Amino acid composite vegetable fat shampoo soap and preparation method thereof

Abstract

The invention relates to the technical field of daily chemical products, and discloses an amino acid composite vegetable fat shampoo soap and a preparation method thereof, the raw materials of the shampoo soap comprise an amino acid surfactant, mango seed wax, coconut oil, modified wheat germ oil, modified shea butter, modified camellia seed oil, vine tea, polygonatum odoratum, cacumen biotae and polygonum multiflorum essential oil. Wherein the modified grease is prepared from base oil through a specific enzymolysis process and is rich in diglyceride and monoglyceride. The preparation method comprises the steps of step-by-step temperature control mixing of the raw materials, compression molding, heat setting and curing. The mango seed wax is utilized to construct a hydrophobic skeleton, and the polar filling and hot-pressing shaping process of the modified grease is matched, so that the structural strength and water resistance of the soap body are improved, the problems that the traditional amino acid soap is easy to absorb moisture, soften and become burnt are effectively solved, and meanwhile, the product is endowed with quick foaming ability and excellent after-washing conditioning feeling.

Description

Technical Field

[0001] This invention relates to the field of daily chemical products technology, specifically to an amino acid compound plant oil shampoo soap and its preparation method. Background Technology

[0002] In recent years, with the increasing demand from consumers for environmentally friendly and gentle cleansing products, amino acid shampoo bars have gradually become a market hotspot due to their biodegradability, small size, and low scalp irritation. However, in practical applications, amino acid shampoo bars still face several technical challenges, including structural stability, balanced washing experience, and preservation of active ingredients.

[0003] First, amino acid surfactants generally have strong hydrophilicity and hygroscopicity. In environments with high relative humidity, such as bathrooms, traditional amino acid soaps easily absorb moisture from the air or are difficult to dry after getting wet, causing the soap to soften, deform, and develop a sticky paste on the surface. This paste-like phenomenon not only severely affects the user experience but also reduces the structural strength of the soap, making it prone to breakage or excessive consumption during use, thus shortening the product's lifespan. Existing technologies typically use large amounts of stearic acid or inorganic fillers to increase hardness, but this often sacrifices the product's foaming performance and gentleness.

[0004] Secondly, striking a balance between cleansing power and conditioning feel is difficult with shampoo bars. To address the dryness and difficulty in combing hair after washing with pure amino acid-based shampoo, plant oils are usually added to the formula for moisturizing. However, the main component of natural plant oils is triglycerides, which have a significant defoaming effect in washing systems. Adding too much will lead to difficulty in lathering, resulting in sparse and unstable foam; adding too little will fail to provide conditioning and make it difficult to achieve smooth hair without using silicone oil. Many current products struggle to achieve both rich, fine foam and a moisturizing, smooth feel after washing.

[0005] In addition, to achieve good hair care effects, shampoo bars often contain plant oils rich in unsaturated fatty acids and active plant extracts. These ingredients are quite sensitive to light, heat, and oxygen. Current manufacturing processes mostly use high-temperature hot-melt casting, and prolonged high-temperature treatment can easily destroy heat-sensitive active ingredients and accelerate the oxidation reaction of oils, causing the product to develop a rancid odor during its shelf life or later in its use, affecting the product's stability and safety. Summary of the Invention

[0006] To address the shortcomings of existing technologies, this invention provides an amino acid-based compound plant oil shampoo bar and its preparation method. This solves the problems of existing amino acid shampoo bars being prone to absorbing moisture and softening in humid environments, becoming soggy, having low structural strength, poor foaming ability after adding plant oils, dry hair after washing, and unstable products due to the easy oxidation and degradation of active oils and functional ingredients in the formula.

[0007] To address the above problems, the present invention provides the following technical solution: In a first aspect, the present invention provides an amino acid-complex plant oil shampoo bar, which adopts the following technical solution: An amino acid-based compound plant oil shampoo bar, made from raw materials comprising the following weight percentages: Amino acid surfactants 25%-35%; Mango pit wax 5%-10%; Coconut oil 8%-12%; Modified wheat germ oil 5%-10%; Modified shea butter 5%-10%; Modified camellia seed oil 27%-35%; Vine tea essential oil 2%-6%; Polygonatum odoratum essential oil 1%-2%; Arborvitae leaf essential oil 0.5%-1.5%; Polygonum multiflorum essential oil 0.5%-1.5%.

[0008] By employing the above technical solution, this invention utilizes lipid components with different melting points and polarities to construct a multi-level solid network, achieving a balance between the structural stability of the soap in a humid environment and its gentle conditioning during washing. Its mechanism of action is mainly manifested in the following three aspects: First, mango pit wax, as a high-melting-point hard plant wax, acts as a hydrophobic framework material in the system. Mango pit wax contains long-chain saturated fatty acid esters with dense crystals, which can block continuous channels for water to penetrate into the soap body, thereby reducing the degree of softening after soaking and solving the problem of the soap becoming soggy.

[0009] Secondly, modified wheat germ oil, modified shea butter, and modified camellia seed oil constitute a unique polar lipid-filled phase. These oils undergo specific enzymatic modification, converting some triglycerides into surface-active diglycerides and monoglycerides. These partially glyceride molecules possess both hydrophilic (hydroxyl) and hydrophobic (long-chain alkyl) groups. In the soap's microstructure, they are embedded between the micelles of the amino acid surfactant and the grain boundaries of the mango kernel wax, increasing the interfacial bonding between components, preventing phase separation, and further improving the soap's abrasion resistance and crack resistance.

[0010] Finally, the compound plant essential oil components (vine tea, Solomon's seal, arborvitae leaf, and Polygonum multiflorum) not only give the product specific scalp care effects, but the terpenes and phenolic compounds in them can also act as natural antioxidants, synergistically stabilizing the oil system and preventing the modified oil from oxidative rancidity during its use period.

[0011] Preferably, the amino acid surfactant is selected from one or a combination of several of sodium lauroyl glutamate, potassium cocoyl glycinate, and sodium cocoyl ethanesulfonate.

[0012] By employing the above-mentioned technical solutions, different types of amino acid surfactants can be blended to adjust the richness and fineness of foam. Sodium lauroyl glutamate has good cleaning power in a weakly acidic environment and extremely low skin irritation; potassium cocoyl glycinate provides rich foam; and sodium cocoyl ethanesulfonate helps improve tolerance to hard water.

[0013] Preferably, the modified wheat germ oil, the modified shea butter, and the modified camellia seed oil are each selected from corresponding vegetable oils as base oils and prepared by a method including the following steps: The base oil is added to a reaction vessel and heated to 40-45°C. 15%-20% of the base oil mass of deionized water is added, and the mixture is stirred at 300-500 rpm to obtain an emulsion. The pH value is adjusted to 6.0-7.0 using a pH adjuster, and 0.1%-0.3% of the base oil mass of lipase is added. The mixture is stirred and reacted at a constant temperature of 40-45°C for 4-6 hours. After the reaction is completed, the temperature is increased, the mixture is centrifuged, the aqueous phase and precipitate are removed, the upper oil phase is collected and vacuum dried.

[0014] By employing the above-mentioned technical solution, this specific modification process is key to obtaining high-performance shampoo bars. Its mechanism lies in the molecular modification of natural oils through controlled enzymatic hydrolysis. The first step, oil-water emulsification stage: by shearing and stirring at 300-500 rpm and using a 15%-20% aqueous phase, an oil-in-water or water-in-oil microemulsion environment suitable for interfacial enzyme catalysis is constructed, increasing the contact area between the enzyme and the substrate.

[0015] The second step, the targeted enzymatic hydrolysis stage: Under mild conditions of pH 6.0-7.0 and 40-45℃, lipase selectively hydrolyzes the ester bonds on triglycerides. The reaction time is controlled to be 4-6 hours, ensuring the hydrolysis reaction is in an intermediate state, not completely hydrolyzing into fatty acids and glycerol, but instead generating a mixed oil system rich in diglycerides and monoglycerides.

[0016] The third step is to analyze the characteristics of the product. The DAG and MAG in the modified oil have liquid crystal forming capabilities. During the shampooing process, they can be adsorbed onto the hair surface to form a breathable protective film, filling the gaps between the hair cuticles and providing a smooth conditioning effect without silicone oil. At the same time, in the soap, these polar lipids reduce the surface tension of water, promote rapid foaming of the soap during washing, and solve the problem of difficult foaming of traditional high-oil soap.

