Carboxylic acid polymer supramolecular emulsifier as well as preparation method and application thereof
By preparing a carboxylic acid polymer supramolecular emulsifier, the problems of reaction complexity and stability of existing emulsifiers have been solved, achieving efficient and low-cost emulsification effects, which are suitable for cosmetics and pharmaceuticals.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- UZIKANG BIOTECHNOLOGY (WUXI) CO LTD
- Filing Date
- 2026-02-04
- Publication Date
- 2026-05-05
AI Technical Summary
Existing carboxylic acid polymer emulsifiers suffer from problems such as harsh reaction conditions, complex reactions, high costs, low emulsification efficiency, large addition amounts, and poor emulsion stability, making it difficult to meet the needs of demanding application scenarios.
A carboxylic acid polymer supramolecular emulsifier was prepared by dispersing a carboxylic acid polymer and sodium fatty acid in a solvent, adding fatty acids and alcohols, mixing thoroughly, and then drying. The particle size was controlled at 400-600 nm using spray drying technology, exhibiting excellent EAI and ESI indices, and forming a dynamically reversible supramolecular structure.
The prepared carboxylic acid polymer supramolecular emulsifier has high emulsification efficiency and low addition amount. The emulsion exhibits excellent stability under high temperature and high humidity environments and freeze-thaw cycles, making it suitable for cosmetic and pharmaceutical preparation. It also possesses good moisturizing properties and cell compatibility.
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Figure CN121975136A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to a carboxylic acid polymer supramolecular emulsifier, its preparation method, and its application, belonging to the field of supramolecular emulsifier preparation technology. Background Technology
[0002] Emulsifiers, as a class of key additives that can stabilize the oil-water interface and reduce surface tension, are widely used in cosmetics, food processing, polymer polymerization, pharmaceutical processing and other fields. Their performance directly determines the stability, safety and application effect of the end product.
[0003] Currently, commonly used emulsifiers mainly fall into two categories: small molecule surfactants and traditional polymer emulsifiers. Small molecule surfactants, such as fatty alcohol polyoxyethylene ethers, alkylbenzene sulfonates, and Span series, while possessing advantages such as simple synthesis processes and low cost, have inherent structural defects: First, the binding force between hydrophilic and lipophilic groups is weak, making them prone to detachment from the interface in low-polarity or non-polar media, leading to emulsion particle aggregation, demulsification, and poor stability; second, the carbon chain length of the lipophilic groups is limited (mostly C18 and below derivatives), failing to form a sufficient steric barrier, resulting in insufficient steric stabilization and difficulty in meeting the demands of complex working conditions. Furthermore, in the cosmetics field, the large amount of small molecule emulsifiers added can easily cause skin irritation, contradicting the trend towards gentle formulations.
[0004] To overcome the shortcomings of small molecule emulsifiers, polymer emulsifiers have been gradually put into use.
[0005] Carboxylic acid polymers, due to the large number of carboxyl groups in their molecular structure, can regulate hydrophilicity-hydrophobicity balance by adjusting pH and possess a certain degree of biocompatibility, making them a key research focus. Existing polycarboxylic acid emulsifiers are mostly prepared by copolymerizing acrylic acid and acrylate monomers, adjusting the HLB value by controlling the monomer ratio, showing some application potential in emulsion polymerization and other scenarios. However, these traditional carboxylic acid polymer emulsifiers still have significant shortcomings: their molecular structures are linear or simple branched structures, lacking dynamically tunable interfacial interaction sites, and their emulsion stability is greatly affected by environmental factors (temperature, salinity, pH); furthermore, they lack supramolecular self-assembly properties, unable to form more stable interfacial film structures through intermolecular non-covalent interactions, requiring higher addition levels to maintain emulsion stability in demanding applications.
[0006] The development of supramolecular chemistry has provided a new path for emulsifier design. Supramolecular emulsifiers form dynamic and reversible supramolecular structures through the self-assembly of host and guest molecules, which can significantly improve emulsification efficiency, stability and functional diversity.
