A low-irritation, high-staining plant-based laundry detergent composition and its preparation method
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-06-22
- Publication Date
- 2026-08-14
AI Technical Summary
[0004]为解决上述背景技术中提到的不足,本发明的目的在于提供一种低刺激高去污植物基洗衣液组合物及其制备方法,该组合物通过构建双层植物多糖触发微囊化复合酶体系、含改性菊粉的外层隔离表活并触发释放层、特定植物基表面活性剂体系以及高浓缩宽温域稳定体系,解决了现有植物基洗衣液中表活与酶相互拮抗、低温去污能力不足及浓缩体系储存稳定性差的问题
本发明通过将双层植物多糖触发微囊化复合酶体系、改性菊粉外层壁材、特定植物基表面活性剂体系以及高浓缩宽温域稳定体系进行协同设计,能够显著提升植物基洗衣液的综合性能。由于复合生物酶并非直接暴露于表面活性剂环境中,而是先由内层稳酶玻璃化保护层进行包埋,再由含改性菊粉的外层隔离表活并触发释放层进行二次保护,因此可有效减轻表活对酶蛋白构象的破坏,降低酶在储存过程中的失活风险。改性菊粉引入后,外层壁材具有更强的水化能力和更低的非特异吸附倾向,既有利于阻滞表活向内层渗透,又有利于在洗涤稀释和机械作用下快速吸水溶胀并释放酶活,从而实现储存期保护与使用期高效释放的统一。与此同时,植物源脂肪醇聚氧乙烯醚羧酸盐、烷基糖苷、氨基酸型表面活性剂和两性表面活性剂形成的植物基表活体系,可在保证较低刺激性的前提下提供良好的润湿、分散和乳化能力,并与复合酶在低温条件下形成协同去污作用,对蛋白渍、油渍和汗渍表现出较优清洗效果。
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Figure CN122563668A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of daily chemical products and detergents, specifically relating to a low-irritation, high-stain-removing plant-based laundry detergent composition and its preparation method. Background Technology
[0002] With the development of energy-saving and environmentally friendly washing methods, low-temperature washing and concentration have become important development directions for liquid laundry detergents. Compared with traditional washing, low-temperature washing can reduce energy consumption and fabric damage. However, under low-temperature conditions, the swelling, emulsification, and dispersion efficiency of stains, especially protein stains, grease stains, and sweat stains, decreases significantly, resulting in insufficient detergency of ordinary laundry detergents. To improve the performance of low-temperature washing, existing technologies often add biological enzyme preparations such as proteases, lipases, and amylases to laundry detergents to enhance the decomposition of different types of stains. However, liquid laundry detergent systems usually contain a high proportion of surfactants, especially anionic surfactants. When these surfactants coexist with enzymes for a long time, they can easily have an adverse effect on the conformation of enzyme proteins, leading to decreased enzyme activity and poor storage stability, thus limiting the application effect of enzymes in concentrated liquid laundry detergents.
[0003] On the other hand, plant-based laundry detergents are receiving increasing attention due to their renewable sources, relatively low irritation, and environmental friendliness. However, existing plant-based surfactant systems still face the challenge of balancing detergency and gentleness. While some plant-based surfactants exhibit good skin compatibility, their detergency at low temperatures is insufficient; and introducing stronger surfactants to enhance detergency can easily increase system irritation and further exacerbate enzyme inactivation. Furthermore, highly concentrated plant-based laundry detergents are prone to problems such as stratification, crystallization, low-temperature solidification, viscosity fluctuations, and enzyme activity degradation during actual storage and transportation, exhibiting particularly poor stability over a wide temperature range. Summary of the Invention
[0004] To address the shortcomings mentioned in the background art, the present invention aims to provide a low-irritation, high-detergency plant-based laundry detergent composition and its preparation method. This composition, through the construction of a bilayer plant polysaccharide-triggered microencapsulated complex enzyme system, an outer layer containing modified inulin that isolates and triggers the release of surfactants, a specific plant-based surfactant system, and a highly concentrated, wide-temperature-range stable system, solves the problems of surfactant-enzyme antagonism, insufficient low-temperature detergency, and poor storage stability of concentrated systems in existing plant-based laundry detergents. The composition of the present invention combines low irritation, high detergency, low-temperature suitability, and good storage stability, making it suitable for low-temperature concentrated laundry detergent products.
[0005] The objective of this invention can be achieved through the following technical solutions: A low-irritation, high-cleaning plant-based laundry detergent composition comprises the following raw materials in parts by weight: 22-42 parts of a plant-based surfactant system, 0.3-6.0 parts of a bilayer plant polysaccharide-triggered microencapsulation complex enzyme system, 3-15 parts of a natural solubilizer, 2-12 parts of plant sugar alcohols, 0.2-6 parts of an enzyme synergistic stabilizer, 0.1-2.0 parts of a pH adjuster, and the balance being deionized water; The plant-based surfactant system includes plant-derived fatty alcohol polyoxyethylene ether carboxylates, alkyl glycosides, amino acid surfactants, and amphoteric surfactants, wherein the mass ratio of the plant-derived fatty alcohol polyoxyethylene ether carboxylates, alkyl glycosides, amino acid surfactants, and amphoteric surfactants is 8-14:6-12:4-8:4-8. The bilayer plant polysaccharide-triggered microencapsulated complex enzyme system includes an inner enzyme-stabilizing vitrified protective layer, an outer isolating surfactant and triggering release layer, and a complex biological enzyme embedded in the inner layer. The outer isolating surfactant and triggering release layer contains modified inulin.