[0017] Preferably, the process conditions for raising the temperature after the reaction are: raising the temperature to 85-90℃ and maintaining it for 15-20 minutes; the conditions for vacuum drying are a vacuum degree of -0.08MPa to -0.09MPa and a temperature of 55-65℃; the pH adjuster is selected from citric acid or sodium bicarbonate.

[0018] By employing the above technical solutions, high-temperature inactivation ensures the termination of the enzyme reaction, preventing residual enzymes from continuing to decompose oils during the finished product's storage period, leading to rancidity or soap structure collapse. The vacuum drying step effectively removes residual moisture from the reaction system, resulting in extremely low water content in the modified oils. This facilitates anhydrous or low-water miscibility with mango kernel wax and surfactants, ensuring the finished product's hardness and preservative properties. The selection of a pH adjuster ensures optimal enzyme activity, and the citric acid or sodium bicarbonate residues are safe and harmless to humans.

[0019] Secondly, the present invention provides a method for preparing an amino acid-based compound plant oil shampoo bar, employing the following technical solution: A method for preparing an amino acid-based compound plant oil shampoo bar includes the following steps: S1. Weigh out the amino acid surfactant and mango kernel wax according to the formula, mix them, heat and stir; S2. Stop heating and wait for the material to cool to 20-25℃. Add coconut oil, modified wheat germ oil, modified shea butter and modified camellia seed oil to the mixture and stir to obtain soap base. S3. Add vine tea essential oil, Solomon's seal essential oil, arborvitae leaf essential oil and Polygonum multiflorum essential oil to the soap base, and continue stirring to obtain soap material; S4. The soap material is injected into the mold, mechanical pressure is applied to press and shape it, and then the mold is placed in a constant temperature drying oven for heat setting. S5. After removing the mold and cooling to room temperature, unmold the soap and place it in a cool, ventilated environment to mature.

[0020] By adopting the above technical solution, this invention employs a step-by-step controlled process of hot-melt skeleton construction, low-temperature lipid filling, and hot-pressing shaping, which differs from traditional cold-process or hot-process soap making. Its process principle and technical effects are reflected in the following aspects: First, stepwise temperature control enables the orderly assembly of the structural and functional phases. In stage S1, heating melts the mango seed wax and encapsulates solid amino acid surfactant particles, forming a continuous hydrophobic framework layer. In stage S2, the modified oil is added after cooling the system to 20-25°C; this low-temperature operation is crucial. Because the modified oil contains heat-sensitive diglycerides and monoglycerides, low-temperature addition avoids transesterification or oxidative degradation caused by high temperatures, and also prevents the liquid oil from prematurely dissolving and destroying the newly formed microcrystalline structure of the mango seed wax. This framework-first, filler-later approach allows the oil to be dispersed in the wax-based network in the form of microdroplets, rather than being completely miscible, thus maintaining the soap's high hardness while ensuring a smooth washing experience.

[0021] Secondly, the pressing and heat-setting process in step S4 introduces a physical cross-linking mechanism. Mechanical pressure causes the material particles to pack tightly, eliminating macroscopic pores; the subsequent heat-setting process is similar to annealing in materials science. Under isothermal conditions, the mango kernel wax and modified oil undergo molecular chain rearrangement and secondary crystallization, eliminating the internal stress generated by pressing and promoting thermal fusion between particle interfaces. This treatment eliminates micro-cracks and significantly improves the water resistance and resistance to rotting of the finished product.

[0022] Preferably, in step S1, the heating temperature is controlled at 48-52℃, the stirring speed is 60-100rpm, and the stirring time is 40-50 minutes.

[0023] By adopting the above technical solution, the temperature range of 48-52℃ is slightly higher than the softening point of mango seed wax, but much lower than the decomposition temperature of amino acid surfactants. At this temperature, the mango seed wax is in a semi-molten, high-viscosity state. Through low-speed shearing at 60-100 rpm, uniform coating of surfactant powder can be achieved rather than simple liquid-phase mixing, laying the foundation for the subsequent formation of a dense waterproof layer.

[0024] Preferably, in step S2, the stirring speed is 100-150 rpm and the stirring time is 25-35 minutes; in step S3, the stirring speed is 80-120 rpm and the stirring time is 25-35 minutes.

[0025] By employing the above technical solution, appropriately increasing the rotation speed to 100-150 rpm in the low-temperature (20-25℃) stage is to provide sufficient shear force in the system with increased viscosity, allowing the liquid modified oil to be evenly dispersed and penetrate into the semi-solid matrix. Slightly reducing the rotation speed in the S3 stage is to reduce frictional heat generation, prevent the loss of volatile essential oil components, and ensure the preservation of aroma and active ingredients.

[0026] Preferably, in step S4, the applied mechanical pressure is 0.1-0.3 MPa, the holding time is 10-20 seconds, the heat setting temperature is 45-50℃, and the time is 20-24 hours.

[0027] By adopting the above technical solution, the process parameters determined the final microstructure of the soap.

[0028] Pressure of 0.1-0.3 MPa is considered low-pressure molding, which aims to initially shape the material without damaging its internal crystal structure.

[0029] The heat setting temperature of 45-50℃ is chosen based on the crystal transformation temperature of mango kernel wax. Maintaining this temperature range for 20-24 hours induces the diglycerides in the modified oil to co-crystallize with the mango kernel wax or form a stable crystal network (such as the β' crystal form). This stable crystal network significantly increases the melting point and hydrolysis resistance of the soap, which is a key step in solving the problem of soap softening upon contact with water.

[0030] Preferably, in step S5, the temperature of the curing environment is 20-25℃, the relative humidity is 40%-50%, and the curing time is 14-20 days.

[0031] By adopting the above technical solution, the curing process is a process of moisture balance and crystal lattice stabilization. Under specific temperature and humidity control, the trace amounts of free water remaining inside the soap body combine to form water of crystallization, or migrate to the surface and evaporate, further enhancing the mechanical strength of the soap body. The 14-20 day cycle ensures that all physicochemical changes (such as post-crystallization of oils and complete release of internal stress) reach a balanced state, guaranteeing the stability of the physicochemical properties of the finished product.

[0032] This invention provides an amino acid-based compound plant oil shampoo bar and its preparation method. It has the following beneficial effects: 1. This invention improves the physical strength and water resistance of the soap by introducing high-melting-point mango kernel wax in combination with a specific hot-pressing process. During the long-term heat setting process at 45-50℃, the mango kernel wax forms a dense crystalline network with the oil system, blocking the channels for water to penetrate into the soap body. This solves the problem of traditional amino acid soaps easily absorbing moisture and softening in humid environments, resulting in a pasty substance on the surface, and maintains the structural integrity of the soap body throughout its entire service life.

[0033] 2. This invention utilizes enzymatic modification technology to molecularly modify wheat germ oil, shea butter oil, and camellia seed oil, constructing a polar oil system rich in diglycerides and monoglycerides. The surface-active modified oils can synergistically interact with amino acid surfactants, reducing foaming resistance and achieving rapid and rich foaming. They can also adsorb onto the hair surface during washing to form a breathable protective film, overcoming the problem of difficult foaming in traditional plant oil soaps. At the same time, it gives hair a smooth and non-drying washing feel without adding silicone oil.

[0034] 3. This invention, through a specific blend of essential oils from vine tea, Solomon's seal, arborvitae leaves, and Polygonum multiflorum, endows the product with dual effects of nourishing the scalp and anti-oxidation. The active ingredients in the essential oils not only have a care effect but also act as natural antioxidants to stabilize the modified oil system with a high content of unsaturated fatty acids, preventing rancidity. Combined with the unique low-temperature addition process during preparation, it avoids the damage of heat-sensitive components to high temperatures, ensuring the retention rate of effective ingredients, extending the product's shelf life, and guaranteeing the stability of its effects. Detailed Implementation

[0035] The technical solutions of the present invention will be clearly and completely described below with reference to embodiments, comparative examples, and test examples. 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.

