Amino acid cleansing cream and preparation method thereof
By precisely controlling the temperature and stirring process, the instability and roughness of amino acid cleansing products caused by temperature changes in preparation are solved, and the long-term stability of the product and delicate and soft appearance are achieved, improving production efficiency and product quality.
Patent Information
- Application Number
- CN202510969004.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-15
- Publication Date
- 2025-08-12
AI Technical Summary
Existing amino acid cleansing products are easily affected by temperature changes during the preparation process, resulting in particle or roughness. There are also problems such as dilution and water leakage on the nozzle of the tube, and the paste becomes thicker and thicker. It is difficult to keep the paste stable for a long time and have a delicate and soft appearance.
A specific temperature control method is adopted, including heating, cooling and insulation and stirring processes. The specific steps are: increase the temperature to 80℃~85℃, cool to crystallization temperature T2 and continuously stir until the paste is beaded, heat to T4 and heat to stir for 20~40 minutes, and then cool to discharge temperature T3. The temperature difference is controlled within the range of T2±5℃, use frame stirring slurry and adjust the speed and rate.
It improves the long-term stability and delicate appearance of amino acid cleansing cream, reduces production costs, improves product quality, has good foaming force, is easy to rinse, has stable clean content, and is easy to extrude at low temperature, solving the problem of unstable paste caused by temperature changes.
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Figure CN120458932A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of cosmetics, and in particular to an amino acid cleansing cream and a preparation method thereof. Background Art
[0002] Because amino acid cleansing products are rich in amino acid surfactants, they are extremely mild, have good affinity with the skin, are resistant to hard water, are easily biodegradable, have rich foam, and are stable and elastic. After use, the skin feels refreshed, natural, not tight, and smooth, and they are highly sought after by consumers.
[0003] The preparation process for amino acid cleansing products is often difficult to control and significantly affected by temperature fluctuations. Raw materials are prone to graininess or roughness after hot and cold cycling. Furthermore, each system presents formulation challenges. For example, potassium glycogenate systems can cause thinning and water seepage at the nozzle, sodium glycogenate systems can cause the paste to clump and become rough after prolonged storage, and sodium glutamate systems can be thick and difficult to spread. These are common issues for amino acid surfactant systems. Therefore, there is an urgent need to develop a method for preparing an amino acid cleansing cream that maintains long-term stability and a delicate, soft appearance. Summary of the Invention
[0004] The purpose of this application is to provide an amino acid cleansing cream and a preparation method thereof, so as to improve the long-term stability of the amino acid cleansing cream and make it delicate and soft in appearance. The specific technical solution is as follows:
[0005] The first aspect of the present application provides a method for preparing an amino acid cleansing cream, comprising:
[0006] (1) Take the amino acid cleansing cream raw materials and heat and stir them to a temperature T1; wherein T1 is 80°C to 85°C;
[0007] (2) Cool down and stir until the crystallization temperature T2, and then continue stirring until the paste is pearlescent, that is, the discharge temperature T3 is reached;
[0008] (3) The temperature is raised and stirred to T4, the mixture is kept at this temperature and stirred for 20 to 40 minutes, and the temperature is lowered and stirred to the discharge temperature T3 to obtain an amino acid cleansing cream; wherein, T2-5°C < T4 < T2+5°C, preferably, T2-3°C ≤ T4 ≤ T2+3°C.
[0009] In one embodiment of the present application, in step (1), the conditions for heating and stirring include: a rotation speed of 60-100 rpm and a heating rate of 1-3°C / min.
[0010] In one embodiment of the present application, in step (2), the cooling and stirring conditions include: a rotation speed of 30-60 rpm and a cooling rate of 1-3°C / min.
[0011] In one embodiment of the present application, in step (3), the conditions for heating and stirring include: a rotation speed of 15~30 rpm and a heating rate of 1~3°C / min; the conditions for cooling and stirring include: a rotation speed of 15~30 rpm and a cooling rate of 1~3°C / min.
[0012] In one embodiment of the present application, the amino acid cleansing cream raw materials include amino acid surfactants and polyols; the amino acid surfactant is selected from at least one of potassium cocoyl glycinate, sodium cocoyl glycinate and sodium lauroyl glutamate; the polyol is selected from at least one of glycerol, 1,2-propylene glycol, butylene glycol, polyethylene glycol and sorbitol; preferably, based on the mass of the amino acid cleansing cream raw materials, the mass percentage of the amino acid surfactant is A, 30%≤A≤35%; the mass percentage of the polyol is B, 30%≤B≤35%.
[0013] In one embodiment of the present application, when the amino acid surfactant is selected from potassium cocoyl glycinate or sodium cocoyl glycinate, the amino acid cleansing cream raw material further includes an acid-base regulator; the acid-base regulator is selected from citric acid.
[0014] In one embodiment of the present application, based on the mass of the amino acid cleansing cream raw material, the mass percentage of the acid-base regulator is C, 4%≤C≤5%.
[0015] In one embodiment of the present application, when the amino acid surfactant is selected from sodium lauroyl glutamate, the amino acid cleansing cream raw material further includes a thickening stabilizer; the thickening stabilizer is selected from at least one of sodium chloride and PEG-150 stearate.
[0016] In one embodiment of the present application, based on the mass of the amino acid cleansing cream raw material, the mass percentage of the thickening stabilizer is D, 4%≤D≤8%.
