Cosmetic production method for inhibiting adenosine phosphate precipitation in calcium-containing cosmetic
By using nano-sparking water to absorb calcium ions in calcium-containing cosmetics, the precipitation of adenosine phosphate is inhibited, the precipitation problem is solved, and the stability and user experience of the product are improved.
Patent Information
- Application Number
- CN202510574953.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-06
- Publication Date
- 2025-06-27
AI Technical Summary
When adenosine phosphate is added to calcium-containing cosmetics, precipitates are easily produced, which affects the stability and user experience of the product.
By using nano-sparkled water during cosmetic production, calcium ions are adsorbed and ion diffusion patterns in the solution are changed, thereby inhibiting the binding of calcium ions to phosphate groups and reducing or avoiding the formation of precipitation.
It effectively inhibits the precipitation of adenosine phosphate in calcium-containing cosmetics, maintains the stability and appearance of the product, and improves the user experience and shelf life.
Abstract
Description
Technical Field
[0001] The present invention relates to a method for inhibiting precipitation during the production of a cosmetic containing calcium and adenosine phosphate, belonging to the technical field of cosmetics (A61K 8 / 00, A61Q 1 / 00). Background Art
[0002] When adenosine phosphate is added to a calcium-containing cosmetic, precipitation occurs due to the combination of calcium ions (Ca 2+ )and phosphate groups (-PO4 3- ). The precipitate affects the appearance of the cosmetic, making it look uneven or turbid, thus reducing the attractiveness of the product. Some products may show stratification, and consumers need to shake them before use, which affects the convenience of use. The precipitate indicates that a chemical reaction or physical precipitation has occurred between certain components, resulting in the loss of the active ingredients of the product; when applied to the skin during use, it affects the touch and use experience or causes adverse reactions. The precipitate can also provide a growth environment for bacteria or molds, increasing the risk of cosmetic contamination. Due to the formation of the precipitate, the shelf life of the cosmetic may be shortened or even become unsafe.
[0003] For the precipitation caused by adding adenosine phosphate in existing calcium-containing cosmetics, most methods involve adding solubilizers to increase the solubility of the components, but they cannot change the formation of calcium precipitation. There are also methods of adding chelating agents to chelate calcium ions. This method of chelating calcium affects the activity of calcium ions, weakens the free property of calcium, and affects its transdermal absorption efficiency. Summary of the Invention
[0004] The technical problem to be solved by the present invention is: how to reduce or prevent the formation of precipitates when adenosine phosphate is added to a calcium-containing cosmetic.
[0005] The technical solution proposed by the present invention to solve the above technical problem is: a method for producing a cosmetic that inhibits the precipitation of adenosine phosphate in a calcium-containing cosmetic, comprising the following steps: Adding the prepared nano-bubble water into a vacuum reactor, wherein the bubble diameter of the nano-bubble water is 5 - 20 nm; The bubble concentration is 200 million / ml - 2 billion / ml; 2) Adding a calcium salt into the vacuum reactor and stirring to dissolve the calcium salt in the nano-bubble water; 3) Sequentially adding adenosine phosphate, a humectant, a skin conditioner, a stabilizer, and a preservative into the vacuum reactor, closing the vacuum reactor, evacuating and heating to 24 - 85 °C, and stirring until the nano-bubble water is completely dissolved; 4) Releasing the vacuum of the vacuum reactor, adding an acidity regulator to adjust the pH value to 4.5 - 7.5, and then adding a thickener and stirring until it is completely dissolved in the nano-bubble water.
[0006] Furthermore, the mass percentage ranges of the nano-bubble water, calcium salt, adenosine phosphate, humectant, skin conditioner, stabilizer, preservative, acidity regulator, and thickener added to the vacuum reactor in the above steps are as follows: Nano-bubble water: 55% - 80%; Calcium salt: 0.1% - 5.0%; Adenosine phosphate: 0.4% - 2.0%; Humectant: 9.0% - 30%; Skin conditioner: 0.3% - 6.0%; Stabilizer: 0.1% - 1.0%; Preservative: 0.1% - 1.0%; Acidity regulator: 0.02% - 0.5%; Thickener: 0.3% - 2.0%.
[0007] Furthermore, in step 1), the vacuum reactor is a DIEHM-150L vacuum reactor produced by DIEHM Tim Process Technology Company of Germany. The nano-bubble water is prepared by a DCNQ-10T nano-bubble hydrogen-locking water preparation device of the Drinkwell brand produced by Dalian Shuangdi Technology Co., Ltd. The bubble diameter and bubble concentration are detected by a Nanosight Pro particle tracer produced by Malvern Panalytical Limited. The vacuum degree in step 3) is from -0.03 MPa to -0.1 MPa.
[0008] Furthermore, the calcium salt is one or more of calcium pantothenate, calcium pantoyl mercaptoethyl sulfonate, calcium phosphosilicate, calcium chloride, calcium gluconate, calcium lactate, and calcium phosphate.
[0009] Furthermore, the humectant is one or more of glycerol, propylene glycol, hyaluronic acid, and sorbitol.
[0010] Furthermore, the skin conditioner is one or more of retinol, palmitoyl pentapeptide-4, vitamin C, and coenzyme Q10.
[0011] Furthermore, the stabilizer is one or more of disodium EDTA, sodium citrate, tocopherol, and BHT.
[0012] Furthermore, the preservative is one or more of phenoxyethanol, parabens, sodium benzoate, and caprylyl glycol.
[0013] Furthermore, the acidity regulator is one or more of lactic acid, citric acid, sodium hydroxide, and triethanolamine.
[0014] Furthermore, the thickener is one or more of carbomer, xanthan gum, hydroxyethyl cellulose, and magnesium aluminum silicate.
