CN113967172A

CN113967172A - Water-in-oil cream containing emulsifier from natural source and preparation method thereof

Info

Publication number: CN113967172A
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: 2022-01-25
Anticipated expiration: 2041-11-16
Also published as: CN113967172B

Abstract

The invention discloses a 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 a large scale. Firstly, mixing the water phase and then completely dissolving, then mixing the oil phase and the emulsifier and then completely dissolving, then adding the water phase mixture into the mixed phase of the oil phase and the emulsifier, and homogenizing or stirring; continuously stirring to obtain water-in-oil cream containing natural source emulsifier; the emulsifier is 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 non-greasy skin feel, no heaviness and good use feeling.

Description

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

Technical Field

The invention relates to the technical field of skin care products, in particular to a 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 cosmetics industry. It is characterized by being easier to spread on the skin and easier to form 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 color cosmetics, sun protection and the like.

However, the water-in-oil system on the market has high requirements on formula, equipment and process. In terms of the process, a certain heating temperature is required during the mixing of the raw materials, a long time and high-energy homogenization are often required, the feeding speed is high, and the feeding speed, frequency and weight of the water phase need to be controlled, so that the large-scale production is difficult. From the formulation, the formulation difficulty is high, various stabilizers and auxiliary emulsifiers are required to be added, the designed HLB value is reasonable, the emulsion is easy to break and exude water and oil, and the product also has the defects of high irritation, greasy and heavy paste body in use, difficult smearing and the like.

Disclosure of Invention

The invention aims to solve the technical problems and provides a preparation method of water-in-oil cream containing a natural source emulsifier, which has the advantages of extremely simple formula process requirement, direct cold mixing, low feeding requirement, no need of slowly controlling the feeding speed of a water phase, no need of long-time high-speed homogenization, direct stirring and easy large-scale production.

The invention also provides the water-in-oil cream containing the natural source emulsifier, which is prepared by the method and has the advantages of simple components, good stability, light and non-greasy skin feel, no heavy weight and better use feeling.

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

completely dissolving a water phase containing polyalcohol;

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

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

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

The emulsifier provided by the invention is a mixture of polyglycerol-3 polyricinoleate and polyglycerol-3 ricinoleate obtained by esterification reaction of polyglycerol-3 and ricinoleic acid serving as raw materials. The preparation method specifically comprises the steps of taking natural vegetable glycerin and castor oil as raw materials, and obtaining polyglycerol-3 by dehydration reaction and distillation of the vegetable glycerin; reacting castor oil with NaOH aqueous solution to obtain fatty acid, and distilling to obtain ricinoleic acid; the polyglycerol-3 and ricinoleic acid are subjected to esterification reaction to obtain a mixture of polyglycerol-3 polyricinoleate and polyglycerol-3 polyricinoleate, wherein the mass ratio of the polyglycerol-3 polyricinoleate is controlled to be not less than 90%, and if the mass ratio of the polyglycerol-3 polyricinoleate is too small, emulsification failure is likely to occur or an auxiliary emulsifier needs to be additionally added, and the emulsification energy consumption is increased.

The emulsifier mixture of polyglycerol-3 polyricinoleate and polyglycerol-3 ricinoleate obtained by the esterification reaction has the characteristics of a polymer structure, and has a triangular three-dimensional structure, narrow hydrophilic ends and wide lipophilic ends. The water-in-oil cream containing the emulsifier can greatly simplify the formula during preparation, does not need various stabilizers, co-emulsifiers or HLB values which are reasonably designed correspondingly, greatly shortens the process flow, reduces the process difficulty, has low feeding requirement, does not need to slowly control the feeding speed of a water phase, does not need to heat, does not need to homogenize at high speed for a long time, can be directly stirred, can reduce the production energy consumption, meets the requirement of large-scale production, and has extremely good market application value.

Preferably, the polyhydric alcohol is at least one of glycerol, 1, 3-propanediol, propanediol and butanediol.

Depending on the products to be produced with different efficacies, the water-in-oil cream may be added with an oil phase well known to those skilled in the art according to the needs of the efficacies, and the oil phase may specifically include at least one of animal-derived fats and oils, vegetable-derived fats and oils, mineral oil or synthetic fats and oils.