[0017] The second aspect of the present application provides an amino acid cleansing cream prepared by the preparation method described in the first aspect of the present application.
[0018] Beneficial effects of this application:
[0019] The present application provides an amino acid cleansing cream and a preparation method thereof. The preparation process of the present application is simple and easy to implement, which reduces production costs while improving product quality. The paste formation point is stable during production, the difference in raw material batches has little effect on the paste, the tolerance is good, and it has the advantages of easy filling and loading, stable net content, and easy extrusion at low temperatures. The amino acid cleansing cream prepared by the present application is weakly acidic and has good foaming power. It is easy to foam and rinse when used, and the foam is relatively rich. The skin is refreshed and not tight after washing, and the paste is in a beautiful pearly state after crystallization; it improves the phenomenon of becoming coarse or having particles that are difficult to apply due to temperature changes.
[0020] Of course, it is not necessary to achieve all the advantages described above at the same time when implementing any product or method of the present application. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other embodiments can also be obtained based on these drawings.
[0022] Figure 1 This is a temperature-time curve diagram for the preparation of amino acid cleansing cream;
[0023] Figure 2 X-ray diffraction spectra (Cu target, Kα) of the amino acid cleansing creams prepared in Example 1 and Example 2 and Comparative Example 1 and Comparative Example 2;
[0024] Figure 3 Small-angle X-ray scattering spectra (Cu target, Kα) of the amino acid cleansing creams prepared in Example 1 and Example 2 and Comparative Example 1 and Comparative Example 2;
[0025] Figure 4 This is a polarizing microscope image of the amino acid cleansing cream prepared in Comparative Example 1;
[0026] Figure 5 This is a polarizing microscope image of the amino acid cleansing cream prepared in Example 1;
[0027] Figure 6 This is a polarizing microscope image of the amino acid cleansing cream prepared in Comparative Example 3;
[0028] Figure 7 This is a polarizing microscope image of the amino acid cleansing cream prepared in Comparative Example 4;
[0029] Figure 8 This is a polarizing microscope image of the amino acid cleansing cream prepared in Comparative Example 2;
[0030] Figure 9 This is a polarizing microscope image of the amino acid cleansing cream prepared in Example 2;
[0031] Figure 10 This is a polarizing microscope image of the amino acid cleansing cream prepared in Comparative Example 5;
[0032] Figure 11 This is a polarizing microscope image of the amino acid cleansing cream prepared in Comparative Example 6;
[0033] Figure 12 The differential scanning calorimetry (DSC) exothermic test curves of the amino acid cleansing creams prepared in Example 1 and Comparative Example 1 are shown;
[0034] Figure 13 The DSC exothermic test curves of the amino acid cleansing creams prepared in Example 2 and Comparative Example 2 are shown;
[0035] Figure 14 The softness and hardness test chart of the amino acid cleansing cream prepared in Comparative Example 1, Example 1, Comparative Example 3 and Comparative Example 4;
[0036] Figure 15 This is a test chart of the softness and hardness of the amino acid cleansing creams prepared in Comparative Example 2, Example 2, Comparative Example 5 and Comparative Example 6. DETAILED DESCRIPTION
[0037] The following will be combined with the embodiments of the present application and the accompanying drawings to clearly and completely describe the technical solutions in this application. Obviously, the embodiments described are only part of the embodiments of the present application, rather than all the embodiments. All other embodiments obtained by those skilled in the art based on this application are within the scope of protection of this application.
[0038] The present application provides a method for preparing an amino acid cleansing cream, which comprises:
[0039] (1) The amino acid cleansing cream raw materials are heated and stirred to a temperature T1; wherein T1 is 80°C to 85°C; for example, the amino acid cleansing cream raw materials are heated and stirred to a temperature of 80°C, 81°C, 82°C, 83°C, 84°C, 85°C or a range consisting of any two of these values;
[0040] (2) Cool down and stir until the crystallization temperature T2, and then continue stirring until the paste is pearlescent, that is, the discharge temperature T3 is reached;
[0041] (3) Then heating and stirring to temperature T4, keeping the temperature warm and stirring for 20 to 40 minutes, then cooling and stirring to the discharge temperature T3, to obtain an amino acid cleansing cream; wherein, T2-5°C < T4 < T2+5°C, preferably, T2-3°C ≤ T4 ≤ T2+3°C. For example, heating and stirring to temperature T2-4.5°C, T2-4°C, T2-3°C, T2-2°C, T2-1°C, T2+1°C, T2+2°C, T2+3°C, T2+4°C, T2+4.5°C or a range consisting of any two of these values, keeping the temperature warm and stirring for 20 minutes, 30 minutes, 40 minutes or a range consisting of any two of these values, then cooling and stirring to the discharge temperature T3, to obtain an amino acid cleansing cream.
