CN113332213A - All-band ultraviolet sunscreen lotion and preparation method thereof - Google Patents
All-band ultraviolet sunscreen lotion and preparation method thereof Download PDFInfo
- Publication number
- CN113332213A CN113332213A CN202110770117.8A CN202110770117A CN113332213A CN 113332213 A CN113332213 A CN 113332213A CN 202110770117 A CN202110770117 A CN 202110770117A CN 113332213 A CN113332213 A CN 113332213A
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- Prior art keywords
- agent
- sunscreen
- percent
- organic
- band ultraviolet
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- 230000006750 UV protection Effects 0.000 claims abstract description 9
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Classifications
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- A—HUMAN NECESSITIES
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9794—Liliopsida [monocotyledons]
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- A—HUMAN NECESSITIES
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/26—Aluminium; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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Abstract
The invention belongs to the field of daily chemicals, and discloses a full-wave-band ultraviolet sunscreen emulsion which comprises the following components in parts by weight: organic sunscreen agents: 10-20 parts by weight; compound organic coating sun-screening agent: 1-3 parts by weight; compound inorganic sunscreen agent: 1-5 parts by weight. The sunscreen lotion has the advantages that: the sun protection agent has the advantages of high sun protection index, safety, mildness, good stability, fresh skin feel and full-wave-band ultraviolet protection function, and can repair sunburn; meanwhile, a preparation method thereof is also disclosed.
Description
Technical Field
The invention belongs to the field of daily chemicals, and particularly relates to a full-wave-band ultraviolet sunscreen lotion and a preparation method thereof.
Background
CN201910001997.5 discloses an inorganic-organic sunscreen composite microsphere, which comprises a polymeric microsphere, inorganic sunscreen nanoparticles and an organic sunscreen agent, wherein the inorganic sunscreen nanoparticles are loaded on the surface of the polymeric microsphere; organic sunscreen agents are encapsulated within the polymeric microspheres. The sun-proof effect of full wave band has, and this application excitement is low, the security is good.
The all-band sun-screening effect is achieved by loading an inorganic sun-screening agent on the surface of the microsphere and loading an organic sun-screening agent in the microsphere. The organic sunscreen agent is embedded in the polymer microspheres, so that greasiness and degradation loss can be avoided, and the inorganic sunscreen agent is uniformly and dispersedly coated on the surfaces of the microspheres, so that agglomeration and whitening can be avoided; the inorganic and organic sunscreens are compounded synergistically, and the optimal ultraviolet full-wave band (UVA + UVB) protection effect is obtained by optimizing the type and the proportion.
However, this case does not discuss the sunscreen effect when the sunscreen agent is not simultaneously loaded on the surface and inside of the microspheres.
CN201710675929.8 discloses a sunscreen composition containing novel inorganic sunscreen agents, which comprises, by weight percent: a. an organic ultraviolet protectant; b. novel inorganic sunscreens; c. at least about 15% water; d. an oil phase comprising water-insoluble components that are liquid at ambient temperature and solid at ambient temperature.
As an alternative to sunscreen, the inorganic sunscreen agent may be in the form of a coating, the sunscreen composition of the invention comprising an inorganic metal oxide, the metal oxide being a modified metal oxide, the sunscreen product comprising the metal oxide having a high sun protection index. The modified inorganic metal oxide can provide high sun protection index, can provide effective ultraviolet irradiation protection, reduces irritation and unclean feeling brought by an organic sun-screening agent, reduces damage to skin caused by the photocatalytic effect of titanium dioxide, and reduces skin damage caused by the photoactivity of the sun-screening agent.
This approach only considers combinations of organic sunscreens and novel inorganic sunscreens, and SPF values are yet to be further improved.
