3. The dual-fermentation bio-enzyme solid microcapsule cleaning granules as described in claim 1, characterized in that, The anti-caking agent comprises citric acid, crospovidone, microcrystalline cellulose and silicon dioxide in a weight ratio of (1-3):(1-3):(2-4):(0.5-1.5).

4. The dual-fermentation bio-enzyme solid microcapsule cleaning granules as described in claim 1, characterized in that, The disintegration promoters include mannitol, microcrystalline cellulose, and crospovidone in a weight ratio of 3:(3-6):(2-4).

5. A method for preparing dual-fermentation bio-enzyme solid microcapsule cleaning particles as described in any one of claims 1-4, characterized in that, Includes the following steps: S1, Enzymatic fermentation of double-fermented biological enzyme powder: Fruit and vegetable raw materials and medicinal and edible plant raw materials are pretreated and extracted at low temperature, mixed with compound biological enzymes, and enzymatically fermented at 37±1℃ and pH 5.0-5.5 for 72±2h. S2, Microbial fermentation of double-fermented biological enzyme powder: The product of enzyme fermentation is inoculated with probiotics after sterilization and anaerobic fermentation is carried out at 37±1℃ and pH 5.5 for 24±1h. S3, the product of microbial fermentation is dried at low temperature and then pulverized to obtain double-fermented biological enzyme powder. S4. Mix the double-fermented biological enzyme powder, anti-caking agent, disintegration promoter and surfactant in proportion to obtain the core powder for later use. S5, Mix fruit and vegetable extracts and medicinal and edible plant extracts in a certain proportion to form a coating solution for later use, which contains an O / W type emulsion; S6, Mix the film-forming agent, hydrophobic softener and fragrance in a certain proportion to form an outer film-forming liquid for later use; S7. Add the double-fermented biological enzyme powder to the fluidized bed granulator, spray with coating liquid, dry for 5±1 min, then spray with outer film-forming liquid, dry for 15±2 min, and collect the material on the sieve after sieving. S8, the material on the sieve is dried until the moisture content is ≤2.5%, and then cooled to room temperature to obtain the product.

6. The preparation method according to claim 5, characterized in that, The probiotics consist of Lactobacillus plantarum, yeast, and Bacillus subtilis in a mass ratio of 3:1:1, with an inoculation amount of 2%-3%.

7. The preparation method according to claim 6, characterized in that, The low-temperature vacuum drying conditions for S3 are ≤60℃, vacuum degree -0.08~-0.09MPa, 8-10h, and pulverization to 100-200 mesh.

8. The preparation method according to claim 7, characterized in that, The inlet air temperature of the S7 fluidized bed granulator is 60-65℃, the fluidizing air velocity is 2.5-3.0 m / s, the material temperature is 38-42℃, the coating liquid spraying flow rate is 4-6 mL / min, and the outer film-forming liquid spraying flow rate is 3-4 mL / min.

9. The preparation method according to claim 1, characterized in that, S8 is dried using a fluidized bed at low temperature, with conditions of 55-60℃ for 10-15 minutes.

10. The application of a dual-fermentation bio-enzyme solid microcapsule cleaning granule as described in any one of claims 1-4, characterized in that, This includes shampoo, facial cleanser, and body wash.