[0042] In one embodiment of the present application, step (1) "taking the amino acid cleansing cream raw materials, heating and stirring to temperature T1" may also include "adjusting the pH to 5-7". For example, in one embodiment of the present application, the preparation temperature-time curve of the amino acid cleansing cream is as follows: Figure 1 As shown, it includes: after adding the raw materials, heating and stirring to temperature T1 to dissolve and deaerate, and adjusting the pH; after dissolving evenly, cooling and stirring until the paste becomes white and viscous, that is, reaching the crystallization temperature T2, and then continuing to stir until the paste is pearlescent, that is, reaching the discharge temperature T3; starting the aging process, that is, heating and stirring to temperature T4 again, keeping warm and stirring for a period of time; then cooling and stirring to the discharge temperature T3, and finally completing the discharge. It should be noted that if the pH of the amino acid cleansing cream raw materials is heated and stirred to temperature T1 to dissolve and deaerate, and is between 5 and 7, there is no need to adjust the pH. In this application, there is no special limitation on the method of adjusting the pH, as long as it can achieve the purpose of this application.
[0043] In the present application, the crystallization temperature refers to the temperature at which a substance changes from liquid to solid. For different amino acid cleansing cream raw materials, the corresponding crystallization temperature is also different.
[0044] In this application, the pearlescent paste refers to a paste that is fine, has a uniform and beautiful pearlescent luster, and has a pearl-like luster.
[0045] In the present application, the discharge temperature T3 is 38°C to 39°C. For example, the discharge temperature T3 can be 38°C, 38.5°C, 39°C, or a range consisting of any two values therein.
[0046] In this application, the initial temperature of the amino acid cleansing cream raw materials is not particularly limited. For example, the initial temperature of the amino acid cleansing cream raw materials can be room temperature. The specific operation method of heating and stirring is not particularly limited. For example, it can be performed in a water bath. The specific operation method of cooling and stirring is not particularly limited. For example, stirring and cooling can be performed at room temperature. In this application, room temperature refers to 20-30°C.
[0047] In the present application, there is no particular limitation on the stirring method, as long as the purpose of the present application can be achieved. For example, a frame-type stirring paddle can be used, which has a larger and wider stirring range and makes it easier for the paste to have a uniform pearlescent effect.
[0048] In the present application, the "heating and stirring again to temperature T4, keeping warm and stirring for 20 to 40 minutes" is a aging process. In the study, it was found that when the temperature was raised and stirred to temperature T4, the melting point of the paste increased and the melting area increased at temperature T4, thereby having a certain thermal stability, and having a crystal form with uniform and orderly shape and size, and the number increased significantly. Keep warm and stir for another 20 to 40 minutes, and keep stirring and shearing continuously when the crystals inside the cleansing cream precipitate and initially form crystal nuclei. This can prevent the disordered and uneven crystal precipitation due to temperature changes and the excessive crystallization of the paste, and prevent the change in the amount (or structure) of internal crystals from causing changes in hardness. The aging process of the present application can provide a greater degree of space for crystal growth.
[0049] Furthermore, T4 is within the range of this application, i.e., T2-5°C < T4 < T2+5°C, preferably, T2-3°C ≤ T4 ≤ T2+3°C, to maintain effective and uniform shearing of the paste. When T4 is below the range of this application, the paste may be too hard; when T4 is above the range of this application, the paste may be soft and have a weak pearlescent effect.
[0050] In one embodiment of the present application, in step (1), the stirring device is selected from a frame stirring paddle; the conditions for the heating and stirring include: a rotation speed of 60 to 100 rpm, and a heating rate of 1 to 3°C / min. For example, the rotation speed can be 60 rpm, 70 rpm, 80 rpm, 90 rpm, 100 rpm, or a range consisting of any two of these values, and the heating rate can be 1°C / min, 1.5°C / min, 2°C / min, 2.5°C / min, 3°C / min, or a range consisting of any two of these values. In one embodiment of the present application, in step (1), the initial rotation speed of the heating and stirring is 60 to 70 rpm, and the rotation speed is increased to 80 to 100 rpm after the amino acid cleansing cream raw materials are completely mixed. The use of the heating and stirring conditions of the present application is conducive to faster dispersion and dissolution of the amino acid cleansing cream raw materials, thereby improving efficiency.
[0051] In one embodiment of the present application, in step (2), the stirring device is selected from a frame stirring paddle; the cooling stirring conditions include: a rotation speed of 30 to 60 rpm, and a cooling rate of 1 to 3°C / min. For example, the rotation speed can be 30 rpm, 40 rpm, 50 rpm, 60 rpm, or a range consisting of any two of these values, and the cooling rate can be 1°C / min, 1.5°C / min, 2°C / min, 2.5°C / min, 3°C / min, or a range consisting of any two of these values. In one embodiment of the present application, in step (2), the initial rotation speed of the cooling stirring is 50 to 60 rpm, and after reaching the crystallization temperature, the rotation speed is reduced to 30 to 40 rpm. When the crystals in the cleansing cream are initially precipitated to form crystal nuclei, the stirring is maintained to continuously shear. By adopting the cooling stirring conditions of the present application, it is possible to prevent the disordered and uneven crystal precipitation and excessive crystallization of the paste due to rapid temperature changes, and at the same time prevent changes in the amount (or structure) of internal crystals from causing changes in hardness.
