CN113967172B

CN113967172B - Water-in-oil cream containing natural source emulsifier and preparation method thereof

Info

Publication number: CN113967172B
Application number: CN202111356166.3A
Authority: CN
Inventors: 夏有章; 周道年; 李名家; 孙金龙; 陈雅芬; 陈格
Original assignee: Ma Yinglong Health Co ltd
Current assignee: Ma Yinglong Health Co ltd
Priority date: 2021-11-16
Filing date: 2021-11-16
Publication date: 2023-05-16
Anticipated expiration: 2041-11-16
Also published as: CN113967172A

Abstract

The invention discloses water-in-oil cream containing a natural source emulsifier and a preparation method thereof, and solves the problems that the existing water-in-oil cream is complex in preparation process, high in difficulty and difficult to produce in large scale. Firstly, mixing water phase and then completely dissolving, then mixing oil phase and emulsifying agent and then completely dissolving, then adding water phase mixture into oil phase and emulsifying agent mixed phase, homogenizing or stirring; continuously stirring to obtain water-in-oil cream containing natural source emulsifier; the emulsifier is a mixture of polyglycerol-3 polyricinoleate and polyglycerol-3 ricinoleate. The water-in-oil cream is prepared by the method, and has the advantages of extremely simple process, low difficulty, simple components, good stability, light and heavy skin feel, no greasiness and good use feeling.

Description

Water-in-oil cream containing natural source emulsifier and preparation method thereof

Technical Field

The invention relates to the technical field of skin care products, in particular to water-in-oil cream containing a natural source emulsifier and a preparation method thereof.

Background

Water-in-oil systems have been widely used in the cosmetic industry. It is characterized by easier spreading on the skin and easier formation of a continuous protective film with a sealing effect on the skin than an oil-in-water system. Therefore, the product has good moisturizing, protecting and repairing effects, and also has good water resistance and powder dispersibility, so that the product is widely applied to products such as make-up, sun protection and the like.

However, the water-in-oil systems generally available in the market place are very demanding in terms of formulation, equipment, and processes. From the technical process, a certain heating temperature is needed when the raw materials are mixed, long-time and high-energy homogenization is often needed, the feeding speed is high, and the feeding speed, the frequency and the weight of the water phase are needed to be controlled, so that the mass production is difficult. From the aspect of the formula, the formula has high difficulty, various stabilizers and auxiliary emulsifying agents are needed to be added, the HLB value is designed reasonably, demulsification, water and oil seepage are easy to occur, and meanwhile, the product has the defects of high irritation, greasy and heavy skin feel when the paste is used, difficult application and the like.

Disclosure of Invention

The invention aims to solve the technical problems, and provides the preparation method of the water-in-oil emulsion containing the natural source emulsifier, which has extremely simple formula process requirements, even can be directly cooled and matched, has low feeding requirements, does not need to slowly control the feeding speed of the water phase, does not need to homogenize at a high speed for a long time, can be directly stirred, and is easy for mass production.

The invention also provides the water-in-oil cream containing the natural source emulsifier, which is prepared by adopting the method and has the advantages of simple components, good stability, light and non-greasy skin feel, non-thick skin feel and good use feeling.

The preparation method of the water-in-oil cream containing the natural source emulsifier comprises the following steps:

step one, dissolving a water phase containing polyol completely;

step two, mixing the emulsifier with the oil phase, and stirring and dissolving completely;

step three, adding the water phase into the mixed phase of the emulsifier and the oil phase, and uniformly stirring to obtain the water-in-oil emulsion;

the emulsifier is a mixture of polyglycerol-3 polyricinoleate and polyglycerol-3 ricinoleate, wherein the mass ratio of the polyglycerol-3 polyricinoleate is not less than 90%.