The rays of sunlight with ultraviolet wavelength of 10nm-400nm are divided into 4 types, specifically long-wave ultraviolet UVA (wavelength of 400 nm-320 nm), medium-and long-wave ultraviolet UVB (wavelength of 320 nm-280 nm), high-frequency short-wave ultraviolet UVC (wavelength of 280 nm-100 nm) and ultrahigh-frequency ultra-short-wave ultraviolet EUV (wavelength of 100 nm-10 nm). Because the atmosphere around the earth has the function of filtering ultraviolet rays, the ultraviolet rays which can reach the earth surface in sunlight are only ultraviolet rays in UVA wave band and ultraviolet rays in UVB wave band. At present, a great deal of research shows that excessive intake of UVA band ultraviolet rays and UVB band ultraviolet rays can cause damage to human skin at different degrees, and the damage mainly comprises sunburn, suntan, photoaging, gene damage, skin cancer and the like. The long-term exposure of human body to ultraviolet rays not only endangers the health of the skin, but also influences the health of the human body to different degrees.
In daily life, ultraviolet rays except sunlight also exist in artificial LED lighting equipment and electronic equipment such as mobile phones, computers and televisions with ultraviolet radiation of different degrees, so that the exposure time and the ultraviolet radiation time of human skin are increased, and ultraviolet protection is always the key direction for maintaining skin health.
CN202011406371.1 discloses an oil-in-water sunscreen emulsion and a preparation method thereof, belonging to the field of cosmetics. The organic sunscreen agent in the oil-in-water sunscreen emulsion is prepared from the following raw materials including ethylhexyl methoxycinnamate, homosalate, octocrylene, ethylhexyl salicylate, diethyl-amino-hydroxybenzoyl hexyl benzoate and bis-ethylhexyloxyphenol methoxyphenyl triazine; the oil and fat comprises cyclopentadimethyl siloxane, isononyl isononanoate, C12-15 alcohol benzoate and hydrogenated polyisobutene. The oil-in-water sun-blocking emulsion provided by the invention has the advantages of strong sun-blocking capability, no stimulation to human bodies, excellent compatibility to silicon oil substances, difficult crystallization and precipitation, easy film formation, safe use, good touch and fresh skin feel. However, the sunscreen emulsion prepared only by using the pure organic sunscreen agent is difficult to completely cover skin textures due to the fact that a sunscreen film formed on the surface of the skin is not compact enough, and the full-wave-band ultraviolet formula and effect cannot be achieved; meanwhile, cyclopentadimethylsiloxane may have cyclotetrapolydimethylsiloxane which is considered as carcinogen by international public inspection in the production process, so that the risk of harming human health exists.
Therefore, it is necessary to provide a sun block with the function of protecting the ultraviolet rays in the whole wave band of 280nm-400nm, high sun protection index, safety, mildness, sunburn restoration and good stability.
Therefore, the technical problem that the present case was solved first is: how to realize the excellent ultraviolet protection effect of the whole wave band.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims at providing the full-wave-band ultraviolet sunscreen lotion and also discloses a preparation method thereof.
The sunscreen lotion has the advantages that: the sun protection agent has the advantages of high sun protection index, safety, mildness, good stability, fresh skin feel and full-wave-band ultraviolet protection function, and can repair sunburn.
The specific scheme is as follows:
the full-wave band ultraviolet sunscreen emulsion comprises the following components in parts by weight:
organic sunscreen agents: 10-20 parts by weight;
compound organic coating sun-screening agent: 1-3 parts by weight;
compound inorganic sunscreen agent: 1-5 parts by weight;
the sun-screening agent in the compound coating organic sun-screening agent is methylene bis-benzotriazolyl tetramethyl butyl phenol, and the content of the methylene bis-benzotriazolyl tetramethyl butyl phenol is 45-55 wt%; the methylene bis-benzotriazolyl tetramethyl butyl phenol is wrapped in the microspheres;
the compound inorganic sun-screening agent consists of titanium dioxide, polydimethylsiloxane, hexyl laurate, PEG-10 polydimethylsiloxane, polyglycerol-4 isostearate, stearic acid and aluminum oxide; the weight ratio of titanium dioxide, polydimethylsiloxane, hexyl laurate, PEG-10 polydimethylsiloxane, polyglycerol-4 isostearate, stearic acid and aluminum oxide is 35-45%, 30-35%, 8-12%, 5-7%, 7-10%, 3-4% and 2-3%.