[0052] In one embodiment of the present application, in step (3), the stirring device is selected from a frame stirring paddle; the conditions for the heating stirring include: a rotation speed of 15 to 30 rpm, a heating rate of 1 to 3°C / min; the conditions for the cooling stirring include: a rotation speed of 15 to 30 rpm, a cooling rate of 1 to 3°C / min. For example, the heating stirring conditions include: a rotation speed of 15 rpm, 20 rpm, 25 rpm, 30 rpm or a range consisting of any two values therein, a heating rate of 1°C / min, 1.5°C / min, 2°C / min, 2.5°C / min, 3°C / min or a range consisting of any two values therein; the cooling stirring conditions include: a rotation speed of 15 rpm, 20 rpm, 25 rpm, 30 rpm or a range consisting of any two values therein, a cooling rate of 1°C / min, 1.5°C / min, 2°C / min, 2.5°C / min, 3°C / min or a range consisting of any two values therein. The use of the heating and cooling stirring conditions of the present application can prevent the disordered and uneven crystal precipitation and excessive crystallization of the paste due to temperature changes, and at the same time prevent the change in the internal crystal amount (or structure) that causes the hardness to change.
[0053] In one embodiment of the present application, the amino acid cleansing cream raw materials include an amino acid surfactant and a polyol; the amino acid surfactant is selected from at least one of potassium cocoyl glycinate, sodium cocoyl glycinate, and sodium lauroyl glutamate; the polyol is selected from at least one of glycerin, 1,2-propylene glycol, butylene glycol, polyethylene glycol, and sorbitol; preferably, based on the mass of the amino acid cleansing cream raw materials, the mass percentage of the amino acid surfactant is A, 30%≤A≤35%; the mass percentage of the polyol is B, 30%≤B≤35%. For example, based on the mass of the amino acid cleansing cream raw materials, the mass percentage of the amino acid surfactant A can be 30%, 33%, 35%, or a range consisting of any two of these values; the mass percentage of the polyol B can be 30%, 33%, 35%, or a range consisting of any two of these values. Using the amino acid surfactant and polyol described in this application and limiting their mass percentages to the above ranges can enhance the stability of the system and achieve a white paste with an attractive appearance.
[0054] In one embodiment of the present application, when the amino acid surfactant is selected from potassium cocoyl glycinate or sodium cocoyl glycinate, the amino acid cleansing cream raw materials further include an acid-base regulator; the acid-base regulator is selected from citric acid.
[0055] In one embodiment of the present application, based on the mass of the amino acid cleansing cream raw material, the mass percentage content of the acid-base regulator is C, and 4%≤C≤5%. For example, based on the mass of the amino acid cleansing cream raw material, the mass percentage content C of the acid-base regulator can be 4%, 4.5%, 5%, or a range consisting of any two of these values.
[0056] In one embodiment of the present application, when the amino acid surfactant is selected from sodium lauroyl glutamate, the amino acid cleansing cream raw material further includes a thickening stabilizer; the thickening stabilizer is selected from at least one of sodium chloride and PEG-150 stearate.
[0057] In one embodiment of the present application, the mass percentage of the thickening and stabilizing agent, based on the mass of the amino acid cleansing cream raw material, is D, and 4%≤D≤8%. For example, based on the mass of the amino acid cleansing cream raw material, the mass percentage D of the thickening and stabilizing agent can be 4%, 5%, 6%, 7%, 8%, or a range consisting of any two of these values.
[0058] By using the acid-base regulator and thickening stabilizer described in this application and limiting the mass percentage content within the scope of this application, the system can have excellent high-temperature stability.
[0059] In the present application, the amino acid cleansing cream raw material includes a solvent, and the solvent is selected from deionized water. Based on the mass of the amino acid cleansing cream raw material, the mass percentage content of the solvent is E, and 22%≤E≤36%. For example, based on the mass of the amino acid cleansing cream raw material, the mass percentage content of the solvent E can be 22%, 24%, 26%, 28%, 30%, 32%, 34%, 36%, or a range consisting of any two of these values.
[0060] The second aspect of the present application provides an amino acid cleansing cream prepared by the preparation method described in the first aspect of the present application.
[0061] The amino acid cleansing cream of the present application is weakly acidic and has good foaming power. It is easy to foam and rinse when used, and the foam is relatively rich. The skin is refreshed and not tight after washing. After crystallization, the cream has a beautiful pearlescent luster. It also has the advantages of easy filling and loading, stable net content, and easy extrusion at low temperatures.
[0062] Test methods and equipment:
[0063] Amino acid cleansing cream hardness test
[0064] At 25°C, a 3.25 g cone was released by free fall from a cone penetration tester (Shanghai Yidian Physical Optical Instrument Co., Ltd., model WSR), and the depth of the cone penetrating into the amino acid cleansing cream was measured 5 seconds after release (unit: 1 / 10 mm).
[0065] Example
[0066] The following examples and comparative examples are provided to further illustrate the embodiments of the present application. Various tests and evaluations were performed according to the following methods. In addition, unless otherwise specified, "parts" and "%" are by mass, and "room temperature" refers to 20-30°C.