The emulsifier is prepared from polyglycerol-3 and ricinoleic acid serving as raw materials through an esterification reaction to obtain a mixture of polyglycerol-3 polyricinoleate and polyglycerol-3 ricinoleate. Specifically, natural plant glycerol and castor oil are used as raw materials, and the plant glycerol is dehydrated and distilled to obtain polyglycerol-3; castor oil reacts with NaOH aqueous solution to obtain fatty acid, and the fatty acid is distilled to obtain ricinoleic acid; the mixture of the polyglycerol-3 polyricinoleate and the polyglycerol-3 ricinoleate is obtained through esterification reaction, wherein the mass ratio of the polyglycerol-3 polyricinoleate is controlled to be not lower than 90%, and if the mass ratio of the polyglycerol-3 polyricinoleate is too small, emulsification failure is likely to be caused, or an auxiliary emulsifier is required to be added, and the emulsification energy consumption is increased.

The emulsifier mixture of the polyglycerol-3 polyricinoleate and the polyglycerol-3 ricinoleate obtained through the esterification reaction has the characteristics of a polymer structure, a triangular three-dimensional structure, a narrow hydrophilic end and a wide lipophilic end, and the curvature of dispersed liquid drops in the emulsion is larger due to the triangular structure, namely the formed dispersed liquid drops are smaller, and the paste is more stable. The water-in-oil emulsion containing the emulsifier can greatly simplify the formula during preparation, does not need various stabilizers and auxiliary emulsifiers or corresponding HLB values with reasonable design, greatly shortens the process flow, reduces the process difficulty, has low feeding requirements, does not need to slowly control the feeding speed of an aqueous phase, does not need to be heated, does not need to be homogenized at a high speed for a long time, can be directly stirred, can reduce the production energy consumption, meets the requirement of mass production, and has excellent market application value.

Preferably, the polyol is at least one of glycerol, 1, 3-propanediol, propylene glycol, and butanediol.

Depending on the product produced, the water-in-oil cream may incorporate, according to the efficacy requirements, an oily phase well known to the person skilled in the art, which may in particular comprise at least one of oils of animal origin, vegetable origin, mineral or synthetic origin.

The animal-derived fat comprises at least one of lanolin, horse oil or beeswax.

The vegetable-derived oil comprises at least one of olive oil, avocado oil, canola oil, wheat germ oil, prinsepia utilis oil, sweet almond oil, shea butter, grape seed oil or jojoba seed oil.

The mineral oil comprises at least one of white oil, vaseline or ceresin.

The synthetic oil comprises at least one of caprylic/capric glyceride, myristic acid ester, silicone oil series derivative, squalane or higher fatty alcohol.

Preferably, the water-in-oil cream further comprises an additive.

According to the produced products with different effects, different types of additives can be added into the water-in-oil cream according to the effect requirements, and the water-in-oil cream is exemplified by, but not limited to, preservatives such as chlorphenesin, phenoxyethanol, ethylparaben and the like; stabilizers such as magnesium sulfate, sodium chloride, etc.; antioxidants such as tocopheryl acetate and the like; chelating agents such as disodium EDTA and the like; pH adjusters such as aminomethylpropanol and the like; various functional components such as bisabolol, zinc oxide, phenylbenzimidazole sulfonic acid, etc.; essence, plant essential oil such as lavender essential oil, etc.

Those skilled in the art can select different types of additives according to the requirements of target products to add, and the addition amounts of the additives are the prior art and are not described in detail; the addition in step one, step two and/or step three of the preparation process according to the invention can be chosen according to the nature of the particular additive (e.g. whether it is soluble in the oil phase or water, etc.), but the amounts to be added are not taken into account in the oil phase, the water phase or the emulsifier.

Preferably, the water phase in the raw materials of the water-in-oil cream accounts for 20-85wt%, the oil phase accounts for 5-75wt%, the emulsifier accounts for 0.1-10wt%, the additive accounts for 0-20wt%, and the total weight is 100wt%. Further preferably, the addition amount of the emulsifier is 2.0-8.0wt%, and when the addition amount of the emulsifier is too high, the paste is greasy and heavy, and when the use process is too low, bad use feelings such as landslide and the like are easy to occur.