[0007] Currently, no carboxylic acid polymer supramolecular emulsifiers have been found.
[0008] Therefore, in order to solve the problems of harsh reaction conditions, complex reactions, and high costs in the preparation of existing carboxylic acid polymer emulsifiers, it is urgent to develop a carboxylic acid polymer supramolecular emulsifier that is simple to prepare, low in cost, has high emulsification efficiency, low addition amount, and excellent emulsion stability. Summary of the Invention
[0009] To address the aforementioned problems, this invention provides a carboxylic acid polymer supramolecular emulsifier, its preparation method, and its applications. Specifically, this invention first disperses a carboxylic acid polymer and sodium fatty acid in a solvent to obtain a dispersion; then, fatty acids and an alcohol are added to the dispersion and mixed thoroughly to obtain a suspension; finally, the suspension is dried to obtain the carboxylic acid polymer supramolecular emulsifier. The method for preparing the carboxylic acid polymer supramolecular emulsifier of this invention is simple and low-cost, and the prepared carboxylic acid polymer supramolecular emulsifier exhibits high emulsification efficiency, low addition amount, and excellent emulsion stability, showing broad application prospects in the fields of cosmetics and pharmaceutical preparation.
[0010] The first objective of this invention is to provide a method for preparing a carboxylic acid polymer supramolecular emulsifier, comprising the following steps: (1) Disperse the carboxylic acid polymer and sodium fatty acid in a solvent to obtain a dispersion; (2) Add fatty acids and alcohol to the dispersion, mix well, and obtain a suspension; (3) The suspension was dried to obtain a carboxylic acid polymer supramolecular emulsifier powder; The mass ratio of carboxylic acid polymer, sodium fatty acid, fatty acid, alcohol, and solvent is 1-30:8-25:0-10:35-91:450.
[0011] Optionally, in step (1), the carboxylic acid polymer is one or two of carbomer and sodium polyglutamate; the carbomer is one or more of carbomer 980 and carbomer U20.
[0012] Optionally, in step (1), the sodium fatty acid may be one or more of sodium stearate, sodium linoleate, sodium palmitate, sodium myristate, sodium oleate, sodium cocoate, sodium laurylate, sodium palmitate, and sodium isostearate.
[0013] Optionally, the solvent in step (1) is water or an aqueous solution of ethanol with a mass fraction of 40-60%.
[0014] Optionally, in step (1), the dispersion is carried out at 25-40℃ and 50-200rpm for 3-12h.
[0015] Optionally, the fatty acids in step (2) are one or more of the following: linolenic acid, stearic acid, linoleic acid, palmitic acid, myristic acid, tall oil acid, oleic acid, hydrogenated coconut acid, coconut oil acid, caprylic acid, capric acid, lauric acid, palmitic acid, stearic acid, isostearic acid, butyloctanoic acid, docosahexaenoic acid, eicosapentaenoic acid, and hexanoic acid.
[0016] Optionally, in step (2), the alcohol is one or more of the following: butyloctanol, decanol, decyltetradecylol, arachidonicol, hexyldecylol, cetyl alcohol, cetearyl alcohol, polydimethylsiloxane alcohol, myristol, octyldodecyl alcohol, lanosterol, lanolin alcohol, coconut oil alcohol, isocetyl alcohol, isostearyl alcohol, stearyl alcohol, oleyl alcohol, lauryl alcohol, and palm oil alcohol.
[0017] Optionally, in step (2), the mixture is stirred at 55-105℃ and 350-600rpm for 5-16 hours.
[0018] Optionally, the drying in step (3) is spray drying, with a temperature of 160-200℃, a pressure of 0.2-0.5MPa, and a time of 4-10h.
[0019] The second objective of this invention is to prepare a carboxylic acid polymer supramolecular emulsifier powder using the method described herein.
[0020] Optionally, the particle size range of the carboxylic acid polymer supramolecular emulsifier powder is 400-600 nm.