[0067] Example 1
[0068] Potassium cocoyl glycinate, 1,2-propylene glycol, citric acid and deionized water are mixed to obtain an amino acid cleansing cream raw material. Based on the mass of the amino acid cleansing cream raw material, the mass percentage of potassium cocoyl glycinate is 30%, the mass percentage of 1,2-propylene glycol is 32%, the mass percentage of citric acid is 4.5%, and the mass percentage of deionized water is 33.5%; the amino acid cleansing cream raw material is added to a 25°C water bath, and a frame-type stirring paddle is used to stir at a speed of 60 rpm and a rate of 2.5°C / min. After the amino acid cleansing cream raw material is completely mixed, the speed is increased to 90 rpm, and the heating and stirring are continuously increased to 85°C for dissolution and degassing, at which time the pH is 6.3;
[0069] At room temperature, cool and stir at a speed of 60 rpm and a rate of 1.5°C / min until the paste becomes white and viscous. Take a thermometer and tilt it 0.5-1 cm below the liquid surface for measurement (the thermometer is lifted up and attached to the surface vertically downward without linear flow). The crystallization temperature is 47°C. Then continue stirring at a speed of 30 rpm until the paste becomes pearlescent, which is the discharge temperature, which is 38°C.
[0070] Then, the mixture was heated to 49°C at a speed of 30 rpm and a rate of 1.5°C / min, stirred at this temperature for 30 minutes, and then cooled to 38°C at a speed of 30 rpm and a rate of 1.5°C / min at room temperature to obtain the amino acid cleansing cream. Figure 2 As shown, the X-ray small angle scattering spectrum is as follows Figure 3 As shown in the polarizing microscope image Figure 5 As shown, the DSC exothermic test curve is as follows Figure 12 As shown in the figure, the hardness test is as follows Figure 14 shown.
[0071] Example 2
[0072] Sodium lauroyl glutamate, 1,2-propylene glycol, sodium chloride, PEG-150 stearate and deionized water are mixed to obtain an amino acid cleansing cream raw material. Based on the mass of the amino acid cleansing cream raw material, the mass percentage of sodium lauroyl glutamate is 30%, the mass percentage of 1,2-propylene glycol is 32%, the mass percentage of sodium chloride is 4%, the mass percentage of PEG-150 stearate is 4%, and the mass percentage of deionized water is 30%; the amino acid cleansing cream raw material is added to a 25°C water bath, and a frame-type stirring paddle is used to stir at a speed of 60 rpm and a rate of 2.5°C / min. After the amino acid cleansing cream raw material is completely mixed, the speed is increased to 90 rpm, and the temperature is continuously raised to 85°C for dissolution and degassing. At this time, the pH is 5.8;
[0073] At room temperature, cool and stir at a speed of 60 rpm and a rate of 1.5°C / min until the paste becomes white and viscous. Take a thermometer and tilt it 0.5-1 cm below the liquid surface for measurement (the thermometer is lifted up and attached to the surface vertically downward without linear flow). The crystallization temperature is 51°C. Then continue stirring at a speed of 30 rpm until the paste becomes pearlescent, which is the discharge temperature, which is 38°C.
[0074] Then, the mixture was heated to 54°C at a speed of 30 rpm and a rate of 1.5°C / min, stirred at this temperature for 30 minutes, and then cooled to 38°C at a speed of 30 rpm and a rate of 1.5°C / min at room temperature to obtain the amino acid cleansing cream. Figure 2As shown, the X-ray small angle scattering spectrum is as follows Figure 3 As shown in the polarizing microscope image Figure 9 As shown, the DSC exothermic test curve is as follows Figure 13 As shown in the figure, the hardness test is as follows Figure 15 shown.
[0075] Comparative Example 1
[0076] Potassium cocoyl glycinate, 1,2-propylene glycol, citric acid and deionized water are mixed to obtain an amino acid cleansing cream raw material. Based on the mass of the amino acid cleansing cream raw material, the mass percentage of potassium cocoyl glycinate is 30%, the mass percentage of 1,2-propylene glycol is 32%, the mass percentage of citric acid is 4.5%, and the mass percentage of deionized water is 33.5%; the raw materials of the amino acid cleansing cream are added to a 25°C water bath, and a frame-type stirring paddle is used to stir at a speed of 60 rpm and a rate of 2.5°C / min. After the amino acid cleansing cream raw materials are completely mixed, the speed is increased to 90 rpm, and the temperature is continuously raised and stirred to 85°C for dissolution and degassing, at which time the pH is 6.3;
[0077] Under room temperature, the mixture was stirred at a speed of 60 rpm and a rate of 1.5°C / min until the paste became white and viscous. A thermometer was tilted 0.5 to 1 cm below the liquid surface for measurement (the thermometer was lifted up and attached to the surface vertically downward without linear flow). The crystallization temperature was measured to be 47°C. The mixture was then stirred at a speed of 30 rpm until the paste became pearlescent, reaching the discharge temperature of 38°C. The amino acid cleansing cream was obtained. Its X-ray diffraction spectrum is shown below. Figure 2 As shown, the X-ray small angle scattering spectrum is as follows Figure 3 As shown in the polarizing microscope image Figure 4 As shown, the DSC exothermic test curve is as follows Figure 12 As shown in the figure, the hardness test is as follows Figure 14 shown.