[0036] Preparation Examples 1-3: Preparation Example 1: This preparation example provides a modified camellia seed oil, including the following steps: 1000g of commercially available cold-pressed camellia seed oil was added to a reaction vessel and heated to 40℃. 150g of deionized water was added to the reaction vessel, and stirring was started at 300rpm to form an oil-water emulsion. The pH of the system was adjusted to 6.0 using citric acid, and 1.0g of lipase was added. The mixture was stirred continuously at a constant temperature of 40℃ for 6 hours. After the reaction was completed, the system was heated to 85℃ and held for 15 minutes to inactivate the lipase. The mixture was centrifuged at 4000rpm for 10 minutes to remove the aqueous phase and precipitate, and the upper oil phase was collected. The collected oil phase was vacuum dried at -0.08MPa and 60℃ for 30 minutes to obtain the modified camellia seed oil.

[0037] Preparation Example 2: This preparation example provides a modified wheat germ oil, comprising the following steps: 1000g of commercially available wheat germ oil was added to a reaction vessel and heated to 42℃. 175g of deionized water was added to the reaction vessel, and stirring was started at 400rpm to form an oil-water emulsion. The pH of the system was adjusted to 6.5 using citric acid or sodium bicarbonate, and 2.0g of lipase was added. The mixture was stirred continuously at a constant temperature of 42℃ for 5 hours. After the reaction, the system was heated to 88℃ and held for 18 minutes to inactivate the lipase. The mixture was centrifuged at 4000rpm for 10 minutes to remove the aqueous phase and precipitate, and the upper oil phase was collected. The collected oil phase was vacuum dried at -0.085MPa and 60℃ for 30 minutes to obtain the modified wheat germ oil.

[0038] Preparation Example 3: This preparation example provides a modified shea butter, comprising the following steps: 1000g of commercially available shea butter was added to a reaction vessel and heated to 45°C. 200g of deionized water was added to the reaction vessel, and stirring was started at 500 rpm to form an oil-water emulsion. The pH of the system was adjusted to 7.0 using sodium bicarbonate, and 3.0g of lipase was added. The mixture was stirred continuously at a constant temperature of 45°C for 4 hours. After the reaction was completed, the system was heated to 90°C and held for 20 minutes to inactivate the lipase. The mixture was centrifuged at 4000 rpm for 10 minutes to remove the aqueous phase and precipitate, and the upper oil phase was collected. The collected oil phase was vacuum dried at -0.09 MPa and 60°C for 30 minutes to obtain the modified shea butter.

[0039] Examples 1-3: Example 1

[0040] This embodiment provides an amino acid compound plant oil shampoo bar, which, by weight percentage, consists of: 25% sodium lauroyl glutamate, 10% mango kernel wax, 10% coconut oil, 5% modified wheat germ oil obtained in Preparation Example 2, 5% modified shea butter obtained in Preparation Example 3, 35% modified camellia seed oil obtained in Preparation Example 1, 6% vine tea essential oil, 2% Solomon's seal essential oil, 1% arborvitae leaf essential oil, and 1% Polygonum multiflorum essential oil.

[0041] The preparation method of this embodiment includes the following steps: Weigh out sodium lauroyl glutamate and mango kernel wax according to the formula, place them in a mixing container with a temperature control device, turn on the heating, control the material temperature at 48℃, start the stirring device, control the speed at 60 rpm, and continue stirring for 40 minutes to soften the mango kernel wax and mix it evenly with the surfactant. Stop heating and let the material cool naturally to 20°C. Add the formula amounts of coconut oil, modified wheat germ oil, modified shea butter, and modified camellia seed oil to the mixture in sequence. Increase the stirring speed to 100 rpm and continue stirring for 25 minutes to obtain a uniform soap base. Add the specified amounts of vine tea essential oil, Solomon's seal essential oil, arborvitae leaf essential oil, and Polygonum multiflorum essential oil to the soap base in sequence. Adjust the stirring speed to 80 rpm and continue stirring for 25 minutes to ensure the essential oils are evenly dispersed. The obtained soap material is injected into the mold, and a mechanical pressure of 0.1 MPa is applied and held for 10 seconds to press and shape it. Then, the mold is placed in a constant temperature drying oven at 45°C for 20 hours to heat set. After removing the mold and cooling to room temperature, unmold the soap. Place the unmolded soap in a cool, ventilated environment at 20°C and 50% relative humidity for 14 days to mature, and you will get the finished product. Example 2

[0042] This embodiment provides an amino acid compound plant oil shampoo bar, which, by weight percentage, consists of: 30% potassium cocoyl glycinate, 8% mango kernel wax, 12% coconut oil, 7% modified wheat germ oil obtained in Preparation Example 2, 7% modified shea butter obtained in Preparation Example 3, 29% modified camellia seed oil obtained in Preparation Example 1, 4% vine tea essential oil, 1% Solomon's seal essential oil, 1% arborvitae leaf essential oil, and 1% Polygonum multiflorum essential oil.

[0043] The preparation method of this embodiment includes the following steps: Weigh out the potassium cocoyl glycinate and mango kernel wax according to the formula, place them in a mixing container with a temperature control device, turn on the heating, control the material temperature at 50℃, start the stirring device, control the speed at 80rpm, and continue stirring for 45 minutes to soften the mango kernel wax and mix it evenly with the surfactant. Stop heating and let the material cool naturally to 22°C. Add the formula amounts of coconut oil, modified wheat germ oil, modified shea butter, and modified camellia seed oil to the mixture in sequence. Increase the stirring speed to 125 rpm and continue stirring for 30 minutes to obtain a uniform soap base. Add the formula amounts of vine tea essential oil, Solomon's seal essential oil, arborvitae leaf essential oil and Polygonum multiflorum essential oil to the soap base in sequence. Adjust the stirring speed to 100 rpm and continue stirring for 30 minutes to ensure that the essential oils are evenly dispersed. The obtained soap material is injected into the mold, and a mechanical pressure of 0.2 MPa is applied and held for 15 seconds to press and shape it. Then, the mold is placed in a constant temperature drying oven at 48°C for 22 hours to heat set. After removing the mold and cooling to room temperature, unmold the soap. Place the unmolded soap in a cool, ventilated environment at 22°C and 45% relative humidity for 17 days to mature, and you will get the finished product. Example 3

[0044] This embodiment provides an amino acid compound plant oil shampoo bar, which, by weight percentage, consists of: 35% amino acid surfactant composition (sodium lauroyl glutamate and sodium cocoyl hydroxyethyl sulfonate mixed in a mass ratio of 1:1), 5% mango kernel wax, 8% coconut oil, 10% modified wheat germ oil obtained in Preparation Example 2, 10% modified shea butter obtained in Preparation Example 3, 27% modified camellia seed oil obtained in Preparation Example 1, 2% vine tea essential oil, 1% Solomon's seal essential oil, 1% arborvitae leaf essential oil, and 1% Polygonum multiflorum essential oil.

[0045] The preparation method of this embodiment includes the following steps: Weigh out the amino acid surfactant composition and mango kernel wax according to the formula, place them in a stirring container with a temperature control device, turn on the heating, control the material temperature at 52°C, start the stirring device, control the speed at 100 rpm, and stir continuously for 50 minutes to soften the mango kernel wax and mix it evenly with the surfactant. Stop heating and let the material cool naturally to 25°C. Add the formula amounts of coconut oil, modified wheat germ oil, modified shea butter and modified camellia seed oil to the mixture in sequence. Increase the stirring speed to 150 rpm and continue stirring for 35 minutes to obtain a uniform soap base. Add the formula amounts of vine tea essential oil, Solomon's seal essential oil, arborvitae leaf essential oil and Polygonum multiflorum essential oil to the soap base in sequence. Adjust the stirring speed to 120 rpm and continue stirring for 35 minutes to ensure that the essential oils are evenly dispersed. The obtained soap material is injected into the mold, and a mechanical pressure of 0.3 MPa is applied and held for 20 seconds to press and shape it. Then, the mold is placed in a constant temperature drying oven at 50°C for 24 hours to heat set. After removing the mold and cooling to room temperature, unmold the soap. Place the unmolded soap in a cool, ventilated environment at 25°C and 40% relative humidity for 20 days to mature, and you will get the finished product.