[0021] The third objective of this invention is to apply the carboxylic acid polymer supramolecular emulsifier powder described herein in the preparation of pharmaceuticals or cosmetics.
[0022] Optional cosmetics include ointments, creams, lotions, etc.; carboxylic acid polymer supramolecular emulsifier powder can enhance the moisturizing, stability, antibacterial and anti-inflammatory functions of cosmetics.
[0023] Optional medications include dressings, creams, etc.
[0024] A fourth objective of this invention is to provide a cosmetic product that utilizes the carboxylic acid polymer supramolecular emulsifier powder described in this invention.
[0025] Alternatively, the preparation method for cosmetics is as follows: Carboxylic acid polymer supramolecular emulsifier powder is added to the oil phase and mixed evenly, then added to the aqueous phase and homogenized and emulsified to obtain cosmetics; The carboxylic acid polymer supramolecular emulsifier powder has a mass concentration of 0.1-2% in the entire cosmetic product.
[0026] Optionally, preservatives and functional ingredients may be added to the cosmetic preparation process at appropriate times as needed.
[0027] Optional cosmetics include lotions, creams, and lotions; different aqueous and oil phases can be selected as needed.
[0028] The fifth objective of this invention is to provide a method for improving the storage stability and emulsification efficiency of emulsions, which employs the carboxylic acid polymer supramolecular emulsifier powder described in this invention.
[0029] The technical effects of this invention are as follows: (1) The method for preparing carboxylic acid polymer supramolecular emulsifiers of the present invention is simple and low in cost. The prepared carboxylic acid polymer supramolecular emulsifiers have high emulsification efficiency, low addition amount and excellent emulsion stability, and have broad application prospects in the fields of cosmetics and pharmaceutical preparation.
[0030] (2) The carboxylic acid polymer supramolecular emulsifier powder of the present invention has a particle size of 400-600 nm and an EAI index of 88 nm. 2 The emulsion has a concentration of 1 g or higher, an ESI index of 85% or higher, and a cell viability retention rate of 90% or higher. The prepared emulsion is homogeneous and stable without stratification after being placed in a high temperature and high humidity environment for 1 month. It is also homogeneous and stable without stratification after a freeze-thaw cycle for 1 month. Furthermore, the prepared cosmetic has excellent moisturizing properties and is homogeneous and stable without stratification after being placed in a high temperature and high humidity environment for 1 month. It is also homogeneous and stable without stratification after a freeze-thaw cycle for 1 month. Attached Figure Description
[0031] Figure 1 The infrared spectrum is shown for the carboxylic acid polymer supramolecular emulsifier powder prepared in Example 1.
[0032] Figure 2 Physical images of the emulsifiers used in Examples 1-3, 15 and Comparative Examples 1-4 during stability testing. Detailed Implementation
[0033] The preferred embodiments of the present invention are described below. It should be understood that the embodiments are for better explanation of the present invention and are not intended to limit the present invention.
[0034] Test method: 1. Emulsifying activity and stability (EAI / ESI index) test: Add the emulsifier powder to water to prepare an emulsifier aqueous solution with a mass concentration of 1%; weigh the emulsifier aqueous solution and liquid paraffin at a mass ratio of 1:4, vortex mix for 5 minutes to form an emulsion; take 0.1 mL of the emulsion and dilute it with distilled water to 10 mL (dilution factor N=100).
[0035] After standing for 10 min, using distilled water as a blank, measure the absorbance A0 at 500 nm. Substitute the absorbance into the formula to calculate EAI; EAI(m) 2 / g)={(2×2.303) / [C×(1-φ)×10 4 ]}×A 500 × dilution factor; where φ is 0.2; Transfer the emulsion to centrifuge tubes and let it stand for 4 hours. Take 0.1 mL of the upper layer of emulsion each time, dilute it, and measure the absorbance A. t ; Calculate ESI using the formula:
[0036] The emulsion was subjected to accelerated aging tests under two conditions: a high temperature and high humidity (40℃ / 75% RH) constant temperature and humidity chamber and a freeze-thaw cycle (alternating between -20℃ and 25℃, with one cycle completed every 24 hours). After one month, the emulsion was observed to determine whether it was uniform and stable and whether it separated into layers.