[0006] More preferably, the modified inulin is mildly sulfo-beet alkalized inulin, and the degree of substitution of the mildly sulfo-beet alkalized inulin is 0.05 to 0.30.
[0007] More preferably, the complex bio-enzyme includes two or three of protease, lipase, and amylase; the inner enzyme-stabilizing vitrified protective layer is selected from one or more of inulin, trehalose, maltodextrin, and gum arabic; the outer surfactant-isolating and release-triggering layer includes one or more of guar gum, gum arabic, and low-ester pectin, in addition to modified inulin.
[0008] More preferably, the plant-derived fatty alcohol polyoxyethylene ether carboxylate is a carboxylate-type surfactant obtained by adding plant-derived C10-C14 fatty alcohols to ethylene oxide and then carboxylating them, with an average addition number of ethylene oxide of 2-5; the alkyl glycoside is selected from one or more of decyl glucoside, octyl glucoside, and lauryl glucoside; the amino acid-type surfactant is selected from one or two of sodium cocoyl glutamate and sodium lauroyl sarcosinate; and the amphoteric surfactant is cocamidopropyl betaine.
[0009] More preferably, the natural solubilizer is selected from one or more of plant-derived glycerol, cocoyl diethanolamide, and plant-derived 1,3-propanediol; the plant sugar alcohol is selected from one or more of sorbitol, xylitol, and erythritol; and the enzyme synergistic stabilizer is selected from one or more of calcium chloride, calcium lactate, sodium citrate, trehalose, and glycerol.
[0010] More preferably, the low-irritation, high-cleaning plant-based laundry detergent composition is a low-temperature concentrated laundry detergent suitable for washing conditions of 10–25°C, wherein the total active ingredient content of the composition is 35%–50%, the system HLB value is 12–14, and the pH value is 6.8–8.5.
[0011] A method for preparing a low-irritation, high-stain-removing plant-based laundry detergent composition includes the following steps: S1. Modify inulin to obtain modified inulin, and carboxymethylate plant-derived fatty alcohol polyoxyethylene ether to obtain plant-derived fatty alcohol polyoxyethylene ether carboxylate. S2. A bilayer plant polysaccharide-triggered microencapsulated complex enzyme system was prepared by combining a complex biological enzyme, an inner layer of enzyme-stabilizing vitrified protective layer components, and an outer layer of isolating surfactant and triggering release layer components. S3. Mix the plant-based surfactant system, natural solubilizer, plant sugar alcohol, enzyme synergist stabilizer, pH adjuster and deionized water to prepare the base solution; S4. Add the bilayer plant polysaccharide-triggered microencapsulation complex enzyme system to the base solution to obtain the low-irritation, high-cleaning plant-based laundry detergent composition.
[0012] More preferably, in step S1, the modified inulin is prepared by the following method: inulin is etherified with a tertiary amine reagent containing an epoxy group to obtain an inulin intermediate with a tertiary amine side chain, and then the inulin intermediate is reacted with a beet alkalizing agent to obtain modified inulin; the plant-derived fatty alcohol polyoxyethylene ether carboxylate is prepared by the following method: the plant-derived fatty alcohol polyoxyethylene ether is reacted with a carboxymethylating agent and neutralized to obtain the plant-derived fatty alcohol polyoxyethylene ether carboxylate.
[0013] Further preferably, step S2 includes: mixing the composite bio-enzyme with the inner layer enzyme-stabilizing vitrification protective layer component to form an inner layer core liquid, and granulating the inner layer core liquid to obtain inner layer particles; contacting the inner layer particles with the outer layer isolating surfactant and triggering release layer component, so that the outer layer isolating surfactant and triggering release layer component is formed on the outer surface of the inner layer particles; and then drying to obtain a bilayer plant polysaccharide-triggered microencapsulated composite enzyme system.
[0014] More preferably, in step S4, after the temperature of the base liquid drops below 30°C, the double-layer plant polysaccharide-triggered microencapsulation complex enzyme system is added to the base liquid and mixed using a low-shear dispersion method to obtain the low-irritation, high-cleaning plant-based laundry detergent composition.
[0015] The beneficial effects of this invention are: This invention significantly improves the overall performance of plant-based laundry detergents by synergistically designing a bilayer plant polysaccharide-triggered microencapsulated complex enzyme system, a modified inulin outer wall material, a specific plant-based surfactant system, and a highly concentrated, wide-temperature-range stabilizing system. Because the complex enzyme is not directly exposed to the surfactant environment, but is first embedded in an inner enzyme-stabilizing vitrified protective layer, and then further protected by an outer layer containing modified inulin that isolates the surfactant and triggers release, the damage to the enzyme protein conformation caused by the surfactant is effectively reduced, lowering the risk of enzyme inactivation during storage. After the introduction of modified inulin, the outer wall material exhibits stronger hydration capacity and lower non-specific adsorption tendency, which not only helps to prevent surfactant penetration into the inner layer but also facilitates rapid water absorption, swelling, and enzyme release under washing dilution and mechanical action, thus achieving a balance between protection during storage and efficient release during use. Meanwhile, the plant-based surfactant system, composed of plant-derived fatty alcohol polyoxyethylene ether carboxylates, alkyl glycosides, amino acid surfactants, and amphoteric surfactants, can provide good wetting, dispersing, and emulsifying capabilities while ensuring low irritation. It also forms a synergistic detergency with the complex enzymes under low-temperature conditions, showing superior cleaning effects on protein stains, oil stains, and sweat stains. Attached Figure Description
[0016] The invention will now be further described with reference to the accompanying drawings.