Preferably, the polyol comprises 3% to 30%, preferably 4% to 20%, and more preferably 5% to 10% of the total mass of the feedstock. According to the invention, the freezing point of the product can be reduced by adding the polyol, the problem of especially low-temperature stability of the product is solved, meanwhile, the oily and thick skin feel of the product is improved, the excessive polyol content can cause irritation, the use feeling is too thick, the product stability is poor when the content is too small, and water is especially easy to be discharged at low temperature.

Preferably, in the second step, stirring is carried out for 5-30 min under the condition of homogenizing at 1000-3000r/min until the dissolution is complete. In the third step, stirring is carried out for 10-80 min under the condition of homogenizing at 1000-3000r/min until the dissolution is complete.

The water-in-oil cream containing the natural source emulsifier is prepared by adopting the method.

Compared with the prior art, the invention has the following beneficial effects:

(1) The invention selects the specific emulsifier, has natural and safe sources, does not need a thickening agent and an auxiliary emulsifier, has simple formula process requirements, can be directly cooled and matched, is beneficial to reducing the cost and meets the requirement of formula simplification.

(2) The method has low feeding requirement, does not need to slowly control the feeding speed of the water phase, does not need to heat, does not need to homogenize at a high speed for a long time, can directly stir, not only can reduce the production energy consumption, but also is very easy for large-scale production, has low difficulty in industrial production,

(3) The product prepared by the method has simple components, good stability, light and greasy skin feel, no thick skin feel and good use feeling, and can be used for preparing various emulsions, creams or ointments and the like.

Detailed Description

Example 1: water-in-oil infant hip-protecting protective milk and preparation method thereof

Step one, completely dissolving a water phase containing polyol;

uniformly dispersing zinc oxide in an oil phase by using caprylic/capric triglyceride, adding other oil phase mixtures, uniformly dispersing, adding an emulsifier phase mixed phase, and uniformly stirring for 10min at a uniform rotation speed of 2000r/min;

and thirdly, adding the water phase containing the polyalcohol into the mixed oil phase mixed phase at one time, stirring for 40min, adding the lavender essential oil, and continuously stirring for 20min to obtain the water-in-oil infant hip-protecting emulsion.

The final product is milky emulsion, and after being inspected at the low temperature of minus 8 ℃ for one month, the product is free from layering, water and oil seepage after being circulated for one month at the temperature of minus 8 ℃ to 45 ℃, and has no obvious abnormal appearance with a constant temperature sample at 6 ℃; after high-temperature stability inspection at 45 ℃ for three months, no layering phenomenon exists; the centrifugal examination at 2000r/min and 30min also did not delaminate.

Example 2: water-in-oil sun protection emulsion and preparation method thereof

Dispersing phenylbenzimidazole sulfonic acid in a water phase containing polyol by using deionized water, adding aminomethylpropanol to adjust the phenylbenzimidazole sulfonic acid to be transparent, and then adding other raw materials in the water phase containing polyol to dissolve completely;

step two, uniformly dispersing zinc oxide by caprylic/capric triglyceride and C12-15 alcohol benzoate to obtain a zinc oxide disperse phase for later use; adding other raw materials except the premixed zinc oxide in the oil phase and an emulsifier phase, homogenizing, stirring and dissolving completely, adding the dispersed zinc oxide disperse phase, homogenizing, stirring uniformly, and homogenizing at a speed of 1500r/min;

and thirdly, adding the water phase containing the polyalcohol into the mixed oil phase mixed phase, stirring for 30min, adding essence, stirring for 5-10min, and obtaining the water-in-oil sun-proof emulsion, wherein the homogenizing rotating speed is 2000r/min.

The final product is milky emulsion, SPF50, after being inspected at the low temperature of minus 8 ℃ for one month, the product is not layered, water and oil seepage after being circulated for one month at the temperature of minus 8 ℃ to 45 ℃, and has no obvious abnormal appearance with a constant temperature sample at 6 ℃; after high-temperature stability inspection at 45 ℃ for three months, no layering phenomenon exists; the centrifugal examination at 2000r/min and 30min also did not delaminate.