[0037] 2. Moisturizing performance test: Using a glass plate covered with 3M tape as a carrier, 0.20g of sample was evenly coated onto the tape surface. The mass of the glass plate with 3M tape and the mass of the sample after coating were accurately recorded. A relative humidity of 60% was created using a saturated potassium acetate solution. The samples were weighed and recorded after 1, 2, 3, 4, 6, and 24 hours in a desiccator. The moisture retention rate (η) was calculated using the formula:
[0038] Where: m t The values represent the mass after 1, 2, 3, 4, 6, and 24 hours of storage. m0 represents the mass of the glass plate with 3M tape applied after the sample is applied, and m represents the mass of the glass plate with 3M tape applied.
[0039] 3. Cell compatibility test: The MTT (3-(4,5-dimethylthiazolyl-2-yl)-2,5-diphenyltetrazolium bromide) method is a classic cell proliferation / toxicity assay that indirectly reflects cell number and viability by detecting the ability of mitochondrial dehydrogenases in living cells to reduce MTT to formazan.
[0040] Take fibroblasts in the logarithmic growth phase and adjust the density (1×10⁻⁶). 4 (cells / well, 96-well plate); add 100 μL of complete culture medium to each well and incubate for 24 h to allow the cells to adhere; Experimental Groups: Blank control group (culture medium only, no cells); Negative control group (untreated cells); Experimental group (0.5% emulsifier aqueous solution); Positive control group (10% FBS stimulation); Add 10 μL of MTT solution (5 mg / mL, prepared in PBS) to each well (final concentration 0.5 mg / mL); incubate at 37 °C for 4 h, then discard the supernatant; add 150 μL of DMSO to each well and shake slowly for 10 min to dissolve the crystals; measure the absorbance at 490 nm using a microplate reader.
[0041] The formula for calculating cell viability retention rate is as follows: Cell viability (%) = (OD value of experimental group - OD value of blank group) / (OD value of control group - OD value of blank group) × 100% Unless otherwise specified, the solvent used in the test method is water, and unless otherwise specified, the percentage refers to mass percentage.
[0042] Raw materials used in the examples: Carbomer 980: 99%; Sodium stearate: 96%; Cocolate acid: 99%; Polydimethylsiloxane alcohol: 99%; Carbomer U20: 99.9%; Sodium palmitate: 99%; Palmitoleic acid: 99%; Cetearyl alcohol: 99%; Sodium polyglutamate: molecular weight 50-100 kDa; Sodium myristate: 98%; Hydrogenated coconut oil acid: 99%; Coconut oil alcohol: 99%; Sodium cocoate: 99%; Docosahexaenoic acid: 99%; Sodium lauryl var.: 97%; Eicosapentaenoic acid: 98%; Sodium palmitate: 97%; Palm oil alcohol: 98% Peanutyl alcohol: ≥95%; Butyloctanol: 98%; Sodium linoleate: 95%; Butyloctanoic acid: 98%; Polyaspartic acid: molecular weight 10 kDa; Sodium decanoate: 98%; Undecenoic acid: CP, 95%; Betaine alcohol: 98%.
[0043] Example 1 A method for preparing a carboxylic acid polymer supramolecular emulsifier includes the following steps: (1) Carbomer 980 and sodium stearate were added to water and dispersed at 35°C and 150 rpm for 7 h to obtain a dispersion. (2) Add coconut oil acid and cetearyl alcohol to the dispersion and stir at 80°C and 400 rpm for 10 h to obtain a suspension; (3) The suspension was spray-dried (temperature 180℃, pressure 0.3MPa, time 7h) to obtain carboxylic acid polymer supramolecular emulsifier powder; The mass ratio of carbomer 980, sodium stearate, coconut oil acid, cetearyl alcohol, and water is 15:20:5:60:450.