[0017] Figure 1 This is a comparison chart of the low-temperature detergency performance of the laundry detergent compositions of Examples 1-3 and Comparative Examples 1-2; Figure 2 The graph shows the mildness test results of the laundry detergent compositions of Examples 1-3 and Comparative Examples 1-2. Detailed Implementation
[0018] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0019] Example 1: Verify the feasibility of preparing the composition of the present invention at a low level of component addition, the system compatibility and basic low-temperature washing performance.
[0020] I. Preparation of Modified Inulin Weigh 50.0 g of inulin, add 150 mL of isopropanol and 80 mL of deionized water, and disperse under nitrogen protection by stirring at 200 r / min for 30 min. Dissolve 1.2 g of sodium hydroxide in a small amount of deionized water and add it to the system, then activate at 30 °C for 40 min. Subsequently, slowly add 4.0 g of N,N-dimethylglycidylamine. After the addition is complete, react at 45 °C for 1 h, then raise the temperature to 55 °C and react for 5 h to obtain an inulin intermediate with a tertiary amine side chain. After the reaction is complete, cool to 40 °C, add 5.0 g of sodium 2-bromoethanesulfonate, and raise the temperature to 65 °C and react for 7 h to complete the beet alkalization reaction. After the reaction solution is cooled to room temperature, it is placed in a dialysis bag with a molecular weight cutoff of 3500 Da and dialyzed with deionized water for 36 h, changing the water every 4 h. After the dialysate was concentrated under reduced pressure, three times its volume of anhydrous ethanol was added to precipitate the product. The precipitate was filtered and washed with anhydrous ethanol. The resulting product was then vacuum dried at 45°C for 10 h to obtain mildly sulfo-betaine alkalized inulin, which is the modified inulin. The degree of substitution was determined by nuclear magnetic resonance or elemental analysis, and the degree of substitution (DS) was controlled within the range of 0.10–0.15.
[0021] II. Preparation of plant-derived fatty alcohol polyoxyethylene ether carboxylates Weigh 100.0 g of plant-derived lauryl alcohol polyoxyethylene ether (EO=2), add 80 mL of isopropanol and 40 mL of deionized water, and stir at approximately 200 r / min until homogeneous under nitrogen protection. Then add 9.0 g of sodium hydroxide and continue stirring for 30 min. Subsequently, add 20.0 g of sodium chloroacetate to the reaction system in three batches, with each batch added 20 min apart, and control the system temperature not to exceed 60℃ during the addition process. After the addition is complete, raise the temperature to 70℃ and maintain the reaction for 6 h to carry out the carboxymethylation reaction. After the reaction is complete, cool to 40℃ and adjust the pH to 7.2–7.8 using a 10% citric acid aqueous solution. Then remove isopropanol by vacuum distillation at 65℃ and -0.09 MPa, followed by cooling to 25℃ and filtering to remove the precipitated inorganic salts. Finally, add an appropriate amount of deionized water to adjust the active ingredient content to 70% ± 1% to obtain plant-derived fatty alcohol polyoxyethylene ether carboxylate.
[0022] III. Preparation of a bilayer plant polysaccharide-triggered microencapsulated complex enzyme system Weigh 2.0 g of protease, 1.0 g of lipase, 1.2 g of inulin, 0.8 g of trehalose, and 0.6 g of maltodextrin, add them to 20 mL of deionized water, and stir at 150 r / min for 20 min at 10 °C to form a homogeneous inner core liquid. Then, atomize the inner core liquid into particles and drop them into an anhydrous ethanol freeze bath for low-temperature solidification to obtain inner layer particles. Separately weigh 1.5 g of modified inulin and 0.5 g of guar gum, add them to 20 mL of deionized water, and stir at 25 °C until fully dissolved to form an outer wall material liquid. Add the obtained inner layer particles to the outer wall material liquid and roll them at 30 r / min for 30 min to coat them, allowing the outer layer to isolate the surfactant and trigger the release layer components to form on the outer surface of the inner layer particles. After coating, the resulting particles were placed in a freeze-drying apparatus for drying. The cold trap temperature was controlled at -50℃, the vacuum degree was not higher than 20 Pa, and the drying time was 24 h to obtain a bilayer plant polysaccharide-triggered microencapsulation complex enzyme system.