Example 3: water-in-oil skin-moisturizing lotion and preparation method thereof

Step one, completely dissolving a water phase containing polyol;

step two, stirring and mixing the oil phase and the emulsifier phase uniformly;

and thirdly, adding the water phase containing the polyalcohol into the mixed oil phase mixed phase at one time, stirring for 40min, adding essence, homogenizing (1500 r/min), and stirring for 6min to obtain the water-in-oil skin-moisturizing emulsion.

The final product is milky emulsion, and after being inspected at the low temperature of minus 8 ℃ for one month, the product does not produce water or oil seepage after being circulated for one month at the temperature of minus 8 ℃ to 45 ℃, and has no obvious abnormal appearance with a constant temperature sample at 6 ℃; after high-temperature stability inspection at 45 ℃ for three months, no layering phenomenon exists; the centrifugal examination at 2000r/min and 30min also did not delaminate.

Example 4: water-in-oil infant buttock protection protective cream and preparation method thereof

Step one, completely dissolving a water phase containing polyol with hot water (75-85 ℃);

step two, uniformly dispersing zinc oxide by caprylic acid/capric acid triglyceride to obtain a zinc oxide disperse phase for later use; adding other raw materials except zinc oxide and caprylic/capric triglyceride and emulsifier into the oil phase, dissolving uniformly (75-85deg.C), adding dispersed zinc oxide disperse phase, homogenizing (1000 r/min), and stirring uniformly;

adding the water phase containing the polyalcohol into the mixed oil phase, homogenizing (1000 r/min), stirring for 20min, cooling, stirring to below 40 ℃, adding essence, homogenizing (2000 r/min), and stirring for 10min to obtain the water-in-oil infant hip-protecting cream.

The final product is cream with milky white color, and the product does not produce water or oil after being inspected at the low temperature of-8 ℃ for one month and circulated at the temperature of-8 ℃ to 45 ℃ for one month, has no obvious dissimilarity with a constant temperature sample at 6 ℃, and has no dissimilarity after being inspected at the high temperature of 45 ℃ for three months.

Example 5: water-in-oil skin cream and preparation method thereof

step two, adding the raw materials in the oil phase into an oil phase pot, heating (75-85 ℃) to dissolve completely, and then adding an emulsifier phase and stirring uniformly;

step three, adding the water phase containing the polyol into the mixed oil phase mixed phase, homogenizing (1000 r/min), stirring for 10-30min, and then cooling and stirring to below 45 ℃; adding essence, homogenizing (2000 r/min), and stirring for 6min to obtain water-in-oil skin cream.

Comparative example 1:

compared with example 1, except that the amount of the emulsifier polyglycerol-3 ricinoleate is increased to 0.3g, the content of the polyglycerol-3 polyricinoleate in the emulsifier is lower than 90%, and the amounts of other components and the preparation method are consistent.

The final product is milky emulsion, does not delaminate after being inspected at the low temperature of-8 ℃ for one month, and has delamination phenomenon after being cycled at the temperature of-8 ℃ to 45 ℃ for one month; delamination phenomenon occurs in three months after high-temperature stability inspection at 45 ℃; delamination also occurred after centrifugation at 2000r/min for 30 min.

Comparative example 2:

in comparison with example 1, the amounts of the other components and the preparation process were identical, except that the emulsifier polyglycerol-3 polyricinoleate and polyglycerol-3 ricinoleate mixture was replaced by 3.9g polyglycerol-10 decaoleate.

The final product is milky emulsion, and the layering phenomenon appears after a month of investigation at the low temperature of-8 ℃ and after a month of circulation at the temperature of-8 ℃ to 45 ℃; delamination phenomenon occurs in three months after high-temperature stability inspection at 45 ℃; delamination also occurred after centrifugation at 2000r/min for 30 min.