[0044] Figure 1 Infrared spectrum of the carboxylic acid polymer supramolecular emulsifier powder prepared in Example 1. Figure 1 It can be seen that: among emulsifiers, Carbomer 980 at 1696 cm⁻¹ -1 The peak at 1558 cm⁻¹ shifts to lower wavenumbers (1558 cm⁻¹). -1 The shift in absorption peak originates from the change in carbonyl electron cloud density after supramolecular interaction, while the emulsifier has a peak density of 3407 cm⁻¹. -1 A distinct hydrogen bond absorption peak was observed at [location missing], indicating the presence of numerous intermolecular forces. Furthermore, the emulsifier showed a peak at 2913 cm⁻¹. -1 With 2846 cm -1 The strong absorption peaks at these locations originate from the stretching vibrations of the CH bonds in the carbon chains of fatty acids such as sodium stearate and coconut oil acid. These data confirm the formation of the supramolecular system.
[0045] Example 2 A method for preparing a carboxylic acid polymer supramolecular emulsifier includes the following steps: (1) Carbomer U20 and sodium palmitate were added to water and dispersed at 25°C and 200 rpm for 10 h to obtain a dispersion. (2) Add palmitoleic acid and polydimethylsiloxane alcohol to the dispersion and stir at 75°C and 500 rpm for 11 h to obtain a suspension; (3) The suspension was spray-dried (temperature 200℃, pressure 0.2MPa, time 5h) to obtain carboxylic acid polymer supramolecular emulsifier powder; The mass ratio of carbomer U20, sodium palmitate, palmitoleic acid, polydimethylsiloxane alcohol, and water is 30:25:10:91:450.
[0046] Example 3 A method for preparing a carboxylic acid polymer supramolecular emulsifier includes the following steps: (1) Add sodium polyglutamate and sodium myristate to water and disperse at 40°C and 150 rpm for 7 h to obtain a dispersion; (2) Add hydrogenated coconut oil acid and coconut oil alcohol to the dispersion, and stir at 105℃ and 350rpm for 10h to obtain a suspension; (3) The suspension was spray-dried (temperature 195℃, pressure 0.3MPa, time 9h) to obtain carboxylic acid polymer supramolecular emulsifier powder; The mass ratio of sodium polyglutamate, sodium myristate, hydrogenated coconut oil acid, coconut oil alcohol, and water is 1:8:0:35:450.
[0047] Example 4 In Example 1, sodium stearate was replaced with sodium cocoate and cocoagulant was replaced with docosahexaenoic acid, while other aspects remained the same as in Example 1, resulting in a carboxylic acid polymer supramolecular emulsifier powder.
[0048] Example 5 In Example 1, sodium stearate was replaced with sodium laurylate and coconut oil acid was replaced with eicosapentaenoic acid, while other aspects remained the same as in Example 1, to obtain a carboxylic acid polymer supramolecular emulsifier powder.
[0049] Example 6 In Example 1, sodium stearate was replaced with sodium palmitate and cetearyl alcohol was replaced with palm oil alcohol, while other aspects remained the same as in Example 1, to obtain a carboxylic acid polymer supramolecular emulsifier powder.
[0050] Example 7 In Example 1, cetearyl alcohol was replaced with arachidonic acid alcohol, while other aspects remained the same as in Example 1, to obtain a carboxylic acid polymer supramolecular emulsifier powder.
[0051] Example 8 In Example 1, cetearyl alcohol was replaced with butyloctanol, while other aspects remained the same as in Example 1, to obtain a carboxylic acid polymer supramolecular emulsifier powder.
[0052] Example 9 In Example 1, sodium stearate was replaced with sodium linoleate, while other aspects remained the same as in Example 1, to obtain a carboxylic acid polymer supramolecular emulsifier powder.
[0053] Example 10 In Example 1, coconut oil acid was replaced with butyloctanoic acid, while other aspects remained the same as in Example 1, to obtain a carboxylic acid polymer supramolecular emulsifier powder.