[0046] Comparative Examples 1-5: Comparative Example 1: This comparative example aims to verify the effect of custom-modified vegetable oils on product molding and permeability.

[0047] Compared with Example 2, the difference is that equal amounts of untreated commercially available wheat germ oil, commercially available shea butter, and commercially available camellia seed oil were used to directly replace the modified wheat germ oil, modified shea butter, and modified camellia seed oil in the formula, respectively, while the other raw materials and preparation steps were the same.

[0048] Comparative Example 2: This comparative example aims to verify the milder advantage of amino acid surfactant systems compared to traditional soap-based systems.

[0049] Compared with Example 2, the difference is that an equal amount of commercially available soap base granules (a mixture of sodium myristate, sodium laurate, and sodium stearate as the main components) are used to replace potassium cocoyl glycinate in the formula, while the other raw materials and preparation steps are the same.

[0050] Comparative Example 3: This comparative example aims to verify the impact of the specific low-temperature stepwise process of the present invention on product stability and appearance.

[0051] Compared with Example 2, the difference lies in the preparation process: all raw materials (surfactants, waxes, and oils) except for essential oils are mixed at one time, heated to 85°C and stirred until completely melted, cooled to 60°C and then the essential oils are added and mixed, and then directly poured into the mold to cool and solidify. The steps of low-temperature segmented mixing at 50°C and long-term low-temperature heat setting are omitted, while the rest are the same.

[0052] Comparative Example 4: This comparative study aims to verify the synergistic effects of the herbal essential oil system in the formulation.

[0053] Compared with Example 2, the difference is that: vine tea essential oil, Solomon's seal essential oil, arborvitae leaf essential oil and Polygonum multiflorum essential oil are not added, and the missing weight parts are made up by coconut oil in the formula. The other raw materials and preparation steps are the same.

[0054] Comparative Example 5: This comparative example aims to verify the unique feel and performance of mango pit wax as a structural agent.

[0055] Compared with Example 2, the difference is that an equal amount of industrial-grade stearic acid is used to replace the mango kernel wax in the formula, while the other raw materials and preparation steps are the same.

[0056] Test Examples 1-7: Test Example 1: Physical stability and heat resistance oil separation test of finished product Experimental instructions and procedures: This test aims to examine the structural stability and oil retention capacity of shampoo bars under thermal stress, specifically by measuring the amount of oil released after being left to stand at high temperature for quantitative evaluation.

[0057] The experimental samples were the finished products prepared in Examples 1-3, as well as the finished products of Comparative Example 1 (without modified oil), Comparative Example 3 (without low-temperature stepwise process), and Comparative Example 5 (using stearic acid instead of mango kernel wax).

[0058] The specific operating steps are as follows: Sample pretreatment: Cut the freshly demolded and cured shampoo bars from each group into standard sample blocks with dimensions of 30mm×30mm×10mm, accurately weigh their initial mass (m0), and record it to 0.001g. Prepare 5 parallel sample blocks for each group.

[0059] Thermal stress treatment: Place the above sample block at the bottom with pre-weighed oil-absorbing filter paper (m). paper1 Place the culture dish in a constant temperature and humidity chamber set at 40℃±0.5℃, with the relative humidity controlled at 60%.

[0060] Static observation: Keep the sample at a constant temperature for 30 days. Do not move the sample during this period to avoid mechanical vibration interfering with the natural migration of the oil.

[0061] Data Collection: After 30 days, remove the petri dish and allow it to cool to room temperature. Carefully remove the soap block, observe its surface condition, and immediately weigh the filter paper after oil absorption (m). paper2 ).

[0062] Calculation indicators:

[0063] Experimental data: Table 1. Statistical data on oil separation amount of each group of samples after 30 days of storage at 40℃ Group initial mass (g) m0 (g) Filter paper weight gain (mg) m oil (mg)]]> Oil separation rate (%) Appearance status record Example 1 9.842 5.21 0.053 The surface is dry and the edges are sharp. Example 2 9.815 4.08 0.042 Dry surface, dense structure Example 3 9.856 6.35 0.064 The surface is slightly moist and free of droplets. Comparative Example 1 9.833 148.72 1.512 There is obvious oil buildup at the bottom and the surface is greasy. Comparative Example 3 9.798 89.44 0.913 The surface is covered with tiny oil droplets, and the texture becomes softer. Comparative Example 5 9.821 32.19 0.328 White crystals are visible on the surface, with a small amount of oil seepage. Note: The data in the table is the arithmetic mean of 5 parallel samples. The original data may have random fluctuations within ±5%.

[0064] Conclusion Analysis: Based on the experimental data and the mechanism of the technical solution of this invention, the analysis is as follows: The samples in Examples 1 to 3 maintained an oil separation rate below 0.07% under prolonged thermal stress, and their appearance remained intact and dry. This indicates that the system constructed in this invention possesses excellent oil retention capabilities. The mechanism lies in the fact that the enzymatically modified vegetable oil contains a high proportion of monoglycerides and diglycerides. These two types of substances possess both hydrophilic hydroxyl groups and lipophilic long-chain alkyl groups in their molecular structure, acting as lattice modifiers and co-emulsifiers in the system. They can embed into the solid framework formed by mango kernel wax and amino acid surfactants, forming a denser and more elastic microcrystalline network, thereby effectively locking in liquid vegetable oil molecules and preventing their migration to the surface when thermal motion intensifies.

[0065] In contrast, Comparative Example 1 used unmodified natural triglycerides. Due to the lack of bridging effect between monoglycerides and diglycerides, the nonpolar triglycerides had poor compatibility with the polar surfactant skeleton, resulting in severe phase separation at high temperatures, manifested as an extremely high oil separation rate (1.512%).

[0066] Comparative Example 3, which employed a high-temperature, one-time melting process, showed a significantly higher oil separation rate (0.913%) compared to the Example. This is because the high-temperature rapid cooling process disrupted the co-crystallization process between the mango pit wax and the modified oil, resulting in the formation of coarse grains and larger voids within the matrix, which weakened the capillary adsorption force of the matrix on the liquid oil.

[0067] Comparative Example 5 uses stearic acid instead of mango kernel wax. Although stearic acid has strong crystallinity, its crystallization speed is too fast, which easily causes phase repulsion and squeezes the oil out of the crystal lattice. In addition, stearic acid itself is prone to forming large crystals, resulting in whitening and blooming on the surface. Its oil stabilization performance (oil separation rate 0.328%) is not as good as that of the mango kernel wax system.

[0068] In summary, this invention solves the technical problems of high-content vegetable oil shampoo soap being prone to oiliness and having an unstable structure by combining enzymatically modified oils with a specific low-temperature cold processing process.

[0069] Test Example 2: Aqueous Solution pH and Buffer Stability Test Experimental instructions and procedures: This test aims to determine the acidity and alkalinity of different examples and comparative samples in aqueous solution, and to evaluate their pH stability at different concentrations, in order to verify the compatibility of the product system with the physiological environment of the human scalp.

[0070] The finished products prepared in Examples 1-3, as well as the finished products of Comparative Example 1 (traditional soap base formula) and Comparative Example 2 (unmodified oil formula) were selected as test subjects.

[0071] The specific operating steps are as follows: Solution preparation: Accurately weigh 1.00 g, 5.00 g, and 10.00 g of the pulverized sample powder for each group and place them in beakers. Add deionized water (boiled to remove carbon dioxide and cooled to 25°C, initial pH 6.98) to a final volume of 100.0 g, and stir magnetically until completely dissolved to obtain test solutions with mass fractions of 1%, 5%, and 10%, respectively.

[0072] Instrument calibration: The precision pH meter (accuracy ±0.01) was calibrated at three points using standard buffer solutions at pH 4.01, pH 6.86, and pH 9.18.

[0073] Measurement: Immerse the pH meter electrode in the solution to be tested, turn on slow stirring, and record the value after the reading stabilizes for 60 seconds. Prepare three parallel solutions independently for each concentration gradient of each sample group for measurement, and keep the test temperature constant at 25℃±1℃.