For example, the mass ratio of the titanium dioxide in the composite inorganic sunscreen agent is as follows: 35%, 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44%, or 45%, etc.
According to the invention, the organic sunscreen agent, the compound coating organic sunscreen agent and the compound inorganic sunscreen agent are matched for use, so that the synergistic effect is achieved, and the safety and the mildness of the sunscreen emulsion are improved; the capability of the sunscreen emulsion for blocking ultraviolet rays can be obviously improved through the filling function of the inorganic sunscreen agent and the film forming function of the organic sunscreen agent.
In the full-wave-band ultraviolet sunscreen emulsion, the organic sunscreen agent is at least one of ethylhexyl methoxycinnamate, ethylhexyl triazone, bis-ethylhexyloxyphenol methoxyphenyl triazine and butyl methoxydibenzoylmethane.
In the full-waveband ultraviolet sunscreen emulsion, the organic sunscreen agent is a combination of ethylhexyl methoxycinnamate and ethylhexyl triazone, and the mass ratio of the ethylhexyl methoxycinnamate to the ethylhexyl triazone is 5-9: 1-3; for example, 5: 1. 6: 1. 7: 1. 8: 1. 9: 1. 5: 2. 6: 2. 7: 2. 8: 2. 9: 2. 5: 3. 6: 3. 7: 3. 8: 3 or 9: 3, etc.
Or the organic sun-screening agent is a combination of ethylhexyl methoxycinnamate and bis-ethylhexyloxyphenol methoxyphenyl triazine, and the mass ratio of the ethylhexyl methoxycinnamate to the bis-ethylhexyloxyphenol methoxyphenyl triazine is 5-9: 2-4; for example, 5: 2. 6: 2. 7: 2. 8: 2. 9: 2. 5: 3. 6: 3. 7: 3. 8: 3. 9: 3. 5: 4. 6: 4. 7: 4. 8: 4 or 9: 4, etc.
Or the organic sunscreen agent is a combination of ethylhexyl methoxycinnamate and butyl methoxydibenzoylmethane, and the mass ratio of the ethylhexyl methoxycinnamate to the butyl methoxydibenzoylmethane is 5-9: 2-4; for example, 5: 2. 6: 2. 7: 2. 8: 2. 9: 2. 5: 3. 6: 3. 7: 3. 8: 3. 9: 3. 5: 4. 6: 4. 7: 4. 8: 4 or 9: 4, etc.
In the full-wave-band ultraviolet sunscreen milk, the compound coated organic sunscreen agent consists of 48-52% of methylene bis-benzotriazolyl tetramethyl butyl phenol, 36.9-45.7% of water, 6-10% of decyl glucoside, 0.2-0.6% of propylene glycol and 0.1-0.5% of xanthan gum.
The composite coated organic sunscreen is purchased from Basff New materials Co., Ltd and is of the brand
M。
The mass ratio of the methylene bis-benzotriazolyl tetramethyl butyl phenol in the compound coating sun-screening agent is as follows: 45-55%, for example, the mass ratio of the methylene bis-benzotriazolyl tetramethyl butyl phenol in the compound encapsulated sunscreen agent is as follows: 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, or the like;
the full-wave-band ultraviolet sunscreen milk comprises the following components:
water: 32 to 66 percent
Emulsifier: 2 to 6 percent
Thickening agent: 0.3 to 1 percent
Grease: 8 to 15 percent of
Organic sunscreen agents: 10 to 20 percent
Compound organic coating sun-screening agent: 1 to 3 percent of
Compound inorganic sunscreen agent: 1 to 5 percent
Polyhydric alcohol humectant: 5-10 percent
Anti-allergy soothing agents: 0.7 to 2 percent
Auxiliary agent: 3 to 6 percent
The sum of the mass percentages of the components is 100 percent.