Comparative example 3:

compared with example 5, except that the amount of the emulsifier polyglycerol-3-ricinoleate is increased to 0.7g, the content of the polyglycerol-3-polyricinoleate in the emulsifier is lower than 90%, and the amounts of other components and the preparation method are consistent.

The final product is milky cream, the oil permeability of the product is more than 5% after the product is restored to room temperature after being inspected at the low temperature of-8 ℃ for one month, and the oil permeability of the product is more than 5% after the product is inspected at the high temperature of 45 ℃ for three months.

Comparative example 4:

in comparison with example 5, the amounts of the other components and the preparation process were identical except that the emulsifier polyglycerol-3 polyricinoleate and polyglycerol-3 ricinoleate mixture was replaced with 5.7g polyglycerol-10 decaoleate.

The final product is milky cream, the oil permeability of the product is more than 10% after the product is restored to room temperature after being inspected at the low temperature of-8 ℃ for one month, and the oil permeability of the product is more than 10% after the product is inspected at the high temperature of 45 ℃ for three months.

Comparative example 5:

compared with example 5, no glycerol is added into the water phase, and the amounts of other components and the preparation method are consistent.

The final product is milky white cream, the cream is rough and obviously water after the room temperature is restored after the cream is inspected for one month at the low temperature of-8 ℃, the oil permeability of the product is more than 10% after the room temperature is inspected for three months at the high temperature of 45 ℃, and the product has obvious landslide feeling when in use.

In summary, the water-in-oil emulsion containing the natural source emulsifier provided by the invention has the advantages that the source of the emulsifier is natural and safe, the formula process requirement is simple, even the direct cold compounding can be realized, the feeding requirement is general, the slow control of the water phase feeding speed is not needed, the long-time high-speed homogenization is not needed, the direct stirring is also needed, the mass production is easy, and the prepared final product has light, non-greasy and non-thick skin feel.

Claims

1. A method for preparing water-in-oil cream containing natural source emulsifier, which is characterized by comprising the following steps:

step one, completely dissolving an aqueous phase containing polyalcohol, wherein the polyalcohol is at least one of glycerol and butanediol or glycerol and 1, 3-propanediol;

the emulsifier is a mixture of polyglycerol-3 polyricinoleate and polyglycerol-3 polyricinoleate, and the mass ratio of the polyglycerol-3 polyricinoleate in the emulsifier is not less than 90%.

2. The method for preparing the water-in-oil emulsion containing the natural source emulsifier according to claim 1, wherein the emulsifier is a mixture of polyglycerol-3 polyricinoleate and polyglycerol-3 ricinoleate obtained by esterification reaction of polyglycerol-3 and ricinoleic acid.

3. The method for preparing a water-in-oil emulsion containing a natural source emulsifier according to claim 1, wherein the oil phase comprises at least one of animal-derived fat, vegetable-derived fat, mineral oil or synthetic fat.

4. A method of preparing a water-in-oil emulsion comprising an emulsifier of natural origin as claimed in claim 1, wherein an additive is also added during the preparation.

5. The method for preparing a water-in-oil emulsion containing a natural source emulsifier as claimed in claim 1, wherein the raw materials comprise, by mass, 20-85% of water phase, 5-75% of oil phase, 0.1-10% of emulsifier, 0-20% of additive and 100% of total.

6. The method for preparing a water-in-oil emulsion containing a natural source emulsifier according to claim 5, wherein the polyol is 1% -30% of the total mass of the raw materials.

7. The method for preparing a water-in-oil emulsion containing a natural source emulsifier according to claim 1, wherein in the second step, stirring is carried out under a homogenizing condition of 1000-3000r/min for 5-30 min until the dissolution is complete.

8. The method for preparing a water-in-oil emulsion containing a natural source emulsifier according to claim 1, wherein in the third step, stirring is carried out under a homogenizing condition of 1000-3000r/min for 10-80 min until the dissolution is complete.

9. A water-in-oil emulsion comprising an emulsifier of natural origin, characterized in that it is obtainable by a process according to any one of claims 1 to 8.