The animal source oil 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 royle oil, sweet almond oil, shea butter, grape seed oil or jojoba seed oil.

The mineral oil comprises at least one of white oil, petrolatum, or ozokerite.

The synthetic oil comprises at least one of caprylic/capric glycerides, myristoleic acid esters, silicone oil derivatives, squalane or higher fatty alcohol.

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

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

The skilled in the art can select different types of additives to add according to the requirements of target products, and the addition amount of the additives is the prior art and is not detailed; the additives in step one, step two and/or step three of the preparation process of the present invention may be selected according to the properties of the specific additive (e.g., soluble in the oil phase or water phase, etc.), respectively, but are not included in the oil phase, water phase or emulsifier.

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

Preferably, the polyol accounts for 3% -30%, preferably 4% -20%, and more preferably 5% -10% of the total mass of the raw materials. According to the invention, the freezing point of the product can be lowered by adding the polyol, the problem of low-temperature stability of the product is solved, the product is simultaneously helpful for improving the greasy, thick and heavy skin feeling of the product, the irritation can be caused by too much polyol content, the product is poor in stability when the use feeling is too thick and heavy, and the product is easy to water at low temperature.

Preferably, in the second step, the mixture is stirred for 5-30 min under the homogenizing condition of 1000-3000r/min until the mixture is completely dissolved. In the third step, stirring is carried out for 10-80 min under the homogenizing condition of 1000-3000r/min until the solution is completely dissolved.

The water-in-oil cream containing the emulsifier from natural sources is prepared by the method.

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

(1) the invention selects the specific emulsifier, the source of the emulsifier is natural and safe, the thickener and the auxiliary emulsifier are not needed, the formula process requirement is simple, and even the cold preparation can be directly carried out, thereby being beneficial to reducing the cost and meeting the formula simplification requirement.

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

(3) the product prepared by the method has simple components, good stability, light and non-greasy skin feel, no thickness 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 protection emulsion and preparation method thereof

Completely dissolving a water phase containing polyhydric alcohol;

step two, uniformly dispersing the zinc oxide in the oil phase by using caprylic/capric triglyceride, then adding other oil phase mixtures, uniformly dispersing, adding the emulsifier phase mixed phase, and uniformly stirring for 10min at the homogenizing rotation speed of 2000 r/min;

and step three, adding the water phase containing the polyhydric alcohol into the mixed oil 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 milk.

The final product is milk white emulsion, and after the low-temperature examination at-8 ℃ for one month, the product does not delaminate, does not produce water or oil after circulating at-8 ℃ to 45 ℃ for one month, and has no obvious difference with a constant temperature sample at 6 ℃; no layering phenomenon occurs after the high-temperature stability inspection at 45 ℃ for three months; and the delamination can not be generated after centrifugal examination at 2000r/min and 30 min.

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

Step one, phenyl benzimidazole sulfonic acid in a water phase containing polyalcohol is dispersed by deionized water, then aminomethyl propanol is added to adjust the mixture to be transparent, and then other raw materials in the water phase containing polyalcohol are added to be completely dissolved;

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

and step three, adding the water phase containing the polyhydric alcohol into the mixed oil phase mixed phase, homogenizing and stirring for 30min, adding the essence, homogenizing and stirring for 5-10min to obtain the water-in-oil sun block, wherein the homogenizing rotation speed is 2000 r/min.

The final product is milk white emulsion, SPF50, and after being inspected at the low temperature of-8 ℃ for one month, the product does not delaminate, does not produce water or oil after being circulated for one month at the temperature of-8 ℃ to 45 ℃, and has no obvious difference with a constant temperature sample at the temperature of 6 ℃; no layering phenomenon occurs after the high-temperature stability inspection at 45 ℃ for three months; and the delamination can not be generated after centrifugal examination at 2000r/min and 30 min.

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

Completely dissolving a water phase containing polyhydric alcohol;

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

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

The final product is milk white emulsion, after being inspected at the low temperature of-8 ℃ for one month, the product does not produce water and oil after being circulated at the temperature of-8 ℃ to 45 ℃ for one month, and has no obvious abnormal sample with a constant temperature sample at the temperature of 6 ℃; no layering phenomenon occurs after the high-temperature stability inspection at 45 ℃ for three months; and the delamination can not be generated after centrifugal examination at 2000r/min and 30 min.