[0023] IV. Preparation of Low-Irritation, High-Stain-Removing Plant-Based Laundry Detergent Composition The low-irritation, high-cleaning plant-based laundry detergent composition comprises the following ingredients in parts by weight: 22 parts of plant-based surfactant system, 0.3 parts of bilayer plant polysaccharide-triggered microencapsulation complex enzyme system, 3 parts of natural solubilizer, 2 parts of plant sugar alcohol, 0.2 parts of enzyme synergistic stabilizer, 0.1 parts of pH adjuster, and the balance being deionized water; The preparation steps of the low-irritation, high-detergency plant-based laundry detergent composition are as follows: 680.0 g of deionized water is weighed and added to a mixing vessel, stirred at 280 r / min at 25°C, followed by the addition of 30.0 g of plant-derived glycerin, 20.0 g of sorbitol, and 2.0 g of calcium chloride. Stirring is continued for 20 min to ensure complete dissolution of all components, yielding an additive premix. While maintaining stirring, 40.0 g of sodium cocoyl glutamate, 40.0 g of cocamidopropyl betaine, 60.0 g of decyl glucoside, and 80.0 g of plant-derived fatty alcohol polyoxyethylene ether carboxylate are added sequentially to the additive premix. After each addition, the mixture is stirred for 8 min to ensure complete dispersion, forming a homogeneous surfactant base solution. Subsequently, 1.0 g of citric acid, a pH adjuster, is added to adjust the pH of the system to 6.8. The above-mentioned base solution was cooled to below 30°C, and the stirring speed was adjusted to 120 r / min. Under low shear conditions, 3.0 g of the bilayer plant polysaccharide-triggered microencapsulation complex enzyme system was slowly added, and dispersion was continued for 15 min to reduce microcapsule breakage and enzyme activity loss. Then, deionized water was added to a total mass of 1000.0 g, and stirring was continued at low speed for 10 min. After standing to remove bubbles, the low-irritation, high-cleaning plant-based laundry detergent composition was obtained.
[0024] Example 2: Verifying the feasibility of preparing the composition of the present invention at higher active components and higher concentration levels, as well as its storage stability and overall detergency performance.
[0025] The preparation method of the modified inulin is the same as that in Example 1. By adjusting the reactant ratio and reaction conditions, the degree of substitution (DS) of the modified inulin is controlled within the range of 0.05 to 0.30. The preparation method of the plant-derived fatty alcohol polyoxyethylene ether carboxylate and bilayer plant polysaccharide-triggered microencapsulation complex enzyme system is the same as that in Example 1; The low-irritation, high-cleaning plant-based laundry detergent composition comprises the following raw materials in parts by weight: 42 parts of plant-based surfactant system, 6 parts of double-layer plant polysaccharide-triggered microencapsulation complex enzyme system, 15 parts of natural solubilizer, 12 parts of plant sugar alcohol, 6 parts of enzyme synergistic stabilizer, 2 parts of pH adjuster, and the balance of deionized water. The preparation steps of the low-irritation, high-detergency plant-based laundry detergent composition are as follows: 120.0 g of deionized water is weighed and added to a mixing vessel, and stirred at 300 r / min at 25°C. Subsequently, 100.0 g of plant-derived glycerin, 50.0 g of plant-derived 1,3-propanediol, 60.0 g of sorbitol, 60.0 g of erythritol, 10.0 g of calcium lactate, 20.0 g of sodium citrate, and 30.0 g of trehalose are added, and stirring is continued for 25 min to fully dissolve all components, obtaining an additive premix. Under the condition of maintaining stirring, 80.0 g of sodium lauroyl sarcosinate, 80.0 g of cocamidopropyl betaine, 120.0 g of lauryl glucoside, and 140.0 g of plant-derived fatty alcohol polyoxyethylene ether carboxylate are added sequentially to the additive premix. After each addition of raw material, stirring is carried out for 8 min to ensure full dispersion, forming a homogeneous surfactant base solution. Subsequently, 20.0 g of pH adjuster was added, and the pH of the system was adjusted to 8.5 using triethanolamine and citric acid. The above base solution was cooled to below 30°C, and the stirring speed was adjusted to 120 r / min. Under low shear conditions, 60.0 g of the bilayer plant polysaccharide-triggered microencapsulation complex enzyme system was slowly added, and dispersion was continued for 20 min to reduce microcapsule breakage and enzyme activity loss. Then, deionized water was added to a total mass of 1000.0 g, and stirring was continued at low speed for 10 min. After standing to remove bubbles, the low-irritation, high-cleaning plant-based laundry detergent composition was obtained.
[0026] Example 3: Verifying the feasibility of preparing the composition of the present invention under balanced formulation conditions, its storage stability and overall detergency performance.