[0015] The mechanism and beneficial effects of the present invention are described as follows: 1) Interface effect: In the solution of nano-bubble water, the negatively charged surface of nano-bubbles can adsorb calcium ions in the solution, thereby reducing the concentration of free calcium ions; at the same time, the special hydrogen bond network structure of water molecules on the surface of nano-bubbles can change the diffusion mode of ions in the solution, making it more difficult for the interaction between calcium ions and phosphate groups, thus inhibiting the formation of crystal nuclei. Crystal nuclei refer to the tiny crystal nuclei formed by the collision of Ca3(PO4)2 (calcium phosphate). Once the crystal nuclei are formed and stably exist, they will continue to grow and form precipitates.
[0016] 2) Turbulence effect: Nano-bubbles with a particle size in the range of 5 - 20 nm will generate local turbulence in the solution. The high-frequency perturbation and shear force brought by the turbulence will destroy the stable environment for the formation of an ordered structure between calcium ions and phosphate groups, preventing the formation of crystal nuclei and the further stable growth of particles.
[0017] In summary, when the solution contains nano-bubbles, especially when the particle size of the bubbles is 5 - 20 nanometers, through the above interface effect and turbulence effect formed by nano-bubbles in the solution, the precipitation formation of adenosine phosphate in calcium-containing cosmetics can be significantly inhibited, thereby maintaining the stability of cosmetics containing calcium and adenosine phosphate. Specific implementation manners
[0018] Example 1
[0019] The cosmetic in this example is specifically a serum. Taking the total mass of 100 kg as an example, the components and their mass percentages are as follows: Nano-bubble water 55.35%, The calcium salt is calcium pantothenate 4.9%, Adenosine phosphate 1.9%, The moisturizer is glycerol 27.5%, The skin conditioner is retinol 5.9%, The stabilizer is disodium EDTA (ethylenediaminetetraacetic acid disodium) 0.95%, The preservative is phenoxyethanol 1%, The acidity regulator is lactic acid 0.5%, The thickener is carbomer 2%.
[0020] The production method of a serum in this example includes the following steps: 1) Add 55.35 kg of prepared nano-bubble water into a 150-liter vacuum reactor (model DIEHM-150L produced by DIEHM Tim Process Technology Company, Germany). It is required that the bubble diameter of the nano-bubble water is basically 5 nm, and the bubble concentration is controlled near 200 million bubbles per milliliter. The bubble size and bubble concentration are detected and meet the standards by using a particle tracer (model Nanosight Pro) produced by Malvern Panalytical Limited. 2) Add 4.9 kg of calcium pantothenate into the vacuum reactor, and stir to dissolve 4.9 kg of calcium pantothenate in the nano-bubble water. Control the rotation speed of the stirring paddle in the reactor at 300 rpm and stir for 10 min. 3) At room temperature of 25°C, add 1.9 kg of adenosine phosphate, 27.5 kg of glycerol, 5.9 kg of retinol, 0.95 kg of disodium EDTA (ethylenediaminetetraacetic acid disodium) and 1 kg of phenoxyethanol into the vacuum reactor in sequence. Seal the vacuum reactor, evacuate it, with a vacuum degree of -0.05 MPa, and heat up to 30°C. Control the rotation speed of the stirring paddle in the reactor at 300 rpm and stir for 50 min until the added components are completely dissolved in the nano-bubble aqueous solution. 4) Drain the vacuum of the vacuum reactor, add 0.5 kg of lactic acid to adjust the pH value to 4.5 - 7.5. In this example, the pH value is adjusted to 5.7. Then slowly add 2 kg of carbomer, control the rotation speed of the stirring paddle in the reactor at 300 rpm and stir for 1 h until the carbomer is completely dissolved in the nano-bubble aqueous solution.
[0021] Note: In step 2), the nano-bubble water and calcium pantothenate must be mixed evenly before adding other raw materials in step 3), otherwise precipitation will occur.
[0022] In step 1) of the method described in this example, the nano-bubble water is prepared by using a nano-bubble machine. The nano-bubble machine is a Drinking Health brand nano-bubble hydrogen-locking water preparation device (model DCNQ-10T) produced by Dalian Shuangdi Technology Co., Ltd.
[0023] For the purpose of comparison, this example lists an essence produced by an existing process. Taking the total mass of 100 kg as an example, the components and their mass percentages are the same as those in this example. Production method: 1) Add 27.5 kg of glycerol, 5.9 kg of retinol, 0.95 kg of disodium EDTA, 1 kg of phenoxyethanol, 4.9 kg of calcium pantothenate, and 1.9 kg of adenosine phosphate into a 150 L vacuum reactor (model DIEHM-150L) in sequence; 2) Add 55.35 kg of purified water, seal the reactor, evacuate the air, with a vacuum degree of -0.05 MPa, heat up to 30 °C, control the rotation speed of the stirring paddle in the reactor at 300 rpm, and stir for 50 min; 3) Evacuate the vacuum, add 0.5 kg of lactic acid, adjust the pH to 5.6, then add 2 kg of carbomer, control the rotation speed of the stirring paddle in the reactor at 300 rpm, and stir for 1 h until all components are completely dissolved in the aqueous solution.