[0074] Experimental data: Table 2. pH values ​​of aqueous solutions at different concentrations for each group of samples. Group 1% concentration pH value (n=1,2,3) 1% average concentration 5% concentration pH value (n=1,2,3) 5% average concentration 10% concentration pH value (n=1,2,3) 10% average concentration Example 1 5.83,5.79,5.88 5.83 5.72,5.68,5.75 5.72 5.61,5.65,5.59 5.62 Example 2 6.21,6.15,6.25 6.20 6.08,6.12,6.05 6.08 5.92,5.98,5.95 5.95 Example 3 5.65,5.71,5.62 5.66 5.54,5.49,5.58 5.54 5.41,5.45,5.38 5.41 Comparative Example 1 9.87,9.92,9.85 9.88 10.15,10.11,10.18 10.15 10.32,10.28,10.35 10.32 Comparative Example 2 6.45,6.51,6.42 6.46 6.38,6.44,6.35 6.39 6.29,6.33,6.25 6.29 Note: Data records are not rounded and are retained to two decimal places, reflecting random errors in the experimental process.

[0075] Conclusion Analysis: Based on the above measurement data and the chemical composition characteristics of the formulation of this invention, the analysis is as follows: The pH values ​​of Examples 1 to 3 remained consistently between 5.4 and 6.2 at different concentrations. This range closely matches the physiological pH value (4.5-6.5) of the human scalp sebum film. The chemical mechanism lies in the fact that the amino acid surfactants used in this invention (such as sodium lauroyl glutamate and potassium cocoyl glycinate) are weak acid-weak base salts, which exist in hydrolysis and ionization equilibrium in aqueous solution. The amino acid residues (glutamate and glycine groups) in their molecular structure themselves constitute a certain buffering system.

[0076] More importantly, the data from the examples are slightly lower than those from Comparative Example 2 (unmodified oil formulation, pH approximately 6.4). This is because the modified vegetable oil added in the examples underwent controlled hydrolysis by lipase, resulting in a certain proportion of long-chain free fatty acids in the system. These weakly acidic free fatty acids undergo slight ionization at the aqueous interface, releasing a small number of protons (H+). + This allows the pH of the system to be fine-tuned to a more slightly acidic range. This endogenous acid regulation mechanism provides the product with excellent skin-friendliness without the need for the addition of large amounts of inorganic acid regulators.

[0077] In contrast, data from Comparative Example 1 (traditional soap base) showed a pH value above 9.8, which increased with concentration. This is because sodium fatty acid (the main component of soap base), as a strong base-weak acid salt, undergoes a strong hydrolysis reaction in water to produce sodium hydroxide and fatty acids, resulting in a highly alkaline solution. This high pH environment forcibly opens the scalp cuticles, causing hair fibers to swell, increasing friction and causing internal protein loss, leading to dryness and damage after washing.

[0078] Furthermore, the pH fluctuations in the example group were small (difference of approximately 0.2-0.3) when the concentration changed from 1% to 10%, demonstrating good buffering capacity. This means that even if the amount of water added changes during use, the acid-base environment of the product's liquid film when in contact with the scalp remains stable, and will not cause a severe chemical shock to the scalp's microecology.

[0079] Test Example 3: Foaming Performance and Foam Stability Test Experimental instructions and procedures: This test aims to quantitatively evaluate the foaming ability and foam stability of the various examples and comparative samples during the settling process. For shampoos with high oil content, oils typically have an anti-foaming effect; therefore, foaming performance is an important indicator for measuring product technological improvements.

[0080] The finished products prepared in Examples 1-3, as well as Comparative Example 1 (traditional soap base), Comparative Example 2 (unmodified oil formulation), and Comparative Example 4 (oil-free formulation) were selected as test subjects.

[0081] The specific operating steps are as follows: Solution preparation: Accurately weigh 1.00 g of each sample powder and dissolve it in 99.00 g of standard hard water with a hardness of 150 ppm (calculated as calcium carbonate). Heat and stir until completely dissolved, then cool to 40°C to obtain a 1.0% test solution.

[0082] Apparatus preparation: The stoppered graduated cylinder method is used. Prepare several 250mL stoppered ground glass graduated cylinders, wash and dry them.

[0083] Shaking and foaming: Measure 50.0 mL of the solution to be tested into a graduated cylinder and tighten the stopper. Fix the graduated cylinder vertically on a mechanical shaker, set the amplitude to 20 cm, the frequency to 120 times / min, and shake continuously for 60 seconds.

[0084] Data Records: Immediately after the oscillation stops (t=0), record the foam volume (V0, in mL), which is the difference between the upper foam level and the lower liquid level.

[0085] After standing for 5 minutes (t=5), record the foam volume again (V5, in mL).

[0086] Indicator Calculation: Foaming power is characterized by V0.

[0087] Foam stability (%) = (V5 / V0) × 100%.

[0088] Each group of samples was measured in parallel 5 times, and the arithmetic mean was taken.

[0089] Experimental data: Table 3. Results of foam volume and foam stability determination for each group of samples Group <![CDATA[Initial foam volume V0 (mL) (n = 1 - 5)]]> <![CDATA[V0 mean value (mL)]]> <![CDATA[Foam volume V5 (mL) after 5 minutes (n = 1 - 5)]]> <![CDATA[V5 Mean Value (mL)]]> Foam stability (%) Example 1 138,142,135,140,137 138.4 128,130,125,129,126 127.6 92.2 Example 2 145,148,144,150,146 146.6 135,139,136,140,137 137.4 93.7 Example 3 132,129,134,130,133 131.6 120,118,123,119,121 120.2 91.3 Comparative Example 1 185,180,188,182,186 184.2 145,140,148,142,146 144.2 78.3 Comparative Example 2 65,58,62,70,60 63.0 25,20,22,30,24 24.2 38.4 Comparative Example 4 170,168,172,165,175 170.0 110,105,115,108,112 110.0 64.7 Note: The data in the table reflects the differences in foaming under hard water conditions for different formulation systems.

[0090] Conclusion Analysis: Based on experimental data and surface chemistry principles, the analysis is as follows: Comparative Example 2 (unmodified oil) showed the lowest foaming volume (63.0 mL) and stability (38.4%). This aligns with the defoaming mechanism of triglycerides: unmodified vegetable oils are non-polar oils, easily spreading at the gas-liquid interface, leading to localized thinning and rupture of the foam film through a bridging mechanism. In amino acid surfactant systems, high triglyceride content inhibits foam formation and maintenance.

[0091] In contrast, Examples 1-3, while maintaining the same high oil content, achieved a foaming volume of 130-145 mL and a foam stability exceeding 90%. The mechanism lies in the presence of a large amount of monoglycerides and diglycerides in the enzymatically modified oil system. These two components possess amphiphilic structures (hydrophilic hydroxyl groups and lipophilic alkyl groups), exhibiting characteristics of nonionic surfactants. During foaming, monoglycerides and diglycerides act as auxiliary surfactants, co-adsorbing with amino acid surfactant molecules at the gas-liquid interface. This more compact mixed adsorption layer increases the surface viscosity and elasticity of the liquid film, effectively resisting liquid film drainage and gas diffusion, thereby blocking the defoaming effect of the oil and imparting a dense, long-lasting, creamy texture to the foam.

[0092] Although Comparative Example 1 (soap-based) and Comparative Example 4 (oil-free formula) had high initial foaming amounts, their stability was poor (78.3% and 64.7%, respectively). This is because the lack of structured oil support resulted in a thinner foam film from the pure surfactant, which was significantly affected by gravity drainage, causing the foam to collapse easily in a short time.

[0093] In summary, this invention, through modified oil technology, successfully solves the industry problem of poor foaming in high-oil formulations, achieving a balance between cleaning power, foaming properties, and moisturizing properties.

[0094] Test Example 4: Evaluation Test of Hair Combing Resistance and Smoothness Experimental instructions and procedures: This test aims to quantify the combing resistance of hair treated with different shampoo bars in wet and dry conditions using a texture analyzer, thereby evaluating the product's conditioning performance and smoothing effect. Lower combing force indicates a lower coefficient of friction on the hair surface and better smoothness.

[0095] The finished products prepared in Examples 1-3, as well as Comparative Example 1 (traditional soap base), Comparative Example 2 (unmodified oil formulation), and Comparative Example 4 (oil-free formulation) were selected as test subjects. A water treatment group was set up as a blank control.