In the full-wave-band ultraviolet sunscreen milk, the emulsifier is at least one of stearic acid, potassium cetyl phosphate, cetearyl alcohol, glyceryl stearate and PEG-100 stearate; the thickening agent is at least one of xanthan gum, carbomer and acryloyl dimethyl ammonium taurate/VP copolymer; the grease is at least one of C12-15 alcohol benzoate, dioctyl carbonate, polydimethylsiloxane and dimethiconol; the polyalcohol humectant is at least one of glycerol, butanediol and 1, 2-hexanediol.
In the full-wave band ultraviolet sunscreen milk, the anti-allergy soothing agent is at least one of stearyl glycyrrhetinate, bisabolol and ginger root extract.
In the full-waveband ultraviolet sunscreen milk, the anti-allergy soothing agent is a combination of stearyl glycyrrhetinate, bisabolol and a ginger root extract, and the mass ratio of the stearyl glycyrrhetinate to the bisabolol to the ginger root extract is 1-2: 1-2: 1-3.
The added anti-allergy soothing agents of the invention, namely the stearyl glycyrrhetinate, the bisabolol and the ginger (ginger OFFICINALE) root extract, can achieve synergistic effect, eliminate inflammation, enhance the activity of skin repair factors, accelerate skin repair and relieve the problem of skin sunburn.
In the full-wave-band ultraviolet sunscreen milk, the auxiliary agent is at least one of a chelating agent, a pH regulator, a skin conditioner and a preservative.
The skin conditioning agent comprises sodium hyaluronate, tocopherol acetate, allantoin, panthenol and nicotinamide.
Preferably, the skin conditioner panthenol is present in the sunscreen milk in an amount of 0.5 to 1% by weight, for example, the skin conditioner panthenol is present in the sunscreen milk in an amount of 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, or 1% by weight.
Preferably, the skin conditioner niacinamide is present in the sunscreen milk in an amount of 0.3-8% by weight, for example, panthenol, which is the skin conditioner, is present in the sunscreen milk in an amount of 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, or 0.8% by weight.
Preferably, the skin conditioner centella asiatica (CENTELLA ASIATICA) extract is present in the sunscreen milk in an amount of 0.1-0.6% by weight, for example, the skin conditioner centella asiatica (CENTELLA ASIATICA) extract is present in the sunscreen milk in an amount of 0.1%, 0.2%, 0.3%, 0.4%, 0.5% or 0.6% by weight.
The skin conditioner sodium hyaluronate, tocopherol acetate, allantoin, panthenol and nicotinamide are added, so that the skin conditioner can be used for enhancing the repair capacity of the skin by cooperating with the anti-allergy soothing agent, promoting the microcirculation of the skin, enhancing the barrier function of the skin and effectively relieving the photoaging and the photodamage of the skin.
The emulsifier comprises stearic acid, potassium cetyl phosphate, cetearyl alcohol, glyceryl stearate, and PEG-100 stearate.
The thickening agent is: xanthan gum, carbomer, and ammonium acryloyldimethyl taurate/VP copolymer.
The grease comprises C12-15 alcohol benzoate, dioctyl carbonate, polydimethylsiloxane and dimethiconol.
The polyhydric alcohol humectant comprises butanediol, glycerol and 1, 2-hexanediol.
Meanwhile, the invention also discloses a preparation method of the full-waveband ultraviolet sunscreen emulsion, which comprises the steps of adding the emulsifier, the grease and the organic sunscreen agent into the oil phase reaction kettle according to a proportion, heating and dissolving the mixture completely until the mixture is transparent and free of insoluble substances; adding water, a thickening agent and a polyol humectant into a vacuum reaction kettle, heating and dissolving until the mixture is transparent and free of insoluble substances; slowly pumping the oil phase and the compound inorganic sunscreen agent into a vacuum reaction kettle, stirring and homogenizing until the oil phase and the compound inorganic sunscreen agent are uniformly mixed, and then, beginning to cool; and sequentially adding the compound organic sunscreen agent, the anti-allergy soothing agent and the auxiliary agent, stirring until the mixture is completely and uniformly mixed, and obtaining the sunscreen emulsion with the full-wave band ultraviolet protection function.