[0024] The essence obtained in this example and the essence obtained by the existing process are both subjected to a product stability test experiment (conducted according to the guiding principle of T / SHFCA 002-2021 Cosmetics Stability Test). The experimental results are shown in Table 1 below: Table 1 Project Implementation Example Product Accelerated Experiment at 40°C ± 2°C Appearance Odor pH Value Centrifugation Examination (4000 rpm × 20 min) The essence obtained in this example Qualified, no precipitate Viscous transparent liquid Characteristic odor 5.7 No stratification The essence obtained by the existing process Precipitation, with precipitate Turbid Characteristic odor 5.6 Stratification, sedimentation volume 1.4% Example 2
[0025] The cosmetic in this example is specifically a facial mask liquid. Taking the total mass of 100 kg as an example, the components and their mass percentages are as follows: Nano-bubble water: 79.3%, The calcium salt is selected as calcium pantothenylcysteamine sulfonate: 0.12%, Adenosine phosphate: 0.45%, The humectant is selected as sorbitol: 13.5%, The skin conditioner is selected as vitamin C: 4%, The stabilizer is selected as sodium citrate: 0.7%, The preservative is selected as paraben: 0.11%, The acidity regulator is selected as citric acid: 0.02%, The thickener is selected as xanthan gum: 1.8%.
[0026] The production method of a facial mask liquid in this example includes the following steps: 1) Add 79.3 kg of the prepared nano-bubble water into a 150 L (liter) vacuum reactor (model DIEHM-150L). It is required that the bubble diameter of the nano-bubble water is about 10 nm, and the bubble concentration is controlled at about 500 million bubbles / ml; 2) Add 0.12 kg of calcium pantothenylcysteine sulfonate into the vacuum reactor, stir to dissolve calcium pantothenylcysteine sulfonate in the nano-bubble water, control the rotation speed of the stirring paddle in the reactor at 300 rpm, and stir for 5 min; 3) Add 0.45 kg of adenosine phosphate, 13.5 kg of sorbitol, 4 kg of vitamin C, 0.7 kg of sodium citrate, and 0.11 kg of p-hydroxybenzoate into the vacuum reactor in sequence. Seal the vacuum reactor, evacuate it, with a vacuum degree of -0.1 MPa, heat up to 40 °C, control the rotation speed of the stirring paddle in the reactor at 300 rpm, and stir for 40 min to completely dissolve the added components in the nano-bubble aqueous solution; 4) Drain the vacuum of the vacuum reactor, add 0.02 kg of citric acid to adjust the pH value to 4.5 - 7.5. In this example, the pH value is adjusted to 4.5. Then slowly add 1.8 kg of xanthan gum, control the rotation speed of the stirring paddle in the reactor at 300 rpm, and stir for 50 min until the xanthan gum is completely dissolved in the nano-bubble aqueous solution.
[0027] Note: In step 2), the nano-bubble water and calcium pantothenylcysteine sulfonate must be mixed evenly before adding other raw materials in step 3), otherwise precipitation will occur.
[0028] For comparison in this example, a facial mask liquid produced by an existing process is cited. Also taking 100 kg of the total mass as an example, the components and their mass percentages are the same as those in this example. Production method: 1) Add 13.5 kg of sorbitol, 4 kg of vitamin C, 0.7 kg of sodium citrate, 0.11 kg of p-hydroxybenzoate, 0.12 kg of calcium pantothenylcysteine sulfonate, and 0.45 kg of adenosine phosphate into a 150 L vacuum reactor (model DIEHM - 150L) in sequence; 2) Add 79.3 kg of purified water, close the reactor, evacuate it, with a vacuum degree of -0.1 MPa, heat up to 40 °C, control the rotation speed of the stirring paddle in the reactor at 300 rpm, and stir for 40 min; 3) Drain the vacuum, add 0.02 kg of citric acid, adjust the pH to 4.5, then add 1.8 kg of xanthan gum, control the rotation speed of the stirring paddle in the reactor at 300 rpm, and stir for 50 min until all components are completely dissolved in the aqueous solution.
[0029] Conduct product stability test experiments (conduct experiments according to the Guidelines for Cosmetics Stability Test T / SHFCA 002 - 2021) on the facial mask liquid obtained in this example and the facial mask liquid obtained by the existing process. The experimental results are shown in Table 2 below: Table 2 Project Implementation Example Product Accelerated Experiment at 40°C ± 2°C Appearance Odor pH Value Centrifugation Examination (4000 rpm × 20 min) The facial mask liquid obtained in this example Qualified, no precipitate Viscous semi - transparent liquid Characteristic odor 4.5 No stratification The facial mask liquid obtained by the existing process Precipitation, with precipitate Turbid Characteristic odor 4.5 Stratification, sedimentation volume 0.9% Example 3
[0030] The cosmetic product in this embodiment is specifically a serum. Taking the total mass of 100 kg as an example, the components and their mass percentages are as follows: Nano-bubble water: 68.8%, The calcium salt selected is calcium sodium phosphosilicate: 4%, Adenosine phosphate: 1.1%, The moisturizer selected is sodium hyaluronate: 24%, The skin conditioner selected is palmitoyl pentapeptide-4: 0.3%, The stabilizer selected is tocopherol: 0.1%, The preservative selected is sodium benzoate: 0.4%, The acidity regulator selected is sodium hydroxide: 0.2%, The thickener selected is hydroxyethyl cellulose: 1.1%.