[0078] Comparative Example 2
[0079] Sodium lauroyl glutamate, 1,2-propylene glycol, sodium chloride, PEG-150 stearate and deionized water are mixed to obtain an amino acid cleansing cream raw material. Based on the mass of the amino acid cleansing cream raw material, the mass percentage of sodium lauroyl glutamate is 30%, the mass percentage of 1,2-propylene glycol is 32%, the mass percentage of sodium chloride is 4%, the mass percentage of PEG-150 stearate is 4%, and the mass percentage of deionized water is 30%; the amino acid cleansing cream raw material is added to a 25°C water bath, and a frame-type stirring paddle is used to stir at a speed of 60 rpm and a rate of 2.5°C / min. After the amino acid cleansing cream raw material is completely mixed, the speed is increased to 90 rpm, and the temperature is continuously raised to 85°C for dissolution and degassing. At this time, the pH is 5.8;
[0080] Under room temperature, the mixture was stirred at a speed of 60 rpm and a rate of 1.5°C / min until the paste became white and viscous. A thermometer was tilted 0.5 to 1 cm below the liquid surface for measurement (the thermometer was lifted up and attached to the surface vertically downward without linear flow). The crystallization temperature was measured to be 51°C. The mixture was then stirred at a speed of 30 rpm until the paste became pearlescent, reaching the discharge temperature of 38°C. The amino acid cleansing cream was obtained. Its X-ray diffraction spectrum is shown below. Figure 2 As shown, the X-ray small angle scattering spectrum is as follows Figure 3 As shown in the polarizing microscope image Figure 8 As shown, the DSC exothermic test curve is as follows Figure 13 As shown in the figure, the hardness test is as follows Figure 15 shown.
[0081] Comparative Example 3
[0082] Potassium cocoyl glycinate, 1,2-propylene glycol, citric acid and deionized water are mixed to obtain an amino acid cleansing cream raw material. Based on the mass of the amino acid cleansing cream raw material, the mass percentage of potassium cocoyl glycinate is 30%, the mass percentage of 1,2-propylene glycol is 32%, the mass percentage of citric acid is 4.5%, and the mass percentage of deionized water is 33.5%; the amino acid cleansing cream raw material is added to a 25°C water bath, and a frame-type stirring paddle is used to stir at a speed of 60 rpm and a rate of 2.5°C / min. After the amino acid cleansing cream raw material is completely mixed, the speed is increased to 90 rpm, and the heating and stirring are continuously increased to 85°C for dissolution and degassing, at which time the pH is 6.3;
[0083] At room temperature, cool and stir at a speed of 60 rpm and a rate of 1.5°C / min until the paste becomes white and viscous. Take a thermometer and tilt it 0.5-1 cm below the liquid surface for measurement (the thermometer is lifted up and attached to the surface vertically downward without linear flow). The crystallization temperature is 47°C. Then continue stirring at a speed of 30 rpm until the paste becomes pearlescent, which is the discharge temperature, which is 38°C.
[0084] Then, the mixture was heated to 42°C at a speed of 30 rpm and a rate of 1.5°C / min, stirred at this temperature for 30 minutes, and then cooled to 38°C at a speed of 30 rpm and a rate of 1.5°C / min at room temperature to obtain the amino acid cleansing cream. Figure 6 As shown in the figure, the hardness test is as follows Figure 14 shown.
[0085] Comparative Example 4
[0086] Potassium cocoyl glycinate, 1,2-propylene glycol, citric acid and deionized water are mixed to obtain an amino acid cleansing cream raw material. Based on the mass of the amino acid cleansing cream raw material, the mass percentage of potassium cocoyl glycinate is 30%, the mass percentage of 1,2-propylene glycol is 32%, the mass percentage of citric acid is 4.5%, and the mass percentage of deionized water is 33.5%; the amino acid cleansing cream raw material is added to a 25°C water bath, and a frame-type stirring paddle is used to stir at a speed of 60 rpm and a rate of 2.5°C / min. After the amino acid cleansing cream raw material is completely mixed, the speed is increased to 90 rpm, and the heating and stirring are continuously increased to 85°C for dissolution and degassing, at which time the pH is 6.3;
[0087] At room temperature, cool and stir at a speed of 60 rpm and a rate of 1.5°C / min until the paste becomes white and viscous. Take a thermometer and tilt it 0.5-1 cm below the liquid surface for measurement (the thermometer is lifted up and attached to the surface vertically downward without linear flow). The crystallization temperature is 47°C. Then continue stirring at a speed of 30 rpm until the paste becomes pearlescent, which is the discharge temperature, which is 38°C.
[0088] Then, the mixture was heated to 52°C at a speed of 30 rpm and a rate of 1.5°C / min, stirred at this temperature for 30 minutes, and then cooled to 38°C at a speed of 30 rpm and a rate of 1.5°C / min at room temperature to obtain the amino acid cleansing cream. Figure 7 As shown in the figure, the hardness test is as follows Figure 14 shown.
[0089] Comparative Example 5
[0090] Sodium lauroyl glutamate, 1,2-propylene glycol, sodium chloride, PEG-150 stearate and deionized water are mixed to obtain an amino acid cleansing cream raw material. Based on the mass of the amino acid cleansing cream raw material, the mass percentage of sodium lauroyl glutamate is 30%, the mass percentage of 1,2-propylene glycol is 32%, the mass percentage of sodium chloride is 4%, the mass percentage of PEG-150 stearate is 4%, and the mass percentage of deionized water is 30%; the amino acid cleansing cream raw material is added to a 25°C water bath, and a frame-type stirring paddle is used to stir at a speed of 60 rpm and a rate of 2.5°C / min. After the amino acid cleansing cream raw material is completely mixed, the speed is increased to 90 rpm, and the temperature is continuously raised to 85°C for dissolution and degassing. At this time, the pH is 5.8;
[0091] At room temperature, cool and stir at a speed of 60 rpm and a rate of 1.5°C / min until the paste becomes white and viscous. Take a thermometer and tilt it 0.5-1 cm below the liquid surface for measurement (the thermometer is lifted up and attached to the surface vertically downward without linear flow). The crystallization temperature is 51°C. Then continue stirring at a speed of 30 rpm until the paste becomes pearlescent, which is the discharge temperature, which is 38°C.