Preferably, the heating temperature of the reactor for introducing into the oil phase is 80-85 deg.C, for example, 80 deg.C, 80.5 deg.C, 81 deg.C, 81.5 deg.C, 82 deg.C, 82.5 deg.C, 83 deg.C, 83.5 deg.C, 84 deg.C, 84.5 deg.C or 85 deg.C.
Preferably, the heating temperature for charging into the vacuum reaction vessel is 85-90 deg.C, for example, the heating temperature for charging into the vacuum reaction vessel is 85 deg.C, 85.5 deg.C, 86 deg.C, 86.5 deg.C, 87 deg.C, 87.5 deg.C, 88 deg.C, 88.5 deg.C, 89 deg.C, 89.5 deg.C or 90 deg.C.
Preferably, the oil phase and the compound inorganic sunscreen agent are slowly pumped into a vacuum reaction kettle and then are reduced to 40-45 ℃;
preferably, the temperature for sequentially adding the compound organic sunscreen agent, the anti-allergy soothing agent and the auxiliary agent is 40-45 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the sunscreen emulsion obtained by the invention not only has a synergistic effect, but also indirectly improves the safety and the mildness of the sunscreen emulsion by matching the organic sunscreen agent, the compound coating organic sunscreen agent and the compound inorganic sunscreen agent; the ultraviolet rays in the whole wave band of 280nm-400nm can be effectively protected through the synergistic effect of the filling function of the inorganic sun-screening agent and the film forming function of the organic sun-screening agent, and the surface of the skin is completely covered with an ultraviolet ray protection film; the anti-inflammatory and repairing effects of the anti-allergy soothing agent and the skin conditioner are matched, so that the skin microcirculation is promoted, the skin barrier function is enhanced, the skin repairing is accelerated, and the problems of skin photoaging and photodamage are effectively relieved.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Description of raw materials:
acryloyldimethyl ammonium taurate/VP copolymer was purchased from Claien chemical (China) Inc. under the trademark ATISTTOFLEX AVC;
root extract of rhizoma Zingiberis recens (Zingiber OFFICINALE)The extract is purchased from Shanghai, Germany Limited under the brand name
AgeRepair 3040；
Kangaroo paw (ANGOZANTHOS FLAVIDUS) extract was purchased from IFF-Lucas Meyer Cosmetics under the trademark SKINectura.
Example 1
The all-band ultraviolet sunscreen emulsion comprises the following components in percentage by mass:
water: 59.5 percent; emulsifier: 3 percent; thickening agent: 0.5 percent; grease: 8 percent; organic sunscreen agents: 13 percent; compound organic coating sun-screening agent: 2 percent; compound inorganic sunscreen agent: 3 percent; polyhydric alcohol humectant: 6 percent; anti-allergy soothing agents: 1 percent; auxiliary agent: 4 percent;
wherein the emulsifier is prepared from the following components in percentage by mass: 3: 2: 1: 2 stearic acid, potassium cetyl phosphate, cetostearyl alcohol, glyceryl stearate, PEG-100 stearate;
the thickening agent is prepared from the following components in a mass ratio of 1: 2: 2 xanthan gum, carbomer, ammonium acryloyldimethyltaurate/VP copolymer;
the mass ratio of the grease is 3: 2: 2: 1C 12-15 alcohol benzoate, dioctyl carbonate, polydimethylsiloxane, dimethiconol;
the organic sunscreen agent is prepared from the following components in a mass ratio of 6: 2: 3: 2 ethylhexyl methoxycinnamate, ethylhexyl triazone, bis-ethylhexyloxyphenol methoxyphenyl triazine, butyl methoxydibenzoylmethane;
the composite coated organic sunscreen agent consists of methylene bis-benzotriazolyl tetramethyl butyl phenol, water, decyl glucoside, propylene glycol and xanthan gum, wherein the mass ratio of the methylene bis-benzotriazolyl tetramethyl butyl phenol in the composite coated sunscreen agent is 48%; the proportions of water, decyl glucoside, propylene glycol, and xanthan gum were 50%, 40%, 9%, 0.5%, and 0.5%, respectively.