[0027] The preparation method of the modified inulin is the same as that in Example 1. By adjusting the reactant ratio and reaction conditions, the degree of substitution (DS) of the modified inulin is controlled within the range of 0.05 to 0.30. The preparation method of the plant-derived fatty alcohol polyoxyethylene ether carboxylate and bilayer plant polysaccharide-triggered microencapsulation complex enzyme system is the same as that in Example 1; The low-irritation, high-cleaning plant-based laundry detergent composition comprises the following ingredients in parts by weight: 32 parts of plant-based surfactant system, 3.15 parts of bilayer plant polysaccharide-triggered microencapsulation complex enzyme system, 9 parts of natural solubilizer, 7 parts of plant sugar alcohol, 3.1 parts of enzyme synergistic stabilizer, 1.05 parts of pH adjuster, and the balance being deionized water. The preparation steps of the low-irritation, high-cleaning plant-based laundry detergent composition are as follows: Weigh 447.0 g of deionized water and add it to the mixing tank. Stir at 280 r / min at 25℃. Then add 60.0 g of plant-derived glycerin, 30.0 g of plant-derived 1,3-propanediol, 40.0 g of sorbitol, 30.0 g of xylitol, 10.0 g of calcium lactate, 10.0 g of sodium citrate and 11.0 g of trehalose. Continue stirring for 20 min to fully dissolve all components and obtain the additive premix. While maintaining stirring, 30.0 g of sodium cocoyl glutamate, 30.0 g of sodium lauroyl sarcosinate, 60.0 g of cocamidopropyl betaine, 45.0 g of decyl glucoside, 45.0 g of lauryl glucoside, and 110.0 g of plant-derived fatty alcohol polyoxyethylene ether carboxylate were added sequentially to the premixed adjuvant solution. After each addition, the mixture was stirred for 10 min to ensure thorough dispersion and form a homogeneous surfactant base solution. Subsequently, 10.5 g of pH adjuster was added, and the pH of the system was adjusted to 7 using triethanolamine and citric acid. The base solution was cooled to below 30°C, and the stirring speed was adjusted to 120 r / min. Under low shear conditions, 31.5 g of the bilayer plant polysaccharide-triggered microencapsulation complex enzyme system was slowly added, and dispersion was continued for 15 min to minimize microcapsule breakage and enzyme activity loss. Then add deionized water to a total mass of 1000.0g, continue stirring at low speed for 10 minutes, let stand to remove bubbles, and obtain the low-irritation, high-cleaning plant-based laundry detergent composition.
[0028] Comparative Example 1: Without inulin modification treatment, unmodified natural inulin was used directly as the outer wall material component to verify the effect of modified inulin on the surface-active permeation resistance, low enzyme adsorption and enzyme release performance of the double-layer microcapsules.
[0029] The preparation method of the plant-derived fatty alcohol polyoxyethylene ether carboxylate is the same as that in Example 1. In the preparation of the bilayer plant polysaccharide-triggered microencapsulation complex enzyme system, except that the modified inulin is replaced with unmodified natural inulin, the other preparation steps are the same as those in Example 1. The low-irritation, high-cleaning plant-based laundry detergent composition comprises the following ingredients in parts by weight: 32 parts of plant-based surfactant system, 3.15 parts of bilayer plant polysaccharide-triggered microencapsulation complex enzyme system, 9 parts of natural solubilizer, 7 parts of plant sugar alcohol, 3.1 parts of enzyme synergistic stabilizer, 1.05 parts of pH adjuster, and the balance being deionized water. The preparation steps of the low-irritation, high-cleaning plant-based laundry detergent composition are as follows: Weigh 447.0 g of deionized water and add it to a mixing vessel. Stir at 280 r / min at 25°C until homogeneous. Then, add 60.0 g of plant-derived glycerin, 30.0 g of plant-derived 1,3-propanediol, 40.0 g of sorbitol, 30.0 g of xylitol, 10.0 g of calcium lactate, 10.0 g of sodium citrate, and 11.0 g of trehalose in sequence. Continue stirring for 20 min to ensure that all components are completely dissolved and a homogeneous premix of additives is formed. While maintaining stirring, 30.0 g of sodium cocoyl glutamate, 30.0 g of sodium lauroyl sarcosinate, 60.0 g of cocamidopropyl betaine, 45.0 g of decyl glucoside, 45.0 g of lauryl glucoside, and 110.0 g of plant-derived fatty alcohol polyoxyethylene ether carboxylate were added sequentially to the above-mentioned premixed auxiliary agent solution. Stirring was continued for 10 min after each addition to form a homogeneous surfactant base solution. Then, 10.5 g of pH adjuster was added, and the pH of the system was adjusted to 7 using triethanolamine and citric acid. The base solution was cooled to below 30°C, and the stirring speed was adjusted to 120 r / min. Under low shear conditions, 31.5 g of a bilayer plant polysaccharide-triggered microencapsulation complex enzyme system was slowly added, and dispersion was continued for 15 min. Deionized water was then added to a total mass of 1000.0 g, and stirring was continued at low speed for 10 min. After standing to remove bubbles, the comparative low-irritation, high-detergency plant-based laundry detergent composition was obtained.
[0030] Comparative Example 2: Except for replacing plant-derived fatty alcohol polyoxyethylene ether carboxylate with a common strong anionic surfactant.