[0054] Example 11 The mass ratio of carbomer 980, sodium stearate, coconut oil acid, cetearyl alcohol, and water in Example 1 was adjusted to 20:25:10:45:450, while other aspects remained the same as in Example 1, to obtain a carboxylic acid polymer supramolecular emulsifier powder.
[0055] Example 12 The mass ratio of carbomer 980, sodium stearate, cocoacid, cetearyl alcohol, and water in Example 1 was adjusted to 5:8:10:77:450, while other aspects remained the same as in Example 1, to obtain a carboxylic acid polymer supramolecular emulsifier powder.
[0056] Example 13 The mass ratio of carbomer 980, sodium stearate, coconut oil acid, cetearyl alcohol, and water in Example 1 was adjusted to 15:20:0:65:450; all other parameters remained the same as in Example 1, resulting in a carboxylic acid polymer supramolecular emulsifier powder.
[0057] Example 14 The water in step (1) of Example 1 was adjusted to anhydrous ethanol with a mass fraction of 50%; the rest remained the same as in Example 1, and a carboxylic acid polymer supramolecular emulsifier powder was obtained.
[0058] The obtained emulsifier was subjected to performance testing, and the test results are as follows: Table 1
[0059] Comparative Example 1 A method for preparing a carboxylic acid polymer supramolecular emulsifier includes the following steps: Carbomer 980, sodium stearate, coconut oil acid, and cetearyl alcohol were added to water and dispersed at 35°C and 150 rpm for 7 h, and then stirred at 80°C and 400 rpm for 10 h to obtain a suspension. The suspension was spray-dried (temperature 180℃, pressure 0.3MPa, time 7h) to obtain a carboxylic acid polymer supramolecular emulsifier powder. The mass ratio of carbomer 980, sodium stearate, coconut oil acid, cetearyl alcohol, and water is 15:20:5:60:450.
[0060] Comparative Example 2 Adjust step (2) of Example 1 as follows: A dispersion was added to coconut oil acid and cetearyl alcohol, and the mixture was stirred at 80°C and 400 rpm for 10 h to obtain a suspension. Everything else remained the same as in Example 1, resulting in a carboxylic acid polymer supramolecular emulsifier powder.
[0061] Comparative Example 3 In Example 1, Carbomer 980 was replaced with polyaspartic acid, while other aspects remained the same as in Example 1, to obtain a carboxylic acid polymer supramolecular emulsifier powder.
[0062] Comparative Example 4 In Example 1, sodium stearate was replaced with sodium decanoate, while other aspects remained the same as in Example 1, to obtain a carboxylic acid polymer supramolecular emulsifier powder.
[0063] Comparative Example 5 In Example 1, coconut oil acid was replaced with undecenoic acid, while other aspects remained the same as in Example 1, to obtain a carboxylic acid polymer supramolecular emulsifier powder.
[0064] Comparative Example 6 In Example 1, cetearyl alcohol was replaced with behenyl alcohol, while other aspects remained the same as in Example 1, to obtain a carboxylic acid polymer supramolecular emulsifier powder.
[0065] Comparative Example 7 Adjust the temperature in step (2) of Example 1 to 110°C, and keep the other conditions the same as in Example 1 to obtain carboxylic acid polymer supramolecular emulsifier powder.
[0066] Comparative Example 8 The mass ratio of carbomer 980, sodium stearate, cocoacid, cetearyl alcohol, and water was adjusted to 15:0:5:60:450, while other parameters remained the same as in Example 1, to obtain a carboxylic acid polymer supramolecular emulsifier powder.
[0067] Comparative Example 9 The mass ratio of carbomer 980, sodium stearate, cocoacid, cetearyl alcohol, and water was adjusted to 15:20:20:60:450, while other parameters remained the same as in Example 1, to obtain a carboxylic acid polymer supramolecular emulsifier powder.