[0092] Then, the mixture was heated to 46°C at a speed of 30 rpm and a rate of 1.5°C / min, stirred at this temperature for 30 minutes, and then cooled to 38°C at a speed of 30 rpm and a rate of 1.5°C / min at room temperature to obtain the amino acid cleansing cream. Figure 10 As shown in the figure, the hardness test is as follows Figure 15 shown.
[0093] Comparative Example 6
[0094] Sodium lauroyl glutamate, 1,2-propylene glycol, sodium chloride, PEG-150 stearate and deionized water are mixed to obtain an amino acid cleansing cream raw material. Based on the mass of the amino acid cleansing cream raw material, the mass percentage of sodium lauroyl glutamate is 30%, the mass percentage of 1,2-propylene glycol is 32%, the mass percentage of sodium chloride is 4%, the mass percentage of PEG-150 stearate is 4%, and the mass percentage of deionized water is 30%; the amino acid cleansing cream raw material is added to a 25°C water bath, and a frame-type stirring paddle is used to stir at a speed of 60 rpm and a rate of 2.5°C / min. After the amino acid cleansing cream raw material is completely mixed, the speed is increased to 90 rpm, and the temperature is continuously raised to 85°C for dissolution and degassing. At this time, the pH is 5.8;
[0095] At room temperature, cool and stir at a speed of 60 rpm and a rate of 1.5°C / min until the paste becomes white and viscous. Take a thermometer and tilt it 0.5-1 cm below the liquid surface for measurement (the thermometer is lifted up and attached to the surface vertically downward without linear flow). The crystallization temperature is 51°C. Then continue stirring at a speed of 30 rpm until the paste becomes pearlescent, which is the discharge temperature, which is 38°C.
[0096] Then, the mixture was heated to 56°C at a speed of 30 rpm and a rate of 1.5°C / min, stirred at this temperature for 30 minutes, and then cooled to 38°C at a speed of 30 rpm and a rate of 1.5°C / min at room temperature to obtain the amino acid cleansing cream. Figure 11 As shown in the figure, the hardness test is as follows Figure 15 shown.
[0097] Figure 2 The X-ray diffraction spectra of the amino acid cleansing creams prepared in Example 1 and Example 2 and Comparative Example 1 and Comparative Example 2 are shown in FIG. Figure 2 It can be seen that the amino acid cleansing creams prepared in Examples 1 and 2 and Comparative Examples 1 and 2 all exhibit scattering peaks of aggregate structures with different scattering intensities, which, combined with the half-peak width and area, can reflect the formation of micelle aggregates. Figure 3 The X-ray small angle scattering spectra of the amino acid cleansing cream prepared in Example 1 and Example 2 and Comparative Example 1 and Comparative Example 2 are shown in FIG. Figure 3 It can be seen that the scattering peak of the sodium lauroyl glutamate system after ripening has a higher scattering intensity and a narrower half-peak width, which indicates that the layered structure has a high degree of order. At the same time, a scattering peak appears at the other end of the potassium cocoyl glycinate system after ripening, which shows a more glossy and delicate paste macroscopically. Figure 4 、 Figure 5 、 Figure 6 and Figure 7 Polarized light microscope images of the amino acid cleansing creams prepared in Comparative Example 1, Example 1, Comparative Example 3 and Comparative Example 4, respectively. Figure 4 and Figure 5 It can be seen that compared with the comparative example 1 which did not undergo the aging process, the crystals of the potassium cocoyl glycinate system of Example 1 of the present application are easy to aggregate after aging, the stability is enhanced, the reflection is obvious under polarized light, and the appearance is brighter; Figure 5 、 Figure 6 and Figure 7 It can be seen that compared with Comparative Examples 3 and 4 in which T4 is outside the scope of this application, the potassium cocoyl glycinate system of Example 1 in which T4 is within the scope of this application has more crystals, enhanced stability, obvious reflection under polarized light, and a brighter appearance. Figure 8 、 Figure 9 、 Figure 10 and Figure 11 Polarized microscope images of the amino acid cleansing creams prepared in Comparative Example 2, Example 2, Comparative Example 5 and Comparative Example 6, respectively. Figure 8 and Figure 9 It can be seen that compared with the comparative example 2 which did not undergo the aging process, the agglomeration phenomenon of the sodium lauroyl glutamate system of Example 2 of the present application was weakened, the stability was enhanced, the matte finish was relatively matte, and the aging crystal nuclei were relatively coarse; Figure 9 、 Figure 10 and Figure 11 It can be seen that compared with Comparative Examples 5 and 6 where T4 is outside the scope of this application, the crystal nuclei precipitated from the sodium lauroyl glutamate system of Example 2 where T4 is within the scope of this application become coarser, the number of crystals increases, the aggregation is weakened, and the crystals are more evenly dispersed. Figure 12 The DSC exothermic test curves of the amino acid cleansing cream prepared in Example 1 and Comparative Example 1 are shown. Figure 13 The DSC exothermic test curves of the amino acid cleansing cream prepared in Example 2 and Comparative Example 2 are shown. Figure 12 and Figure 13 It can be seen that the melting peak melting point (T m ) increases and the melting enthalpy (ΔH f ) increases, which shows that the hardness of the cream has been significantly improved macroscopically, and to a certain extent, the thermal stability of the cleansing cream has been improved and the number of crystals has increased. Figure 14 The hardness test chart of the amino acid cleansing cream prepared in Comparative Example 1, Example 1, Comparative Example 3 and Comparative Example 4 shows that the amino acid cleansing cream of the potassium cocoyl glycinate system in Example 1 of the present application has moderate hardness and a finer paste; when T4 is lower than the range of the present application (for example, Comparative Example 3), the paste is relatively hard and prone to granularity; when T4 is higher than the range of the present application (for example, Comparative Example 4), the paste is relatively soft and tends to become thinner, and water seepage occurs. Figure 15 The hardness test diagrams of the amino acid cleansing creams prepared in Comparative Example 2, Example 2, Comparative Example 5 and Comparative Example 6 show that the amino acid cleansing cream of the sodium lauroyl glutamate system of Example 2 of the present application has moderate hardness; when T4 is lower than the range of the present application (for example, Comparative Example 5), the crystals are excessively cross-aggregated, resulting in the paste being too hard; when T4 is higher than the range of the present application (for example, Comparative Example 6), the crystals are small, resulting in the paste becoming soft and unstable.