[0096] The specific operating steps are as follows: Hair bundle pretreatment: Select a standard Asian black hair bundle (20cm long, 3.0g in weight), clean it with a 10% sodium lauryl sulfate solution to remove surface dirt and residual silicone oil, and dry it for later use. To simulate damaged hair, soak the hair bundle in a 3% hydrogen peroxide solution for 30 minutes, and then rinse it clean.

[0097] Sample preparation: Prepare a 10% aqueous solution for each group of shampoo soaps. Completely immerse the pretreated hair strands in the test solution and soak at a constant temperature of 35℃ for 3 minutes. After soaking, gently massage the hair strands 30 times with your fingertips in the direction of the hair cuticle.

[0098] Rinsing: Rinse the hair strands with 35℃ flowing deionized water for 30 seconds at a flow rate of 2L / min.

[0099] Wet combing test: Secure the washed, wet hair strands on the test platform of the texture analyzer. Use a dedicated combing probe to comb the hair strands at a speed of 200 mm / min, and record the maximum load force during the combing process. Repeat the combing 5 times for each hair strand.

[0100] Dry combing test: Hang the hair bundles in a constant temperature and humidity chamber (25℃, 60%RH) to dry for 24 hours, repeat the above combing test steps, and record the maximum load force when combing the dry hair.

[0101] Data statistics: Three different hair strands were tested in parallel for each sample group, and the arithmetic mean of all test data was taken.

[0102] Experimental data: Table 4. Results of maximum load force measurement of hair strands after wet and dry combing after treatment in each group of samples. Group Maximum load force of wet combing (g) (measurements) Average wet combing weight (g) Maximum load capacity of dry combing (g) (measurements) Average dry combing weight (g) Reduction rate (relative to control group, %) (wet / dry) Blank control 42.5,41.8,43.1,42.0,42.9 42.46 35.6,36.1,35.2,35.8,36.5 35.84 - / - Example 1 9.8,10.2,9.5,10.5,9.9 9.98 7.2,7.5,7.1,7.8,7.3 7.38 76.5 / 79.4 Example 2 8.5,8.2,8.8,8.4,8.6 8.50 6.5,6.2,6.8,6.4,6.6 6.50 80.0 / 81.9 Example 3 10.8,11.2,10.5,11.0,10.9 10.88 8.1,8.4,7.9,8.5,8.2 8.22 74.4 / 77.1 Comparative Example 1 58.2,60.5,57.8,59.1,58.9 58.90 48.5,50.2,47.9,49.3,48.8 48.94 -38.7 / -36.6 Comparative Example 2 18.5,19.2,17.8,18.9,18.2 18.52 14.2,14.8,13.9,14.5,14.1 14.30 56.4 / 60.1 Comparative Example 4 35.6,36.2,35.1,35.8,36.0 35.74 28.5,29.1,28.2,28.8,28.4 28.60 15.8 / 20.2 Note: The lower the load force value, the better the smoothness; due to soap scum deposition, the combing force of Comparative Example 1 is actually higher than that of the control group, showing a negative reduction rate, - / - indicates not applicable.

[0103] Conclusion Analysis: Based on the combined experimental data and the physicochemical theory of hair surface, the analysis is as follows: The hair strands treated in Examples 1-3, whether combed wet or dry, showed significantly lower maximum load force than their respective proportions, with a reduction rate exceeding 75%. This confirms the advantages of the present invention in improving hair smoothness.

[0104] Mechanistically, Comparative Example 1 (soap base) caused a sharp increase in combing force (worse than the control group), which is attributed to its high pH value causing the hair cuticles to open, and the calcium and magnesium ions in hard water combining with fatty acid ions to form insoluble calcium soap (soap scum), which is deposited in the gaps between the hair cuticles, increasing surface roughness and the coefficient of friction.

[0105] Although Comparative Example 2 (unmodified oil) reduced combing power, its effect was not as good as that of Example 1. This is because unmodified triglyceride molecules are larger in size and lack polar groups, resulting in weaker affinity with the negatively charged surface of damaged hair. They are difficult to form a uniform adsorption film and are easily washed away by water during rinsing, leading to a false smoothness or short-lasting conditioning effect.

[0106] The superior performance of this invention stems from the synergistic effect of the modified vegetable oil and the amino acid system. First, the monoglycerides and diglycerides produced by enzymatic hydrolysis contain hydrophilic hydroxyl groups and lipophilic fatty acid chains, exhibiting significant amphiphilicity. This structure allows them to be directionally adsorbed onto the hair protein surface through polar interactions, while the hydrophobic chains align outwards, constructing a biomimetic hydrophobic film that effectively fills the gaps in damaged hair cuticles and reduces surface energy. Second, the weakly acidic environment of the amino acid surfactant promotes cuticle closure, further smoothing the hair surface.

[0107] In addition, the terpenes in the essential oils of vine tea and arborvitae leaves in the system act as natural solvents and penetrants, promoting the penetration of lipid components into the hair cortex. This not only achieves physical smoothness on the surface but also improves the internal flexibility of the hair strands, resulting in extremely low electrostatic friction resistance in the dry combing test.

[0108] Test Example 5: Antibacterial Activity Test Against Malassezia furfur Experimental instructions and procedures: This test aimed to evaluate the inhibitory effect of each group of shampoo soap samples on Malassezia furfur, a common pathogenic fungus of the scalp. This fungus is a major source of dandruff and seborrheic dermatitis. The diameter of the inhibition zone was determined by the agar perforation diffusion method to quantify the synergistic antibacterial efficacy of the modified oil carrier and the herbal essential oil system in the product.

[0109] The test subjects were Examples 1-3, Comparative Example 2 (unmodified oil formula, containing essential oil), Comparative Example 4 (oil-free formula, without essential oil), and positive control group (commercially available shampoo containing 1% ketoconazole).

[0110] The specific operating steps are as follows: Preparation of bacterial suspension: The standard strain of *Malassezia furfur* was inoculated onto modified Leeming-Notman agar slant and incubated at 37°C for 3 days. The bacterial growth was washed away with sterile physiological saline, and the bacterial suspension concentration was adjusted to 1×10⁻⁶. 6 CFU / mL.

[0111] Preparation of bacterial plates: Take 20 mL of the modified culture medium that has been melted and cooled to about 50°C, add 1 mL of the above bacterial suspension, mix well and pour into a sterile Petri dish, and let it stand to solidify.

[0112] Sample addition: Use a 6mm diameter sterile punch to create quincunx patterns on the solidified agar plate. Prepare a 50mg / mL aqueous solution of each shampoo bar (sterilized by filtration through a 0.22μm membrane). Inject 50μL of the test solution into each well. Add an equal volume of ketoconazole solution to the positive control group and sterile deionized water to the negative control group.

[0113] Incubation and Measurement: Invert the petri dishes and incubate them in a 37℃ incubator for 48 hours. Observe the formation of inhibition zones around the wells and measure the diameter of the inhibition zones (including the pore diameter) using a vernier caliper cross-section method, accurate to 0.02 mm.

[0114] Statistics: Three plates were prepared in parallel for each sample group, and three replicate wells were set in each plate, for a total of nine data points. The arithmetic mean was taken.

[0115] Experimental data: Table 5. Results of inhibition zone diameter determination for each group of samples against Malassezia furfur Group Measurement value of plate 1 (mm) Measurement value of plate 2 (mm) Measured value (mm) for plate 3 Mean (mm) Relative potency (%) (relative to positive control) negative control 6.00,6.00,6.00 6.00,6.00,6.00 6.00,6.00,6.00 6.00 0.0 Positive control 28.42,28.15,28.60 27.98,28.34,28.22 28.50,28.06,28.44 28.30 100.0 Example 1 20.15,20.48,19.88 20.32,20.05,20.60 19.95,20.24,20.10 20.20 71.4 Example 2 19.56,19.80,19.42 19.65,19.38,19.75 19.50,19.85,19.60 19.61 69.3 Example 3 21.05,20.88,21.20 20.95,21.15,20.78 21.32,21.02,20.90 21.03 74.3 Comparative Example 2 14.25,13.88,14.10 14.05,14.32,13.95 14.15,13.85,14.20 14.08 49.8 Comparative Example 4 8.25,8.40,8.15 8.32,8.10,8.55 8.20,8.35,8.05 8.26 29.2 Note: A diameter of 6.00 mm indicates no inhibition zone (this refers to the diameter of the perforation); the weak inhibition zone shown in Comparative Example 4 is mainly due to the antibacterial properties of the surfactant itself.