The composite coated organic sunscreen is purchased from Basff New materials Co., Ltd and is of the brand
M
The composite inorganic sun-screening agent consists of titanium dioxide, polydimethylsiloxane, hexyl laurate, PEG-10 polydimethylsiloxane, polyglycerol-4 isostearate, stearic acid and aluminum oxide, wherein the mass percentage of the titanium dioxide in the composite inorganic sun-screening agent is 40%; the proportions of polydimethylsiloxane, hexyl laurate, PEG-10 polydimethylsiloxane, polyglycerol-4 isostearate, stearic acid and alumina are respectively 40%, 33%, 10%, 5%, 7%, 3% and 2%;
the polyol humectant is prepared from the following components in a mass ratio of 3: 2: 1, glycerol, butylene glycol, 1, 2-hexanediol;
the anti-allergy relieving agent is prepared from the following components in a mass ratio of 1: 1: 3 stearyl glycyrrhetinate, bisabolol, and rhizoma Zingiberis recens (Zingiber OFFICINALE) root extract.
The auxiliary agent is prepared from the following components in a mass ratio of 1: 2: 1: 1: 5: 30: 30: 8: 2 disodium EDTA, aminomethyl propanol, sodium hyaluronate, tocopherol acetate, allantoin, panthenol, niacinamide, kangaroo paw (ANIGOZANTHOS FLAVIDUS) extract, phenoxyethanol, and ethylhexylglycerin.
The preparation method of this example comprises the following steps: adding the emulsifier, the grease and the organic sunscreen agent into an oil phase reaction kettle according to the proportion, heating to 80 ℃, and completely dissolving until the mixture is transparent and free of insoluble substances; adding water, a thickening agent and a polyalcohol humectant into a vacuum reaction kettle, heating to 85 ℃, and dissolving until the mixture is transparent and free of insoluble substances; slowly pumping the oil phase and the compound inorganic sunscreen agent into a vacuum reaction kettle, stirring and homogenizing until the oil phase and the compound inorganic sunscreen agent are uniformly mixed, and then cooling to 45 ℃; and sequentially adding the compound organic sunscreen agent, the anti-allergy soothing agent and the auxiliary agent, stirring until the mixture is completely and uniformly mixed, and obtaining the sunscreen emulsion with the full-wave band ultraviolet protection function.
Example 2
The all-band ultraviolet sunscreen emulsion comprises the following components in percentage by mass:
water: 50.7 percent; emulsifier: 5 percent; thickening agent: 0.6 percent; grease: 10 percent; organic sunscreen agents: 15 percent; compound organic coating sun-screening agent: 3 percent; compound inorganic sunscreen agent: 4 percent; polyhydric alcohol humectant: 8 percent; anti-allergy soothing agents: 0.7 percent; auxiliary agent: 3 percent;
wherein the emulsifier is prepared from the following components in percentage by mass: 3: 2: 1: 2 stearic acid, potassium cetyl phosphate, cetostearyl alcohol, glyceryl stearate, PEG-100 stearate;
the thickening agent is prepared from the following components in a mass ratio of 1: 2: 3 xanthan gum, carbomer, ammonium acryloyldimethyl taurate/VP copolymer;
the mass ratio of the grease is 3: 3: 3: 1C 12-15 alcohol benzoate, dioctyl carbonate, polydimethylsiloxane, dimethiconol;
the organic sunscreen agent is prepared from the following components in percentage by mass: 2: 3: 2 ethylhexyl methoxycinnamate, ethylhexyl triazone, bis-ethylhexyloxyphenol methoxyphenyl triazine, butyl methoxydibenzoylmethane;
the compound coated organic sunscreen agent consists of methylene bis-benzotriazolyl tetramethyl butyl phenol, water, decyl glucoside, propylene glycol and xanthan gum, wherein the mass ratio of the methylene bis-benzotriazolyl tetramethyl butyl phenol in the compound coated sunscreen agent is 53%; the proportions of water, decyl glucoside, propylene glycol, xanthan gum were 48%, 43%, 8%, 0.6%, 0.4%, respectively.