[0098] In summary, the amino acid cleansing cream prepared by the present application is weakly acidic, has good foaming power, is easy to foam and rinse when used, has rich foam, and the skin is refreshed and not tight after washing. After crystallization, the paste is in a beautiful pearlescent state; it improves the phenomenon of coarsening or granularity that is difficult to apply with temperature changes. Furthermore, the preparation process of the present application is simple and easy to implement, which reduces production costs while improving product quality. The paste point is stable during production, the difference in raw material batches has little effect on the paste, and the tolerance is good. It also has the advantages of easy filling and loading, stable net content, and easy extrusion at low temperatures.
[0099] The above description is only a preferred embodiment of the present application and is not intended to limit the present application. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present application shall be included in the scope of protection of the present application.
Claims
1. A method for preparing an amino acid cleansing cream, comprising: (1) Take the amino acid cleansing cream raw materials and heat and stir them to a temperature T1; wherein T1 is 80°C to 85°C; (2) Cool down and stir until the crystallization temperature T2, and then continue stirring until the paste is pearlescent, that is, the discharge temperature T3 is reached; (3) The temperature is raised and stirred to T4, the mixture is kept at this temperature and stirred for 20 to 40 minutes, and the temperature is lowered and stirred to the discharge temperature T3 to obtain an amino acid cleansing cream; wherein, T2-5°C < T4 < T2+5°C.
2. The preparation method according to claim 1, wherein T2-3℃≤T4≤T2+3℃.
3. The preparation method according to claim 1, wherein In step (1), the heating and stirring conditions include: a rotation speed of 60-100 rpm and a heating rate of 1-3°C / min.
4. The preparation method according to claim 1, wherein In step (2), the cooling and stirring conditions include: a rotation speed of 30-60 rpm and a cooling rate of 1-3°C / min.
5. The preparation method according to claim 1, wherein In step (3), the conditions for heating and stirring include: a rotation speed of 15~30 rpm and a heating rate of 1~3°C / min; the conditions for cooling and stirring include: a rotation speed of 15~30 rpm and a cooling rate of 1~3°C / min.
6. The preparation method according to claim 1, wherein The amino acid cleansing cream comprises amino acid surfactants and polyols; the amino acid surfactant is selected from at least one of potassium cocoyl glycinate, sodium cocoyl glycinate and sodium lauroyl glutamate; and the polyol is selected from at least one of glycerin, 1,2-propylene glycol, butylene glycol, polyethylene glycol and sorbitol.
7. The preparation method according to claim 6, wherein Based on the mass of the amino acid cleansing cream raw material, the mass percentage of the amino acid surfactant is A, 30%≤A≤35%; the mass percentage of the polyol is B, 30%≤B≤35%.
8. The preparation method according to any one of claims 6 to 7, wherein When the amino acid surfactant is selected from potassium cocoyl glycinate or sodium cocoyl glycinate, the amino acid cleansing cream raw materials further include an acid-base regulator; and the acid-base regulator is selected from citric acid.
9. The preparation method according to claim 8, wherein Based on the mass of the amino acid cleansing cream raw material, the mass percentage of the acid-base regulator is C, 4%≤C≤5%.
10. The preparation method according to any one of claims 6 to 7, wherein When the amino acid surfactant is selected from sodium lauroyl glutamate, the amino acid cleansing cream raw material further includes a thickening stabilizer; the thickening stabilizer is selected from at least one of sodium chloride and PEG-150 stearate.
11. The preparation method according to claim 10, wherein Based on the mass of the amino acid cleansing cream raw material, the mass percentage of the thickening stabilizer is D, 4%≤D≤8%.
12. An amino acid cleansing cream prepared according to the preparation method according to any one of claims 1 to 11.
Citation Information
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