[0068] The obtained emulsifier was subjected to performance testing, and the test results are as follows: Table 2
[0069] Example 15 A method for preparing an emulsion based on the carboxylic acid polymer supramolecular emulsifier of Example 1 includes the following steps: Cetyl ethylhexanoate (7506), caprylic / capric triglyceride (gtcc), squalane, and polydimethylsiloxane were added to an oil pan and heated and stirred at 85°C and 500 rpm until completely dissolved. The carboxylic acid polymer supramolecular emulsifier powder from Example 1 was added, mixed evenly, and kept warm to obtain the oil phase. Add glycerin, 980 (carbomer), and water to an emulsifying vessel, heat at 85°C and 500 rpm and stir until completely dissolved to obtain the aqueous phase; Add the oil phase to the aqueous phase, homogenize at 2500 rpm for 5 min, and keep warm at 85℃ for 20 min; Then, the temperature was lowered to 55°C, arginine was added, and stirring and cooling continued. When the temperature reached 40°C, preservative (PE9010) was added. After the temperature dropped to room temperature, the finished emulsion was obtained. The emulsion contains, by mass percentage, 4% cetyl ethylhexanoate (7506), 3% caprylic / capric triglyceride (GTCC), 3% squalane, 1% polydimethylsiloxane, 5% glycerol, 0.3% 980 (carbomer), 1% carboxylic acid polymer supramolecular emulsifier powder from Example 1, 0.3% arginine, 0.5% preservatives, and the remainder is water.
[0070] The obtained emulsion was subjected to performance testing, and the test results are as follows: Table 3
[0071] Example 16 A method for preparing a cream based on the carboxylic acid polymer supramolecular emulsifier powder of Example 1 includes the following steps: Cetyl ethylhexanoate (7506), caprylic / capric triglyceride (gtcc), squalane, cetearyl alcohol, and polydimethylsiloxane were added to an oil pan and heated and stirred at 85°C and 450 rpm until completely dissolved. The carboxylic acid polymer supramolecular emulsifier powder from Example 1 was added, mixed evenly, and kept warm to obtain the oil phase. Add glycerin and water to an emulsifying pot, heat and stir at 85°C and 450 rpm until completely dissolved to obtain the aqueous phase; Add the oil phase to the aqueous phase, homogenize at 2650 rpm for 2 min, add Clariant Aristoflex AVC, homogenize at 450 rpm for 5 min, and keep warm at 85℃ for 20 min. Then, the temperature is lowered to 40°C, preservatives (PE9010) are added, and the finished cream is obtained after the temperature drops to room temperature. The cream contains, by weight percentage, 10% cetyl ethylhexanoate (7506), 7% caprylic / capric triglyceride (GTCC), 4.5% squalane, 1.5% hexadecyl alcohol, 2% polydimethylsiloxane, 3% glycerin, 0.5% Clariant Aristoflex AVC, 1.5% carboxylic acid polymer supramolecular emulsifier powder from Example 1, 0.5% preservatives, and the remainder is water.
[0072] The obtained cream was subjected to performance testing, and the test results are as follows: Table 4
[0073] Example 16 A method for preparing a cream based on the carboxylic acid polymer supramolecular emulsifier powder of Example 1 includes the following steps: Add meadowfoam seed oil, caprylic / capric triglyceride (gtcc), squalane, cetearyl alcohol, polydimethylsiloxane, and shea butter to an oil pan, heat and stir at 85°C and 600 rpm until completely dissolved, add the carboxylic acid polymer supramolecular emulsifier powder from Example 1, mix evenly, keep warm, and obtain the oil phase; Add glycerin and water to an emulsifying pot, heat and stir at 85°C and 600 rpm until completely dissolved to obtain the aqueous phase; Add the oil phase to the aqueous phase, homogenize at 2500 rpm for 2 min, add Clariant Aristoflex AVC, homogenize at 600 rpm for 5 min, and keep warm at 85℃ for 20 min. Then, the temperature is lowered to 40°C, preservative (PE9010) is added, and the finished cream is obtained after the temperature drops to room temperature. The cream, by weight percentage, contains: meadowfoam seed oil 5%, caprylic / capric triglyceride (GTCC) 8%, squalane 3%, cetearyl alcohol 2.5%, polydimethylsiloxane 2%, shea butter 3%, glycerin 3%, Clariant Aristoflex AVC 0.8%, the carboxylic acid polymer supramolecular emulsifier powder from Example 1 2%, preservatives 0.5%, and the remainder is water.