[0031] The preparation method of the modified inulin is the same as that in Example 1. By adjusting the reactant ratio and reaction conditions, the degree of substitution (DS) of the modified inulin is controlled within the range of 0.05 to 0.30. The preparation method of the bilayer plant polysaccharide-triggered microencapsulation complex enzyme system is the same as that in Example 1; The low-irritation, high-cleaning plant-based laundry detergent composition comprises the following raw materials in parts by weight: 32 parts of a common surfactant system, 3.15 parts of a bilayer plant polysaccharide-triggered microencapsulation complex enzyme system, 9 parts of a natural solubilizer, 7 parts of plant sugar alcohol, 3.1 parts of an enzyme synergistic stabilizer, 1.05 parts of a pH adjuster, and the balance being deionized water. The preparation steps of the low-irritation, high-detergency plant-based laundry detergent composition are as follows: 447.0 g of deionized water is weighed and added to a mixing vessel, and stirred at 280 r / min at 25℃. Then, 60.0 g of plant-derived glycerin, 30.0 g of plant-derived 1,3-propanediol, 40.0 g of sorbitol, 30.0 g of xylitol, 10.0 g of calcium lactate, 10.0 g of sodium citrate, and 11.0 g of trehalose are added, and stirring is continued for 20 min to fully dissolve all components, obtaining an additive premix. Subsequently, under stirring conditions, 30.0 g of sodium cocoyl glutamate, 30.0 g of sodium lauroyl sarcosinate, 60.0 g of cocamidopropyl betaine, 45.0 g of decyl glucoside, 45.0 g of lauryl glucoside, and 110.0 g of sodium fatty alcohol polyoxyethylene ether sulfate are added sequentially, stirring for 10 min after each addition to ensure full dispersion and form a homogeneous surfactant base solution. Subsequently, 10.5 g of pH adjuster was added, and the pH of the system was adjusted to 7 using triethanolamine and citric acid. The above base solution was cooled to below 30°C, and the stirring speed was adjusted to 120 r / min. Under low shear conditions, 31.5 g of the bilayer plant polysaccharide-triggered microencapsulation complex enzyme system was slowly added, and dispersion was continued for 15 min to reduce microcapsule breakage and enzyme activity loss. Then, deionized water was added to a total mass of 1000.0 g, and stirring was continued at low speed for 10 min. After standing to remove bubbles, the low-irritation, high-cleaning plant-based laundry detergent composition was obtained.
[0032] Performance testing: 1. Low-temperature detergency performance test The tests were conducted according to GB / T 13174-2021 "Determination of Stain-Removing Power and Recycled Washing Performance of Detergents for Clothing". Three pieces each of protein-stained cloth, oil-stained cloth, sweat-stained cloth, and composite-stained cloth were selected and cut to uniform specifications. The initial reflectance was measured and recorded using a reflectometer. The washing solutions for Examples 1-3 and Comparative Examples 1-2 were prepared with a uniform concentration of 2 g / L and a liquid-to-liquid ratio of 1:50. The washing temperature was controlled at 15℃ (low-temperature washing condition), the washing time for each group was 15 min, and the mechanical stirring speed was 120 r / min. After washing, the samples were thoroughly rinsed with deionized water and air-dried. The reflectance of the samples was measured again, and the stain removal rate was calculated according to the national standard formula. Each group of tests was measured in triplicate. After removing outliers, the average value was taken. The results are shown in Table 1 below.
[0033] Table 1 Results of Low-Temperature Decontamination
[0034] As shown in Table 1, Examples 1-3 of the present invention exhibited good removal effects on protein stains, oil stains, sweat stains, and complex stains under low-temperature conditions of 15℃, and the overall stain removal rate was significantly better than that of Comparative Examples 1 and 2. Among them, Example 3 showed the best overall stain removal performance, indicating that under relatively balanced formulation conditions, the plant-based surfactant system, the bilayer plant polysaccharide-triggered microencapsulation complex enzyme system, and the modified inulin outer wall material could form a good synergistic effect, thereby simultaneously improving the removal ability of different types of stains under low-temperature conditions. In Comparative Example 1, after replacing the modified inulin with unmodified natural inulin, the removal rate of various stains decreased, indicating that modified inulin is beneficial to enhancing the anti-surfactant interference ability and enzyme release efficiency of the microencapsulation outer layer. In Comparative Example 2, after replacing the plant-derived fatty alcohol polyoxyethylene ether carboxylate with a common strong anionic surfactant, the low-temperature stain removal effect also decreased, indicating that the plant-based surfactant system selected in the present invention is more conducive to stain removal under low-temperature washing conditions.
[0035] 2. Enzyme activity retention rate test Samples from Examples 1-3 and Comparative Examples 1-2 were sealed and stored in a 45°C constant-temperature accelerated storage chamber. Samples were taken at 0, 30, 60, and 90 days. The activity values of protease, lipase, and amylase in the samples at 0 days were used as the initial enzyme activities. The enzyme activities of the stored samples were measured according to the corresponding enzyme activity assay methods, and the enzyme activity retention rate was calculated. Protease activity was measured using the casein method, lipase activity using the olive oil emulsion method, and amylase activity using the soluble starch method. Each group was measured in triplicate, and the average value was taken. The results are shown in Tables 2 and 3 below.