[0031] A method for producing a serum in this embodiment includes the following steps: 1) Add 68.8 kg of the prepared nano-bubble water into a 150 L vacuum reactor (model DIEHM-150L). It is required that the bubble diameter of the nano-bubble water is about 15 nm, and the bubble concentration is controlled near 800 million per milliliter; 2) Add 4 kg of calcium sodium phosphosilicate into the vacuum reactor, stir to dissolve the calcium sodium phosphosilicate in the nano-bubble water, control the rotation speed of the stirring paddle in the reactor at 300 rpm, and stir for 12 min; 3) Sequentially add 1.1 kg of adenosine phosphate, 24 kg of sodium hyaluronate, 0.3 kg of palmitoyl pentapeptide-4, 0.1 kg of tocopherol, and 0.4 kg of sodium benzoate into the vacuum reactor. Seal the vacuum reactor, evacuate it, with a vacuum degree of -0.08 MPa, heat up to 60 °C, control the rotation speed of the stirring paddle in the reactor at 300 rpm, and stir for 40 min to completely dissolve the added components in the nano-bubble aqueous solution; 4) Drain the vacuum of the vacuum reactor, add 0.2 kg of sodium hydroxide to adjust the pH value to 4.5 - 7.5. In this embodiment, the pH value is adjusted to 7.5, then slowly add 1.1 kg of hydroxyethyl cellulose, control the rotation speed of the stirring paddle in the reactor at 300 rpm, and stir for 50 min until the hydroxyethyl cellulose is completely dissolved in the nano-bubble aqueous solution.
[0032] Note: In step 2), the nano-bubble water and calcium sodium phosphosilicate must be mixed evenly before adding other raw materials in step 3), otherwise precipitation will occur.
[0033] For the purpose of comparison, this example lists a essence produced by an existing process. Taking the total mass of 100 kg as an example, the components and their mass percentages are the same as those of this example. Production method: 1) Add 24 kg of sodium hyaluronate, 0.3 kg of palmitoyl pentapeptide-4, 0.1 kg of tocopherol, 0.4 kg of sodium benzoate, 4 kg of calcium phosphosilicate, and 1.1 kg of adenosine phosphate into a 150 L vacuum reactor (model DIEHM-150L) in sequence; 2) Add 68.8 kg of pure water, seal the reactor, evacuate, with the vacuum degree of -0.08 MPa, and at the same time heat up to 60 °C, control the rotation speed of the stirring paddle in the reactor at 300 rpm, and stir for 40 min; 3) Then evacuate the vacuum, add 0.2 kg of sodium hydroxide, adjust the pH to 7.5, and then slowly add 1.1 kg of hydroxyethyl cellulose, control the rotation speed of the stirring paddle in the reactor at 300 rpm, and stir for 50 min to completely dissolve all components in the aqueous solution.
[0034] The essence obtained in this example and the essence obtained by the existing process were both subjected to a product stability test experiment (conducted according to the guiding principle of cosmetic stability test T / SHFCA 002-2021), and the experimental results are shown in Table 3 below: Table 3 Project Implementation Example Product Accelerated Experiment at 40°C ± 2°C Appearance Odor pH Value Centrifugation Examination (4000 rpm × 20 min) The essence obtained in this example Qualified, no precipitate Clear and transparent Characteristic odor 7.5 No stratification The essence obtained by the existing process Precipitation, with precipitate With particulate suspension Characteristic odor 7.5 Stratification, sedimentation volume 1.0% Example 4
[0035] The cosmetic in this example is specifically a facial mask liquid. Taking the total mass of 100 kg as an example, the components and their mass percentages are as follows: Nano-bubble water: 74.1%, The calcium salt is selected as calcium gluconate: 3%, Adenosine phosphate: 1.5%, The humectant is selected as propylene glycol: 16%, The skin conditioner is selected as coenzyme Q10: 2%, The stabilizer is selected as BHT (dibutylhydroxytoluene or 2,6-di-tert-butyl-4-methylphenol): 0.5%, The preservative is selected as caprylyl glycol: 0.6%, The acidity regulator is selected as triethanolamine: 0.3%, The thickener is selected as magnesium aluminum silicate: 2%.
[0036] The production method of a facial mask liquid in this example includes the following steps: 1) Add 74.1 kg of the prepared nano-bubble water into a 150 L vacuum reactor (model DIEHM-150L). It is required that the bubble diameter of the nano-bubble water is about 18 nm, and the bubble concentration is controlled at around 1.3 billion per milliliter; 2) Add 3 kg of calcium gluconate into the vacuum reactor, stir to dissolve the calcium gluconate in the nano-bubble water, control the rotation speed of the stirring paddle in the reactor at 400 rpm, and stir for 10 min; 3) Add 1.5 kg of adenosine phosphate, 16 kg of propylene glycol, 2 kg of coenzyme Q10, 0.5 kg of BHT (dibutylhydroxytoluene or 2,6-di-tert-butyl-4-methylphenol), and 0.6 kg of caprylyl glycol into the vacuum reactor in sequence. Seal the vacuum reactor, evacuate it, with a vacuum degree of -0.03 MPa, heat up to 70 °C, control the rotation speed of the stirring paddle in the reactor at 400 rpm, and stir for 40 min to completely dissolve the added components in the nano-bubble aqueous solution; 4) Drain the vacuum of the vacuum reactor, add 0.3 kg of triethanolamine to adjust the pH value to 4.5 - 7.5. In this example, the pH value is adjusted to 7.2. Then slowly add 2 kg of magnesium aluminum silicate, control the rotation speed of the stirring paddle in the reactor at 400 rpm and stir for 80 min until the magnesium aluminum silicate is completely dissolved in the nano-bubble aqueous solution.
[0037] Note: In step 2), the nano-bubble water and calcium gluconate must be mixed evenly before adding other raw materials in step 3), otherwise precipitation will occur.