Sources of composite encapsulated organic sunscreens refer to example 1.
The composite inorganic sunscreen agent consists of titanium dioxide, polydimethylsiloxane, hexyl laurate, PEG-10 polydimethylsiloxane, polyglycerol-4 isostearate, stearic acid and aluminum oxide, wherein the mass percentage of the titanium dioxide in the composite inorganic sunscreen agent is 42%; (ii) a The proportions of polydimethylsiloxane, hexyl laurate, PEG-10 polydimethylsiloxane, polyglycerol-4 isostearate, stearic acid and alumina are respectively 35%, 8%, 7%, 8%, 4% and 3%;
the polyhydric alcohol humectant is prepared from the following components in percentage by mass of 4: 3: 1, glycerol, butylene glycol, 1, 2-hexanediol; the anti-allergy relieving agent is prepared from the following components in a mass ratio of 2: 2: 3 stearyl glycyrrhetinate, bisabolol, and rhizoma Zingiberis recens (Zingiber OFFICINALE) root extract.
The auxiliary agent is prepared from the following components in a mass ratio of 1: 2: 1: 1: 15: 15: 15: 8: 2 disodium EDTA, aminomethyl propanol, sodium hyaluronate, tocopherol acetate, allantoin, panthenol, niacinamide, kangaroo paw (ANIGOZANTHOS FLAVIDUS) extract, phenoxyethanol, and ethylhexylglycerin.
The preparation method of this example comprises the following steps: adding the emulsifier, the grease and the organic sunscreen agent into an oil phase reaction kettle according to the proportion, heating to 85 ℃, and completely dissolving until the mixture is transparent and free of insoluble substances; adding water, a thickening agent and a polyalcohol humectant into a vacuum reaction kettle, heating to 90 ℃, and dissolving until the mixture is transparent and free of insoluble substances; slowly pumping the oil phase and the compound inorganic sunscreen agent into a vacuum reaction kettle, stirring and homogenizing until the oil phase and the compound inorganic sunscreen agent are uniformly mixed, and then cooling to 40 ℃; and sequentially adding the compound organic sunscreen agent, the anti-allergy soothing agent and the auxiliary agent, stirring until the mixture is completely and uniformly mixed, and obtaining the sunscreen emulsion with the full-wave band ultraviolet protection function.
Example 3
The all-band ultraviolet sunscreen emulsion comprises the following components in percentage by mass:
water: 47.5 percent; emulsifier: 6 percent; thickening agent: 1 percent; grease: 12 percent; organic sunscreen agents: 10 percent; compound organic coating sun-screening agent: 1 percent; compound inorganic sunscreen agent: 5 percent; polyhydric alcohol humectant: 10 percent; anti-allergy soothing agents: 1.5 percent; auxiliary agent: 6 percent;
wherein the emulsifier is prepared from the following components in a mass ratio of 1: 2: 1: 1: 1 stearic acid, potassium cetyl phosphate, cetostearyl alcohol, glyceryl stearate, PEG-100 stearate;
the thickening agent is prepared from the following components in a mass ratio of 1: 2: 7 xanthan gum, carbomer, ammonium acryloyldimethyl taurate/VP copolymer;
the mass ratio of the grease is 5: 3: 3: 1C 12-15 alcohol benzoate, dioctyl carbonate, polydimethylsiloxane, dimethiconol;
the organic sunscreen agent is prepared from the following components in a mass ratio of 5: 1: 2: 2 ethylhexyl methoxycinnamate, ethylhexyl triazone, bis-ethylhexyloxyphenol methoxyphenyl triazine, butyl methoxydibenzoylmethane;
the composite coated organic sunscreen agent consists of methylene bis-benzotriazolyl tetramethyl butyl phenol, water, decyl glucoside, propylene glycol and xanthan gum, wherein the mass ratio of the methylene bis-benzotriazolyl tetramethyl butyl phenol in the composite coated sunscreen agent is 45%; the proportions of water, decyl glucoside, propylene glycol, xanthan gum were 52%, 38%, 9.2%, 0.5%, 0.3%, respectively. Sources of composite encapsulated organic sunscreens refer to example 1.