[0036] Table 2. Retention rates of protease and lipase activities
[0037] Table 3. Amylase activity retention rate
[0038] As shown in Tables 2 and 3, the retention rates of protease, lipase, and amylase activities in Examples 1-3 after accelerated storage at 45℃ for 30, 60, and 90 days were significantly higher than those in Comparative Examples 1 and 2, indicating that the composition of the present invention has a better protective effect on the complex biological enzymes. Among them, Example 3 showed the highest retention rates of all enzyme activities. In Comparative Example 1, after replacing the modified inulin with unmodified natural inulin, the retention rates of all enzyme activities decreased significantly, indicating that modified inulin is beneficial to improving the barrier ability of the outer wall material to surfactants and reducing the non-specific adsorption of enzymes. In Comparative Example 2, after replacing the plant-derived fatty alcohol polyoxyethylene ether carboxylate with a common strong anionic surfactant, the enzyme activity retention rate further decreased, indicating that the plant-based surfactant system used in the present invention is more conducive to maintaining the stability of enzymes under high-temperature storage conditions.
[0039] 3. Enzyme release behavior test Samples from Examples 1-3 and Comparative Examples 1-2 were taken and prepared into test solutions in three states: stock solution, 10-fold dilution, and 50-fold dilution. Mechanical disturbance conditions involved stirring at 120 r / min for 15 min, and low shear conditions involved stirring at 60 r / min for 15 min. After each treatment, the unreleased microcapsule particles were separated by centrifugation. The activities of protease, lipase, and amylase in the supernatant were measured and compared with the total enzyme activity in the sample to calculate the enzyme release rate. Each group was measured in triplicate, and the average value was taken. The enzyme release rates were compared under stock solution conditions, different dilution ratios, and different disturbance conditions. The results are shown in Table 4 below.
[0040] Table 4. Results of enzyme release behavior test (enzyme release rate, %)
[0041] Table 4 shows that the enzyme release rates in Examples 1-3 were low in the undiluted state, but significantly increased under 10-fold dilution, 50-fold dilution, and mechanical disturbance conditions. This indicates that the bilayer plant polysaccharide-triggered microencapsulated complex enzyme system constructed in this invention can effectively inhibit premature enzyme release during storage and achieve rapid enzyme release with dilution and external force during use. In Comparative Example 1, after replacing modified inulin with unmodified natural inulin, the enzyme release rate increased in the undiluted state, while the release rate decreased after dilution. This indicates that the outer layer of modified inulin is more conducive to inhibiting enzyme leakage during storage and enhancing the triggering release effect. In Comparative Example 2, after replacing plant-derived fatty alcohol polyoxyethylene ether carboxylate with a common strong anionic surfactant, the enzyme release rate further increased in the undiluted state, and the release effect was poor under dilution and mechanical disturbance conditions. This indicates that the plant-based surfactant system and the bilayer microencapsulated enzyme system of this invention have better synergistic matching.
[0042] 4. Mildness test Samples from Examples 1-3 and Comparative Examples 1-2 were prepared into 1.0% (w / w) test solutions using deionized water, with a blank control group included. Protein denaturation rate was tested using bovine serum albumin (BSA) method. An equal volume of sample test solution was mixed with 0.5 mg / mL BSA standard solution and incubated in a 37℃ constant temperature water bath for 30 min in the dark. The absorbance was measured at 280 nm using a UV spectrophotometer, and the protein denaturation rate was calculated using the blank group as a baseline. In vitro skin irritation evaluation used a reconstructed human epidermal model method. 50 μL of sample test solution was uniformly applied to the surface of the skin model, incubated for 15 min, and then rinsed. Epidermal cell viability was determined using the MTT assay, and the irritation level was determined according to industry standards. Each experiment was performed in triplicate, and the average value was taken. The test results are shown in Table 5 below.
[0043] Table 5. Mildness Test Results
[0044] As shown in Table 5, the protein denaturation rates of Examples 1-3 were significantly lower than those of Comparative Examples 1 and 2, while the cell survival rates of the reconstructed human epidermal models were high, all exhibiting low irritation, indicating that the compositions of the present invention have good mildness. Among them, Example 3 had the lowest protein denaturation rate and the highest cell survival rate, indicating that under relatively balanced formulation conditions, the plant-based surfactant system, the bilayer plant polysaccharide-triggered microencapsulation complex enzyme system, and the modified inulin outer wall material can form a better synergy, thereby reducing the irritation to the protein and skin model while ensuring detergency performance. In Comparative Example 1, after replacing the modified inulin with unmodified natural inulin, the protein denaturation rate increased and the cell survival rate decreased, indicating that the modified inulin helps improve the interface mildness of the microcapsule outer layer. In Comparative Example 2, after replacing the plant-derived fatty alcohol polyoxyethylene ether carboxylate with a common strong anionic surfactant, the protein denaturation rate further increased and the irritation evaluation worsened, indicating that the plant-based surfactant system used in the present invention is more conducive to achieving low-irritation and mild cleansing effects.
[0045] In the description of this specification, references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.
[0046] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claimed invention.
Claims
1. A low-irritation, high-cleaning-strength plant-based laundry detergent composition, characterized in that, It contains the following raw materials in parts by weight: 22-42 parts of plant-based surfactant system, 0.3-6.0 parts of bilayer plant polysaccharide-triggered microencapsulation complex enzyme system, 3-15 parts of natural solubilizer, 2-12 parts of plant sugar alcohol, 0.2-6 parts of enzyme synergistic stabilizer, 0.1-2.0 parts of pH adjuster, and the balance of deionized water; The plant-based surfactant system includes plant-derived fatty alcohol polyoxyethylene ether carboxylates, alkyl glycosides, amino acid surfactants, and amphoteric surfactants, wherein the mass ratio of the plant-derived fatty alcohol polyoxyethylene ether carboxylates, alkyl glycosides, amino acid surfactants, and amphoteric surfactants is 8-14:6-12:4-8:4-8. The bilayer plant polysaccharide-triggered microencapsulated complex enzyme system includes an inner enzyme-stabilizing vitrified protective layer, an outer isolating surfactant and triggering release layer, and a complex biological enzyme embedded in the inner layer. The outer isolating surfactant and triggering release layer contains modified inulin.