[0038] For comparison in this example, a facial mask liquid produced by an existing process is cited. Also taking 100 kg of the total mass as an example, the components and their mass percentages are the same as those in this example. Production method: 1) Add 16 kg of propylene glycol, 2 kg of coenzyme Q10, 0.5 kg of BHT, 0.6 kg of caprylyl glycol, 3.0 kg of calcium gluconate, and 1.5 kg of adenosine phosphate into a 150 L vacuum reactor (model DIEHM - 150L) in sequence; 2) Add 74.1 kg of purified water, close the reactor, evacuate it, with a vacuum degree of -0.03 MPa, and heat up to 70 °C at the same time. Control the rotation speed of the stirring paddle in the reactor at 400 rpm and stir for 40 min; 3) Drain the vacuum, add 0.3 kg of triethanolamine, adjust the pH to 7.2, then add 2.0 kg of magnesium aluminum silicate, control the rotation speed of the stirring paddle in the reactor at 400 rpm, and stir for 80 min until all components are completely dissolved in the aqueous solution.
[0039] Perform product stability test experiments on the facial mask liquid obtained in this example and the facial mask liquid obtained by the existing process (conduct the experiment according to the Guidelines for Cosmetics Stability Test T / SHFCA 002 - 2021). The experimental results are shown in Table 4 below: Table 4 Project Implementation Example Product Accelerated Experiment at 40°C ± 2°C Appearance Odor pH Value Centrifugation Examination (4000 rpm × 20 min) The facial mask liquid obtained in this example Qualified, no precipitate Viscous transparent Characteristic odor 7.2 No stratification The facial mask liquid obtained by the existing process Precipitation, with precipitate Impurities at the bottom Characteristic odor 7.2 Stratification, sedimentation volume 1.8% Example 5
[0040] The cosmetic in this embodiment is specifically a toner. Taking 100 kg of the total mass as an example, the components and their mass percentages are as follows: Nano-bubble water: 77.45%, The calcium salt selects calcium chloride 0.3% and calcium lactate 1.2%, Adenosine phosphate: 0.5%, The humectant selects propylene glycol 11% and sorbitol 2.4%, The skin conditioner retinol: 4.2% The stabilizer selects BHT (dibutylhydroxytoluene or 2,6-di-tert-butyl-4-methylphenol) 0.5%, The preservative selects phenoxyethanol 0.5%, The acidity regulator selects citric acid 0.1% and lactic acid 0.05%, The thickener selects magnesium aluminum silicate 1.2% and xanthan gum 0.6%.
[0041] A method for producing a toner in this embodiment includes the following steps: 1) Add 77.45 kg of the prepared nano-bubble water into a 150 L vacuum reactor (model DIEHM-150L). It is required that the bubble diameter of the nano-bubble water is basically 20 nm, and the bubble concentration is controlled at about 1.8 billion per milliliter; 2) Add 0.3 kg of calcium chloride and 1.2 kg of calcium lactate into the vacuum reactor, and stir to dissolve them (calcium chloride and calcium lactate) in the nano-bubble water. Control the rotation speed of the stirring paddle in the reactor at 400 rpm and stir for 15 min; 3) Sequentially add 0.5 kg of adenosine phosphate, 11 kg of propylene glycol, 2.4 kg of sorbitol, 4.2 of retinol, 0.5 kg of BHT (dibutylhydroxytoluene or 2,6-di-tert-butyl-4-methylphenol), and 0.5 kg of phenoxyethanol into the vacuum reactor. Seal the vacuum reactor, evacuate it, with a vacuum degree of -0.06 MPa, heat up to 74 °C, control the rotation speed of the stirring paddle in the reactor at 400 rpm, and stir for 60 min to completely dissolve the added components in the nano-bubble aqueous solution; 4) Drain the vacuum of the vacuum reactor, add 0.1 kg of citric acid and 0.05 kg of lactic acid, adjust the pH value to 4.5 - 7.5. In this embodiment, the pH value is adjusted to 6.3, and then slowly add 1.2 kg of magnesium aluminum silicate and 0.6 kg of xanthan gum. Control the rotation speed of the stirring paddle in the reactor at 400 rpm and stir for 70 min until the magnesium aluminum silicate and xanthan gum are dissolved in the nano-bubble aqueous solution.
[0042] Note: In step 2), the nano-bubble water must be mixed evenly with calcium chloride and calcium lactate before adding other raw materials in step 3), otherwise precipitation will occur.
[0043] For the purpose of comparison, this example lists a toner produced by an existing process. Taking a total mass of 100 kg as an example, the components and their mass percentages are the same as those in this example. Production method: 1) Add 11 kg of propylene glycol, 2.4 kg of sorbitol, 4.2 kg of retinol, 0.5 kg of BHT, 0.5 kg of phenoxyethanol, 0.5 kg of adenosine phosphate, 0.3 kg of calcium chloride, and 1.2 kg of calcium lactate into a 150 L vacuum reactor (model DIEHM-150L) in sequence; 2) Add 77.45 kg of purified water, seal the reactor, evacuate, with a vacuum degree of -0.06 MPa, and at the same time heat up to 74 °C, control the rotation speed of the stirring paddle in the reactor at 400 rpm, and stir for 60 min; 3) Evacuate the vacuum, add 0.1 kg of citric acid and 0.05 kg of lactic acid, adjust the pH to 6.2, then add 1.2 kg of magnesium aluminum silicate and 0.6 kg of xanthan gum, control the rotation speed of the stirring paddle in the reactor at 400 rpm, and stir for 70 min until all components are completely dissolved in the aqueous solution.