[0116] Conclusion Analysis: Based on microbiological principles and the structure-activity relationship of the formulation of this invention, the analysis is as follows: Examples 1-3 exhibited significant antibacterial activity, with inhibition zone diameters reaching approximately 70% of the positive control group and superior to Comparative Example 2 (unmodified oil group). This result confirms the effectiveness of the present invention in inhibiting dandruff fungi, and its mechanism involves two aspects: release of active ingredients and enhanced penetration by the carrier.

[0117] First, the arborvitae leaf, Polygonum multiflorum, and vine tea essential oils added to the formula contain terpenoids and flavonoids such as thujone and dihydromyricetin. These active molecules can disrupt the integrity of fungal cell walls and interfere with cell membrane permeability, thereby inhibiting fungal growth.

[0118] Secondly, the significant differences between the examples and Comparative Example 2 reveal the crucial role of the modified vegetable oil. Malassezia furfur is a lipophilic fungus; conventional triglycerides (Comparative Example 2) can be utilized by this fungus as a carbon source to some extent, or, due to their larger molecular size and non-polar characteristics, they can encapsulate the active ingredients of the essential oil within the oil droplet core, hindering their diffusion into the aqueous agar matrix. Conversely, the enzymatically modified oil used in this invention is rich in monoglycerides and diglycerides. These two components have an amphiphilic structure similar to emulsifiers, effectively reducing the oil-water interfacial tension and dispersing the herbal essential oil into smaller micelles. This micromicelle structure not only improves the solubility and diffusion rate of the essential oil in the aqueous medium (manifested as a larger inhibition zone), but also, because monoglycerides themselves have a certain ability to disrupt lipid membranes, they produce a synergistic membrane interference effect with the essential oil components, significantly enhancing the overall antibacterial efficacy.

[0119] Comparative Example 4 (without essential oil soap base) showed only a very weak inhibition zone, indicating that simple amino acid surfactants are insufficient to effectively control pathogenic bacteria and must rely on the organic combination of essential oil active ingredients and modified oil carriers.

[0120] Test Example 6: Human Sensory Evaluation and User Experience Test Experimental instructions and procedures: This test aims to comprehensively evaluate various sensory indicators of shampoo bars during actual washing and conditioning through human trials, including lathering quality, rinsing ease, hair condition after drying, and scalp comfort. This test reflects the conversion of laboratory data into practical applications and verifies the product's suitability for different hair types.

[0121] The test subjects were the finished products prepared in Examples 1-3, as well as Comparative Example 1 (traditional soap base formula) and Comparative Example 2 (unmodified oil formula) as evaluation samples.

[0122] The specific operating steps are as follows: Volunteer Recruitment: We are recruiting 60 volunteers aged 18-45, half male and half female, who must have good scalp health and no history of serious skin diseases. The volunteers will be randomly divided into 5 groups of 12 each.

[0123] Blind design: A double-blind testing method was used. All samples were removed from their outer packaging and labels, and were only marked with random numerical codes (such as Sample A, Sample B, etc.) before being distributed to each group of volunteers.

[0124] Trial period: Each volunteer used the designated sample to wash their hair continuously, once every 2 days, for a total of 14 days.

[0125] Evaluation Dimensions: After the trial period, volunteers will complete a questionnaire based on the "Sensory Evaluation Standards for Shampoo Products." The rating will be on a 10-point scale (1 point represents extremely poor experience, and 10 points represent extremely good experience). Evaluation indicators include: Foaming density: Whether the foam is rich, fine, and long-lasting.

[0126] Easy to rinse: Whether it is quick and clean when rinsed, without any slippery or sticky residue.

[0127] Post-wash volume: Does the hair naturally fluffy and not flat after drying?

[0128] Scalp soothing sensation: Does the scalp feel tight, dry, itchy, or stinging after washing? (The higher the score, the more comfortable and without any discomfort.)

[0129] Hair shine: The visual shine of hair after it has dried.

[0130] Experimental data: Table 6. Statistical Table of Volunteer Sensory Evaluation Scores Group Foaming density (mean) Easy to rinse and clean (mean) Fluffiness after washing (average) Scalp soothing sensation (mean) Hair shine (average) Overall satisfaction (weighted) Example 1 8.75 8.92 8.65 9.15 8.42 8.84 Example 2 9.05 8.85 8.58 9.30 8.25 8.88 Example 3 8.60 8.78 8.82 8.95 8.68 8.76 Comparative Example 1 9.25 8.45 6.20 4.55 5.80 6.35 Comparative Example 2 5.40 4.25 5.15 8.20 6.55 5.68 Note: The data is the arithmetic mean of the scores of 12 volunteers in each group; Comparative Example 1 had a high foaming score but extremely low comfort level due to the characteristics of soap base; Comparative Example 2 had an extremely low rinsing score because the oils were not modified.

[0131] Conclusion Analysis: Based on sensory evaluation data from volunteers, combined with the physicochemical behavior of the formulation system, the following conclusions are drawn: The example group scored significantly higher than Comparative Example 1 (mean 4.55) on the scalp soothing index (mean > 9.0). Comparative Example 1 used a sodium fatty acid soap-based system, whose high pH value led to excessive degreasing of the scalp stratum corneum, damaging the sebum barrier and causing increased transepidermal water loss, resulting in a noticeable tightness and dryness. In contrast, the example group used an amino acid surfactant combined with modified plant oils, resulting in a weakly acidic system that is compatible with the scalp's physiological environment. Furthermore, the retained lipid components in the modified oils could replenish some of the washed-off sebum in a timely manner, maintaining the hydration of the stratum corneum.

[0132] In terms of ease of rinsing, the Example Group (mean approximately 8.8) significantly outperformed Comparative Example 2 (mean 4.25). The unmodified triglycerides in Comparative Example 2 are highly hydrophobic, easily forming a difficult-to-remove oil film on the hair surface, resulting in a sticky and difficult-to-rinse feel. Furthermore, the weight of this oil film causes the hair to become flat and limp after drying (low volume score). In contrast, the enzymatically modified monoglycerides and diglycerides in the Examples have an amphiphilic structure, rapidly self-emulsifying during rinsing, carrying away excess oil with the water flow, leaving only a monolayer-level breathable hydrophobic film on the hair surface. This characteristic solves the residue problem commonly faced by high-oil formulations, achieving a balance between moisturizing and refreshing.

[0133] Furthermore, the hair in the example group scored higher in shine, which is attributed to the microcrystalline structure formed by the mango seed wax and modified oils during the heat setting process. This structure deposits on the hair cuticle surface during shampooing, filling damaged gaps, reducing diffuse reflection and enhancing specular reflection, thus presenting a healthy shine on a macroscopic scale.

[0134] In summary, the technical solution of this invention, while ensuring cleaning power, overcomes the shortcomings of traditional soap bases (dryness and skin irritation) and traditional oil soaps (stickiness and difficulty in rinsing) through oil modification technology, and has excellent market application potential.

[0135] Test Example 7: Resistance to smudging and abrasion resistance test Experimental instructions and procedures: This test aims to evaluate the structural integrity of shampoo bars in a humid environment, specifically measuring the sludge value (i.e., the quality of the softened, sticky substance formed on the surface) under immersion conditions and the natural wear rate during washing. This indicator is directly related to the product's lifespan and physical condition during storage.

[0136] The test subjects were the finished products prepared in Examples 1-3, as well as the finished products of Comparative Example 1 (traditional soap base), Comparative Example 3 (non-low temperature stepwise process), and Comparative Example 5 (stearic acid replacing mango kernel wax).

[0137] The specific operating steps are as follows: Sample preparation: Cut and polish each group of samples into standard cuboids with a mass of approximately 30g, equilibrate them in an environment of 25℃ and 50%RH for 24 hours, and accurately weigh the initial mass W0.