[0074] The obtained frost was subjected to performance testing, and the test results are as follows: Table 5
[0075] Comparative Example 10 The carboxylic acid polymer supramolecular emulsifier powder in Example 16 was changed to the emulsifier in Comparative Example 1, while everything else remained the same as in Example 16, until the face cream was ready.
[0076] The moisturizing properties of the face creams obtained in Example 16 and Comparative Example 10 were tested, and the results are as follows: Table 6. Test results of the moisturizing rate of face cream
[0077] Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Anyone skilled in the art can make various modifications and alterations without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention should be determined by the claims.
Claims
1. A method for preparing a carboxylic acid polymer supramolecular emulsifier, characterized in that, Includes the following steps: (1) Disperse the carboxylic acid polymer and sodium fatty acid in a solvent to obtain a dispersion; (2) Add fatty acids and alcohol to the dispersion, mix well, and obtain a suspension; (3) The suspension was dried to obtain a carboxylic acid polymer supramolecular emulsifier powder; The mass ratio of carboxylic acid polymer, sodium fatty acid, fatty acid, alcohol, and solvent is 1-30:8-25:0-10:35-91:
450.
2. The method according to claim 1, characterized in that, In step (1), the carboxylic acid polymer is one or two of carbomer and sodium polyglutamate; the carbomer is one or more of carbomer 980 and carbomer U20; and the sodium fatty acid is one or more of sodium stearate, sodium linoleate, sodium palmitate, sodium myristate, sodium oleate, sodium cocoate, sodium laurylate, sodium palmitate, and sodium isostearate.
3. The method according to claim 1, characterized in that, In step (2), the fatty acids are one or more of the following: linolenic acid, stearic acid, linoleic acid, palmitic acid, myristic acid, tall oil acid, oleic acid, hydrogenated coconut oil acid, coconut oil acid, caprylic acid, capric acid, lauric acid, palmitic acid, stearic acid, isostearic acid, butyloctanoic acid, docosahexaenoic acid, eicosapentaenoic acid, and hexanoic acid; and the alcohols are one or more of the following: butyloctanol, decanol, decyltetradecyl alcohol, arachidonic acid, hexyldecyl alcohol, cetyl alcohol, cetearyl alcohol, polydimethylsiloxane alcohol, myristic alcohol, octyldodecyl alcohol, lanosterol, lanolin alcohol, coconut oil alcohol, isocetyl alcohol, isostearyl alcohol, stearyl alcohol, oleyl alcohol, lauryl alcohol, and palm oil alcohol.
4. The method according to claim 1, characterized in that, In step (1), dispersion is carried out at 25-40℃ and 50-200rpm for 3-12 hours; in step (2), uniform mixing is carried out at 55-105℃ and 350-600rpm for 5-16 hours.
5. The method according to claim 1, characterized in that, In step (3), the drying is spray drying. The spray drying temperature is 160-200℃, the pressure is 0.2-0.5MPa, and the time is 4-10h.
6. The method according to claim 1, characterized in that, In step (1), the solvent is water or an aqueous solution of ethanol with a mass fraction of 40-60%.
7. The carboxylic acid polymer supramolecular emulsifier powder prepared by the method according to any one of claims 1-6.
8. The carboxylic acid polymer supramolecular emulsifier powder of claim 7 is used in the preparation of pharmaceuticals or cosmetics.
9. A cosmetic product, characterized in that, The carboxylic acid polymer supramolecular emulsifier powder described in claim 7 was used.
10. A method for improving the storage stability and emulsification efficiency of emulsions, characterized in that, The carboxylic acid polymer supramolecular emulsifier powder described in claim 7 was used.