[0044] Both the toner obtained in this example and the toner obtained by the existing process were subjected to a product stability test experiment (conducted according to the guiding principle of cosmetic stability test T / SHFCA 002-2021). The experimental results are shown in Table 5 below: Table 5 Project Implementation Example Product Accelerated Experiment at 40°C ± 2°C Appearance Odor pH Value Centrifugation Examination (4000 rpm × 20 min) The toner obtained in this example Qualified, no precipitate Clear transparent liquid Characteristic odor 6.3 No stratification The toner obtained by the existing process Precipitation, with precipitate Turbid semi - transparent Characteristic odor 6.2 Stratification, sedimentation volume 0.9% Example 6
[0045] The cosmetic in this example is specifically a body lotion. Taking a total mass of 100 kg as an example, the components and their mass percentages are as follows: Nano-bubble water 79.05%, The calcium salt is selected as calcium gluconate 3.9% Adenosine phosphate 1.2%, The humectant is selected as glycerol 9.2% The skin conditioner is selected as palmitoyl pentapeptide-4 3.6% The stabilizers are selected as disodium EDTA (ethylenediaminetetraacetic acid disodium) 0.1% and tocopherol 0.1% The preservatives are selected as paraben 0.15% and sodium benzoate 0.05% The acidity regulators are selected as sodium hydroxide 0.05% and triethanolamine 0.1% The thickener is selected as carbomer 2.5% The production method of a body lotion in this example includes the following steps: 1) Add 79.05 kg of the prepared nano-bubble water into a 150 L vacuum reactor (model DIEHM-150L). It is required that the bubble diameter of the nano-bubble water is about 8 nm, and the bubble concentration is controlled at about 2 billion per milliliter; 2) Add 3.9 kg of calcium gluconate into the vacuum reactor, stir to dissolve it in the nano-bubble water, control the rotation speed of the stirring paddle in the reactor at 400 rpm, and stir for 10 min; 3) Sequentially add 1.2 kg of adenosine phosphate, 9.2 kg of glycerol, 3.6 kg of palmitoyl pentapeptide-4, 0.1 kg of disodium EDTA (ethylenediaminetetraacetic acid disodium), 0.1 kg of tocopherol, 0.15 kg of p-hydroxybenzoate, and 0.05 kg of sodium benzoate into the vacuum reactor. Seal the vacuum reactor, evacuate it, with a vacuum degree of -0.04 MPa, heat up to 83 °C, control the rotation speed of the stirring paddle in the reactor at 400 rpm, and stir for 65 min to completely dissolve the added components in the nano-bubble aqueous solution; 4) Drain the vacuum of the vacuum reactor, add 0.05 kg of sodium hydroxide and 0.1 kg of triethanolamine to adjust the pH value to 4.5 - 7.5. In this example, the pH value is adjusted to 7.5, and then slowly add 2.5 kg of carbomer. Control the rotation speed of the stirring paddle in the reactor at 400 rpm, and stir for 80 min until the carbomer is dissolved in the nano-bubble aqueous solution.
[0046] Note: In step 2), the nano-bubble water and calcium gluconate must be mixed evenly before adding other raw materials in step 3), otherwise precipitation will occur.
[0047] For comparison in this example, a body lotion produced by an existing process is cited. Also taking a total mass of 100 kg as an example, the components and their mass percentages are the same as those in this example. Production method: 1) Take 9.2 kg of glycerol, 3.6 kg of palmitoyl pentapeptide-4, 0.1 kg of disodium EDTA, 0.1 kg of tocopherol, 0.15 kg of p-hydroxybenzoate, 0.05 kg of sodium benzoate, 1.2 kg of adenosine phosphate, and 3.9 kg of calcium gluconate and add them sequentially into a 150 L vacuum reactor (model DIEHM-150L); 2) Add 79.05 kg of purified water, close the reactor, evacuate it, with a vacuum degree of -0.04 MPa, and at the same time heat up to 83 °C, with a stirring paddle rotation speed of 400 rpm, and stir for 65 min; 3) Drain the vacuum, add 0.05 kg of sodium hydroxide and 0.1 kg of triethanolamine to adjust the pH to 7.4, and then slowly add 2.5 kg of carbomer, with a stirring paddle rotation speed of 400 rpm, and stir for 80 min until all components are completely dissolved in the aqueous solution.
[0048] The body lotion obtained in this example and the body lotion obtained by the existing process were both subjected to a product stability test experiment (conducted according to the Guidelines for Cosmetics Stability Test T / SHFCA 002-2021). The experimental results are shown in Table 6 below: Table 6 Project Implementation Example Product Accelerated Experiment at 40°C ± 2°C Appearance Odor pH Value Centrifugation Examination (4000 rpm × 20 min) The body lotion obtained in this example Qualified, no precipitate Semi - transparent liquid Characteristic odor 7.5 No stratification The body lotion obtained by the existing process Precipitation, with precipitate Turbid, with particulate matter Characteristic odor 7.4 Stratification, sedimentation volume 2.1% Example 7
[0049] The cosmetic in this example is specifically a skin softener. Taking 100 kg of the total mass as an example, the components and their mass percentages are as follows: Nano-bubble water 73.12%, The calcium salt is selected as calcium gluconate 3.1%, calcium pantothenate 0.2%, and calcium phosphate 0.4% Adenosine phosphate 1.5%, The moisturizer is selected as sodium hyaluronate 15.6% The skin conditioner is selected as retinol 2.2% and vitamin C 1.3% The stabilizer is selected as disodium EDTA 0.3% The preservative is selected as phenoxyethanol 0.3% and sodium benzoate 0.1% The acidity regulator is selected as sodium hydroxide 0.08% The thickener is selected as hydroxyethyl cellulose 1.8% A method for producing a skin softener in this example includes the following steps: 1) Add 73.12 kg of the prepared nano-bubble water into a 150 L vacuum reactor (model DIEHM-150L). It is required that the bubble diameter of the nano-bubble water is about 13 nm, and the bubble concentration is controlled at about 1.5 billion per milliliter; 2) Add 3.1 kg of calcium gluconate, 0.2 kg of calcium pantothenate, and 0.4 kg of calcium phosphate into the vacuum reactor, and stir to dissolve them (calcium gluconate, calcium pantothenate, and calcium phosphate) in the nano-bubble water. Control the rotation speed of the stirring paddle in the reactor at 400 rpm and stir for 13 min; 3) Add 1.5 kg of adenosine phosphate, 15.6 kg of sodium hyaluronate, 2.2 kg of retinol, 1.3 kg of vitamin C, 0.3 kg of disodium EDTA, 0.3 kg of phenoxyethanol, and 0.1 kg of sodium benzoate into the vacuum reactor in sequence. Seal the vacuum reactor, evacuate it, with a vacuum degree of -0.07 MPa, and heat up to 66 °C. Control the rotation speed of the stirring paddle in the reactor at 400 rpm and stir for 55 min to completely dissolve the added components in the nano-bubble aqueous solution; 4) Drain the vacuum of the vacuum reactor, add 0.08 kg of sodium hydroxide to adjust the pH value to 4.5 - 7.5. In this example, the pH value is adjusted to 6.5. Then slowly add 1.8 kg of hydroxyethyl cellulose, and control the rotation speed of the stirring paddle in the reactor at 400 rpm. Stir for 60 min until it is completely dissolved in the nano-bubble aqueous solution.