Example 4: water-in-oil infant hip-protecting cream and preparation method thereof

Step one, completely dissolving a water phase containing polyalcohol by using hot water (75-85 ℃);

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

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

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

Example 5: water-in-oil moisturizer 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, then adding the emulsifier phase, and stirring uniformly;

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

Comparative example 1:

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

The final product is milk white emulsion, and is not layered after being examined at the low temperature of 8 ℃ below zero for one month, and the layering phenomenon of the product appears after being cycled at the temperature of 8 ℃ below zero to 45 ℃ for one month; the layering phenomenon appears in three months after the high-temperature stability inspection at 45 ℃; the layering phenomenon also occurs after centrifugal examination at 2000r/min and 30 min.

Comparative example 2:

compared to example 1, the amounts of the other components and the preparation method were consistent except that the emulsifier polyglycerol-3 polyricinoleate and polyglycerol-3 ricinoleate mixture was replaced with 3.9g of polyglycerol-10 decaoleate.

The final product is milk white emulsion, and the layering phenomenon appears after one month of low temperature investigation at-8 ℃ and after one month of circulation at-8-45 ℃; the layering phenomenon appears in three months after the high-temperature stability inspection at 45 ℃; the layering phenomenon also occurs after centrifugal examination at 2000r/min and 30 min.

Comparative example 3:

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

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

Comparative example 4:

compared with example 5, the amounts of the other components and the preparation method were consistent except that the emulsifier polyglycerol-3 polyricinoleate and polyglycerol-3 ricinoleate mixture was replaced by 5.7g of polyglycerol-10 decaoleate.

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

Comparative example 5:

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

The final product is milky cream, after the room temperature is restored for one month at the low temperature of-8 ℃, the cream of the product is rough and obviously produces water, and after the room temperature is restored for three months at the high temperature of 45 ℃, the oil permeability of the product is more than 10 percent, and the skin feel of the product has obvious landslide feeling.

In conclusion, the water-in-oil cream containing the natural 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 water-in-oil cream can be directly prepared in a cold manner, the feeding requirement is general, the feeding speed of a water phase does not need to be controlled slowly, long-time high-speed homogenization is not needed, the water-in-oil cream can be directly stirred, the mass production is easy, and the prepared final product has light skin feel, is not greasy and heavy.

Claims

1. A preparation method of water-in-oil cream containing natural source emulsifier is characterized by comprising the following steps:

completely dissolving a water phase containing polyalcohol;

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

2. The method of claim 1, wherein the polyhydric alcohol in the aqueous phase is at least one of glycerol, 1, 3-propanediol, propylene glycol, and butylene glycol.

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

4. The method for producing a water-in-oil cream containing an emulsifier derived from natural sources as claimed in claim 1 or 2, wherein the oil phase comprises at least one of animal-derived fats and oils, vegetable-derived fats and oils, mineral oils or synthetic fats and oils.

5. The method for preparing water-in-oil cream containing emulsifier derived from natural sources as claimed in claim 1 or 2, wherein additives are further added during the preparation process.

6. The method for producing a water-in-oil cream containing a naturally derived emulsifier according to claim 1 or 5, wherein the raw materials comprise, in mass%, 20 to 85% of the water phase, 5 to 75% of the oil phase, 0.1 to 10% of the emulsifier, 0 to 20% of the additive, and 100% in total.

7. The method of preparing a water-in-oil cream containing a naturally derived emulsifier according to claim 6, wherein the polyol is present in an amount of 1% to 30% by weight based on the total weight of the raw materials.

8. The method for preparing water-in-oil emulsion containing natural source emulsifier as claimed in claim 1, wherein in the second step, the mixture is stirred for 5-30 min under the homogenizing condition of 1000-3000r/min until the mixture is completely dissolved.

9. The method for preparing water-in-oil emulsion containing natural source emulsifier as claimed in claim 1, wherein in the third step, stirring is carried out for 10-80 min under the homogenizing condition of 1000-3000r/min until the emulsion is completely dissolved.

10. A water-in-oil cream containing emulsifiers of natural origin, characterized in that it is obtained by a process according to any one of claims 1 to 9.