2. The low-irritation, high-cleaning-strength plant-based laundry detergent composition according to claim 1, characterized in that, The modified inulin is a mildly sulfo-saccharified beet alkalized inulin, and the degree of substitution of the mildly sulfo-saccharified beet alkalized inulin is 0.05 to 0.
30.
3. The low-irritation, high-cleaning-strength plant-based laundry detergent composition according to claim 1, characterized in that, The composite bio-enzyme includes two or three of the following: protease, lipase, and amylase; the inner enzyme-stabilizing vitrified protective layer is selected from one or more of the following: inulin, trehalose, maltodextrin, and gum arabic; the outer surfactant-isolating and release-triggered layer includes one or more of the following: guar gum, gum arabic, and low-ester pectin, in addition to modified inulin.
4. The low-irritation, high-cleaning-strength plant-based laundry detergent composition according to claim 1, characterized in that, The plant-derived fatty alcohol polyoxyethylene ether carboxylate is a carboxylate-type surfactant obtained by adding plant-derived C10-C14 fatty alcohols to ethylene oxide and then carboxylating the resulting solution, wherein the average addition number of the ethylene oxide is 2-5; the alkyl glycoside is selected from one or more of decyl glucoside, octyl glucoside, and lauryl glucoside; the amino acid-type surfactant is selected from one or two of sodium cocoyl glutamate and sodium lauroyl sarcosinate; and the amphoteric surfactant is cocamidopropyl betaine.
5. The low-irritation, high-cleaning-strength plant-based laundry detergent composition according to claim 1, characterized in that, The natural solubilizer is selected from one or more of plant-derived glycerol, cocoyl diethanolamide, and plant-derived 1,3-propanediol; the plant sugar alcohol is selected from one or more of sorbitol, xylitol, and erythritol; and the enzyme synergistic stabilizer is selected from one or more of calcium chloride, calcium lactate, sodium citrate, trehalose, and glycerol.
6. The low-irritation, high-cleaning-strength plant-based laundry detergent composition according to claim 1, characterized in that, The composition is a low-temperature concentrated laundry detergent suitable for washing conditions of 10-25°C. The total active ingredient content of the composition is 35%-50%, the HLB value of the system is 12-14, and the pH value is 6.8-8.
5.
7. A method for preparing a low-irritation, high-staining plant-based laundry detergent composition according to any one of claims 1 to 6, characterized in that, Includes the following steps: S1. Modify inulin to obtain modified inulin, and carboxymethylate plant-derived fatty alcohol polyoxyethylene ether to obtain plant-derived fatty alcohol polyoxyethylene ether carboxylate. S2. A bilayer plant polysaccharide-triggered microencapsulated complex enzyme system was prepared by combining a complex biological enzyme, an inner layer of enzyme-stabilizing vitrified protective layer components, and an outer layer of isolating surfactant and triggering release layer components. S3. Mix the plant-based surfactant system, natural solubilizer, plant sugar alcohol, enzyme synergist stabilizer, pH adjuster and deionized water to prepare the base solution; S4. Add the bilayer plant polysaccharide-triggered microencapsulation complex enzyme system to the base solution to obtain the low-irritation, high-cleaning plant-based laundry detergent composition.
8. The preparation method according to claim 7, characterized in that, In step S1, the modified inulin is prepared by the following method: inulin is etherified with a tertiary amine reagent containing an epoxy group to obtain an inulin intermediate with a tertiary amine side chain, and then the inulin intermediate is reacted with a beet alkalizing agent to obtain modified inulin; the plant-derived fatty alcohol polyoxyethylene ether carboxylate is prepared by the following method: the plant-derived fatty alcohol polyoxyethylene ether is reacted with a carboxymethylating agent and neutralized to obtain the plant-derived fatty alcohol polyoxyethylene ether carboxylate.
9. The preparation method according to claim 7, characterized in that, Step S2 includes: mixing the composite bio-enzyme with the inner layer enzyme-stabilizing vitrification protective layer component to form an inner core liquid, and granulating the inner core liquid to obtain inner particles; contacting the inner particles with the outer layer isolating surfactant and triggering release layer component, so that the outer layer isolating surfactant and triggering release layer component is formed on the outer surface of the inner particles; and then drying to obtain a bilayer plant polysaccharide-triggered microencapsulated composite enzyme system.
10. The preparation method according to claim 7, characterized in that, In step S4, after the temperature of the base liquid drops below 30°C, the bilayer plant polysaccharide-triggered microencapsulation complex enzyme system is added to the base liquid and mixed using a low-shear dispersion method to obtain the low-irritation, high-cleaning plant-based laundry detergent composition.