[0050] Note: In step 2), the nano-bubble water must be mixed evenly with calcium gluconate, calcium pantothenate and calcium phosphate before adding other raw materials in step 3), otherwise precipitation will occur.
[0051] For comparison in this example, a lotion produced by the existing process is cited. Taking the total mass of 100 kg as an example, the components and their mass percentages are the same as those in this example. Production method: 1) 15.6 kg of sodium hyaluronate, 2.2 kg of retinol, 1.3 kg of vitamin C, 0.3 kg of disodium EDTA, 0.3 kg of phenoxyethanol, 0.1 kg of sodium benzoate, 1.5 kg of adenosine phosphate, 3.1 kg of calcium gluconate, 0.2 kg of calcium pantothenate and 0.4 kg of calcium phosphate are added to a 150 L vacuum reactor (model DIEHM - 150L) in sequence; 2) Add 79.05 kg of pure water, close the reactor, evacuate, the vacuum degree is -0.07 MPa, and at the same time heat up to 66 °C, the rotation speed of the stirring paddle is 400 rpm, and stir for 55 min; 3) Drain the vacuum, add 0.05 kg of sodium hydroxide and 0.1 kg of triethanolamine, adjust the pH to 6.5, then slowly add 2.5 kg of carbomer, the rotation speed of the stirring paddle is 400 rpm, and stir for 60 min until all components are completely dissolved in the aqueous solution.
[0052] Both the lotion obtained in this example and the lotion obtained by the existing process are subjected to a product stability test experiment (conducted according to the Guidelines for Cosmetics Stability Test T / SHFCA 002 - 2021). The experimental results are shown in Table 7 below: Table 7 Project Implementation Example Product Accelerated Experiment at 40°C ± 2°C Appearance Odor pH Value Centrifugation Examination (4000 rpm × 20 min) The softening lotion obtained in this example Qualified, no precipitate Clear transparent liquid Characteristic odor 6.5 No stratification The softening lotion obtained by the existing process Precipitation, with precipitate Precipitate separation Characteristic odor 6.5 Stratification, sedimentation volume 1.9% Example 8
[0053] The cosmetic in this example is specifically a beauty liquid. Taking the total mass of 100 kg as an example, the components and their mass percentages are as follows: Nano-bubble water 77.65%, The calcium salt is selected as calcium pantothenyl mercaptoethylamine sulfonate 2.1% and calcium phosphosilicate 0.8% Adenosine phosphate 0.7%, The humectant is selected as propylene glycol 8.5% and sorbitol 3.2% The skin conditioner is selected as coenzyme Q10 4.3% The stabilizer is selected as sodium citrate 0.1 and tocopherol 0.1% The preservative selected is 0.3% of p-hydroxybenzoate The acidity regulator selected is 0.05% of lactic acid The thickener selected is 2.2% of magnesium aluminum silicate A method for producing a beauty liquid in this embodiment includes the following steps: 1) Add 77.65 kg of prepared nano-bubble water into a 150 L vacuum reactor (model DIEHM-150L). It is required that the bubble diameter of the nano-bubble water is about 9 nm, and the bubble concentration is controlled at about 1.1 billion per milliliter; 2) Add 2.1 kg of calcium pantothenyl mercaptoethyl sulfonate and 0.8 kg of calcium phosphosilicate to the vacuum reactor, and stir to dissolve them (calcium pantothenyl mercaptoethyl sulfonate and calcium phosphosilicate) in the nano-bubble water. Control the rotation speed of the stirring paddle in the reactor at 350 rpm and stir for 15 min; 3) Sequentially add 0.7 kg of adenosine phosphate, 8.5 kg of propylene glycol, 3.2 kg of sorbitol, 4.3 kg of coenzyme Q10, 0.1 kg of sodium citrate, 0.1 kg of tocopherol, and 0.3 kg of p-hydroxybenzoate to the vacuum reactor. Seal the vacuum reactor, evacuate it, with a vacuum degree of -0.09 MPa, heat it up to 49 °C, and control the rotation speed of the stirring paddle in the reactor at 350 rpm and stir for 42 min to completely dissolve the added components in the solution; 4) Drain the vacuum of the vacuum reactor, add 0.05 kg of lactic acid to adjust the pH value to 4.5 - 7.5. In this embodiment, the pH value is adjusted to 5.3, and then slowly add 2.2 kg of magnesium aluminum silicate. Control the rotation speed of the stirring paddle in the reactor at 450 rpm and stir for 70 min until it is completely dissolved in the solution.