[0138] Immersion treatment: Fix the sample on a stainless steel mesh frame and immerse it in deionized water at 25°C, with the immersion depth being 1 / 2 of the sample height. Let it stand and soak for 2 hours.

[0139] Collection of mushy material: Remove the sample and drain the surface free water for 1 minute. Use pre-weighed (W) material. b The scraper is used to scrape away all the softened, sticky layer (i.e., the mushy layer) on the surface of the sample after it has been submerged in water with constant force until the hard core is exposed.

[0140] Quality determination: Immediately weigh the scraper containing the mushy material (W). c Calculate the mass M of the mushy paste. mush =W c -W b。 After scraping off the rotten paste, place the remaining soap block in a ventilated area to dry for 24 hours, and weigh the remaining dried mass W. f .

[0141] Index Calculation: Paste Value (g): i.e., M mush The smaller the value, the stronger the resistance to hydrolysis and softening.

[0142] Wear rate (%): (W0-W f W0 100% reflects the matrix loss after a single deep immersion.

[0143] Experimental data: Table 7. Data on resistance to rotting and wear rate of each group of samples. Group <![CDATA[Initial mass (g) W0 (g)]]> <![CDATA[Paste quality (g) M mush (g)]]> <![CDATA[Residual dry mass (g) W f (g)]]> Wear rate (%) Surface condition observation Example 1 30.125 2.15 27.55 8.55 The surface is moist, with no deep softening. Example 2 29.980 1.88 27.82 7.20 Dense structure, thin softening layer Example 3 30.054 2.32 27.28 9.23 The edges are intact and slightly sticky. Comparative Example 1 30.210 1.05 29.15 3.51 The surface is hard, with fine cracks appearing. Comparative Example 3 29.855 6.85 22.10 25.98 The whole thing is loose and falls off in a paste-like consistency. Comparative Example 5 30.092 3.45 25.88 13.99 The surface is rough and has flaking particles. Note: Comparative Example 1 (soap base) has high hardness and less mushy residue, but it is prone to cracking; Comparative Example 3 suffers from severe structural disintegration due to process issues.

[0144] Conclusion Analysis: Based on the combined experimental data and the physicochemical properties of the materials, the analysis is as follows: The samples in Examples 1-3, under prolonged immersion in water, exhibited a wear rate below 10% and a mushy residue value below 2.5g. This indicates that the mango kernel wax-modified oil-amino acid surfactant ternary system constructed in this invention possesses excellent water resistance and structural toughness. The mechanism is as follows: First, mango pit wax, as a high-melting-point plant wax, forms a continuous hydrophobic framework during the low-temperature pressing process. This framework effectively blocks the rapid diffusion of water into the soap body, preventing excessive swelling and loss of water-soluble amino acid surfactants.

[0145] Secondly, the modified oils are rich in diglycerides and monoglycerides, which have liquid crystal forming capabilities. During the soap curing process, these molecules fill the spaces between surfactant micelles and wax crystals, enhancing the interfacial bonding between components and preventing phase separation. In contrast, Comparative Example 3 used a high-temperature full-melting process, which destroyed the original crystalline morphology of the mango pit wax, resulting in a coarse phase-separated structure after cooling. Moisture easily penetrated along the grain boundaries, causing severe matrix disintegration, manifested as an extremely high sludge value (6.85 g) and a wear rate (25.98%).

[0146] Third, compared with Comparative Example 5 which used stearic acid, the abrasion rate of the embodiment was lower. Stearic acid crystals are hard and brittle, lack elasticity when swollen in water, and are prone to microscopic fracture and particle peeling. Mango pit wax, on the other hand, contains long-chain esters, which endow the soap with a certain degree of plasticity and cohesion, enabling it to resist moisture erosion without brittle peeling while maintaining its solid form.

[0147] Although Comparative Example 1 (conventional soap base) exhibited the lowest smear value due to the extremely high lattice energy of sodium fatty acid salts, the accompanying surface cracks indicated excessive internal stress in the material. The embodiments of the present invention, while ensuring sufficient durability, avoid cracking problems, achieving a balance between physical stability and user experience.

Claims

1. An amino acid complexed vegetable fat shampoo bar, characterized by, Made from raw materials comprising the following weight percentages: Amino acid surfactants 25%-35%; Mango pit wax 5%-10%; Coconut oil 8%-12%; Modified wheat germ oil 5%-10%; Modified shea butter 5%-10%; Modified camellia seed oil 27%-35%; Vine tea essential oil 2%-6%; Polygonatum odoratum essential oil 1%-2%; Arborvitae leaf essential oil 0.5%-1.5%; Polygonum multiflorum essential oil 0.5%-1.5%.

2. The amino acid complexed vegetable fat shampoo bar according to claim 1, characterized in that, The amino acid surfactant is selected from one or a combination of several of sodium lauroyl glutamate, potassium cocoyl glycinate, and sodium cocoyl ethanesulfonate.

3. The amino acid complexed vegetable fat shampoo bar according to claim 1, wherein The modified wheat germ oil, the modified shea butter, and the modified camellia seed oil are each prepared by selecting corresponding vegetable oils as base oils and using a method including the following steps: The base oil is added to a reaction vessel and heated to 40-45°C. 15%-20% of the base oil mass of deionized water is added, and the mixture is stirred at 300-500 rpm to obtain an emulsion. The pH value is adjusted to 6.0-7.0 using a pH adjuster, and 0.1%-0.3% of the base oil mass of lipase is added. The mixture is stirred and reacted at a constant temperature of 40-45°C for 4-6 hours. After the reaction is completed, the temperature is increased, the mixture is centrifuged, the aqueous phase and precipitate are removed, the upper oil phase is collected and vacuum dried.

4. The amino acid complexed vegetable fat shampoo bar according to claim 3, wherein The process conditions for raising the temperature after the reaction are as follows: raise the temperature to 85-90℃ and maintain it for 15-20 minutes; the conditions for vacuum drying are a vacuum degree of -0.08MPa to -0.09MPa and a temperature of 55-65℃; the pH adjuster is selected from citric acid or sodium bicarbonate.

5. A process for the preparation of an amino acid complexed vegetable fat shampoo bar characterized in that, The amino acid compound plant oil shampoo bar according to any one of claims 1-4 comprises the following steps: S1. Weigh out the amino acid surfactant and mango kernel wax according to the formula, mix them, heat and stir; S2. Stop heating and wait for the material to cool to 20-25℃. Add coconut oil, modified wheat germ oil, modified shea butter and modified camellia seed oil to the mixture and stir to obtain soap base. S3. Add vine tea essential oil, Solomon's seal essential oil, arborvitae leaf essential oil and Polygonum multiflorum essential oil to the soap base, and continue stirring to obtain soap material; S4. The soap material is injected into the mold, mechanical pressure is applied to press and shape it, and then the mold is placed in a constant temperature drying oven for heat setting. S5. After removing the mold and cooling to room temperature, unmold the soap and place it in a cool, ventilated environment to mature.

6. A process for the preparation of an amino acid complexed vegetable fat shampoo bar according to claim 5, characterized in that, In step S1, the heating temperature is controlled at 48-52℃, the stirring speed is 60-100rpm, and the stirring time is 40-50 minutes.

7. A process for the preparation of an amino acid complexed vegetable fat shampoo bar according to claim 5, characterized in that, In step S2, the stirring speed is 100-150 rpm and the stirring time is 25-35 minutes.

8. A process for the preparation of an amino acid complexed vegetable fat shampoo bar as claimed in claim 5, wherein, In step S3, the stirring speed is 80-120 rpm and the stirring time is 25-35 minutes.

9. A process for the preparation of an amino acid complexed vegetable oil soap shampoo according to claim 5, characterized in that, In step S4, the applied mechanical pressure is 0.1-0.3 MPa, and the holding time is 10-20 seconds; the heat setting temperature is 45-50℃, and the time is 20-24 hours.

10. A process for the preparation of an amino acid complexed vegetable fat shampoo bar as claimed in claim 5, wherein, In the S5 step, the temperature of the curing environment is 20-25°C, the relative humidity is 40-50%, and the curing time is 14-20 days. In the S5 step, the temperature of the curing environment is 20-25°C, the relative humidity is 40-50%, and the curing time is 14-20 days.

Images