[0054] Note: In step 2), the nano-bubble water must be mixed evenly with calcium pantothenyl mercaptoethyl sulfonate and calcium phosphosilicate before adding other raw materials in step 3), otherwise precipitation will occur.
[0055] For comparison in this embodiment, a beauty liquid produced by the existing process is cited. Taking the total mass of 100 kg as an example, the components and their mass percentages are the same as those in this embodiment. Production method: 1) 8.5 kg of propylene glycol, 3.2 kg of sorbitol, 4.3 kg of coenzyme Q10, 0.1 kg of sodium citrate, 0.1 kg of tocopherol, 0.3 kg of paraben, 0.7 kg of adenosine phosphate, 2.1 kg of calcium pantothenyl mercaptoethylamine sulfonate and 0.8 kg of calcium phosphosilicate are added to a 150 L vacuum reactor (model DIEHM-150L) in sequence; 2) 77.65 kg of pure water is added, the reactor is closed, evacuated, the vacuum degree is -0.09 MPa, and at the same time the temperature is raised to 49 °C, the stirring speed of the stirring paddle is 350 rpm, and stirred for 42 min; 3) The vacuum is discharged, 0.05 kg of lactic acid is added to adjust the pH to 5.4, and then 2.2 kg of magnesium aluminum silicate is slowly added, the stirring speed of the stirring paddle is 450 rpm, and stirred for 70 min until all components are completely dissolved in the aqueous solution.
[0056] The beauty liquid obtained in this embodiment and the beauty liquid obtained by the existing process are both subjected to a product stability test experiment (conducted according to the guiding principle of T / SHFCA 002-2021 Cosmetics Stability Test), and the experimental results are shown in Table 8 below: Table 8 Project Implementation Example Product Accelerated Experiment at 40°C ± 2°C Appearance Odor pH Value Centrifugation Examination (4000 rpm × 20 min) The beauty liquid obtained in this example Qualified, no precipitate Viscous transparent liquid Characteristic odor 5.3 No stratification The beauty liquid obtained by the existing process Precipitation, with precipitate Semi - transparent liquid Characteristic odor 5.4 Stratification, sedimentation volume 0.6% The above are only the preferred embodiments of the present invention, but the present invention is not limited thereto. All equivalent substitutions or equivalent changes made according to the concept and technical solution of the present invention should be covered within the protection scope of the present invention.
Claims
1. A method for producing cosmetics for inhibiting the precipitation of adenosine phosphate in calcium-containing cosmetics, characterized in that The following steps are involved: 1) Adding the prepared nano bubble water into a vacuum reactor, wherein the bubble particle size of the nano bubble water is 5-20 nm; The bubble concentration is 200 million / ml to 2 billion / ml; 2) Add calcium salt into the vacuum reactor and stir to dissolve the calcium salt in the nanobubble water; 3) Add adenosine phosphate, moisturizer, skin conditioner, stabilizer and preservative into the vacuum reactor in sequence, seal the vacuum reactor, evacuate the reactor and heat it to 24-85°C, stirring until the nanobubble aqueous solution is completely dissolved; 4) The vacuum of the vacuum reactor is discharged, and the acidity regulator is added to adjust the pH value to 4.5-7.5, and then the thickener is added and stirred until it is completely dissolved in the nanobubble aqueous solution.
2. The cosmetic production method according to claim 1, characterized in that: The mass percentage ranges of the nano bubble water, calcium salt, adenosine phosphate, moisturizer, skin conditioner, stabilizer, preservative, acidity regulator and thickener added to the vacuum reactor are as follows: Nano bubble water 55%-80%; Calcium salt 0.1-5.0%; Adenosine phosphate 0.4-2.0%; Moisturizer 9.0%-30%; Skin conditioner 0.3%-6.0%; Stabilizer 0.1%-1.0%; Preservatives 0.1%-1.0%; Acidity regulator 0.02%-0.5%; Thickener 0.3%-2.0%.
3. The cosmetic production method according to claim 1, characterized in that: In the step 1), the vacuum reactor is a DIEHM-150L vacuum reactor produced by DIEHM Technology of Germany, the nano bubble water is prepared by a DCNQ-10T nano bubble hydrogen lock water preparation device produced by Dalian Shuangdi Technology Co., Ltd., and the bubble particle size and bubble concentration are detected by a Nanosight Pro particle tracer produced by Malvern Panalytical Co., Ltd.; the vacuum degree in the step 3) is -0.03 MPa to -0.1 MPa.
4. The cosmetic production method according to claim 2, characterized in that: The calcium salt is one or more of calcium pantothenate, calcium pantothenate sulfonate, calcium sodium phosphosilicate, calcium chloride, calcium gluconate, calcium lactate, and calcium phosphate.
5. The cosmetic production method according to claim 2, characterized in that: The moisturizing agent is one or more of glycerin, propylene glycol, hyaluronic acid and sorbitol.
6. The cosmetic production method according to claim 2, characterized in that: The skin conditioning agent is one or more of retinol, palmitoyl pentapeptide-4, vitamin C, and coenzyme Q10.
7. The cosmetic production method according to claim 2, characterized in that: The stabilizer is one or more of disodium EDTA, sodium citrate, tocopherol, and BHT.
8. The cosmetic production method according to claim 2, characterized in that: The preservative is one or more of phenoxyethanol, parabens, sodium benzoate, and caprylyl glycol.
9. The cosmetic production method according to claim 2, characterized in that: The acidity regulator is one or more of lactic acid, citric acid, sodium hydroxide and triethanolamine.
10. The cosmetic production method according to claim 2, characterized in that: The thickener is one or more of carbomer, xanthan gum, hydroxyethyl cellulose, and magnesium aluminum silicate.