The composite inorganic sunscreen agent consists of titanium dioxide, polydimethylsiloxane, hexyl laurate, PEG-10 polydimethylsiloxane, polyglycerol-4 isostearate, stearic acid and aluminum oxide, wherein the mass ratio of the titanium dioxide in the composite inorganic sunscreen agent is 45%; (ii) a The proportions of polydimethylsiloxane, hexyl laurate, PEG-10 polydimethylsiloxane, polyglycerol-4 isostearate, stearic acid and alumina are respectively 45%, 30%, 8%, 5%, 7%, 3% and 2%;
the polyhydric alcohol humectant is prepared from the following components in percentage by mass: 4: 1, glycerol, butylene glycol, 1, 2-hexanediol;
the anti-allergy relieving agent is prepared from the following components in a mass ratio of 2: 4: 9 stearyl glycyrrhetinate, bisabolol, and rhizoma Zingiberis recens (Zingiber OFFICINALE) root extract.
The auxiliary agent is prepared from the following components in a mass ratio of 1: 2: 1: 1: 30: 30: 45: 8: 2 disodium EDTA, aminomethyl propanol, sodium hyaluronate, tocopherol acetate, allantoin, panthenol, niacinamide, kangaroo paw (ANIGOZANTHOS FLAVIDUS) extract, phenoxyethanol, and ethylhexylglycerin.
The preparation method of this example comprises the following steps: adding the emulsifier, the grease and the organic sunscreen agent into an oil phase reaction kettle according to the proportion, heating to 83 ℃, and completely dissolving until the mixture is transparent and free of insoluble substances; adding water, a thickening agent and a polyol humectant into a vacuum reaction kettle, heating to 87 ℃, and dissolving until the mixture is transparent and free of insoluble substances; pumping the oil phase and the compound inorganic sunscreen agent into a vacuum reaction kettle slowly, stirring and homogenizing until the oil phase and the compound inorganic sunscreen agent are mixed uniformly, and then cooling to 443 ℃; and sequentially adding the compound organic sunscreen agent, the anti-allergy soothing agent and the auxiliary agent, stirring until the mixture is completely and uniformly mixed, and obtaining the sunscreen emulsion with the full-wave band ultraviolet protection function.
Example 4
The difference between the embodiment and the embodiment 1 is that the mass ratio of the organic sunscreen agent is 6: 2: 2: ethylhexyl methoxycinnamate, ethylhexyl triazone, bis-ethylhexyloxyphenol methoxyphenyl triazine, and butyl methoxydibenzoylmethane of 3 under the same conditions as in example 1.
Example 5
The difference between the embodiment and the embodiment 1 is that the mass ratio of the organic sunscreen agent is 7: 2: 3: ethylhexyl methoxycinnamate, ethylhexyl triazone, bis-ethylhexyloxyphenol methoxyphenyl triazine, and butyl methoxydibenzoylmethane of 3 under the same conditions as in example 1.
Example 6
The difference between this example and example 1 is that the composite coated organic sunscreen agent is composed of methylene bis-benzotriazolyl tetramethyl butylphenol, water, decyl glucoside, propylene glycol, and xanthan gum, wherein the mass ratio of methylene bis-benzotriazolyl tetramethyl butylphenol in the composite coated sunscreen agent is 45%, the reduced amount of methylene bis-benzotriazolyl tetramethyl butylphenol is supplemented with water, and the other conditions are the same as in example 1.
Example 7
The difference between this example and example 1 is that the composite coated organic sunscreen agent is composed of methylene bis-benzotriazolyl tetramethyl butylphenol, water, decyl glucoside, propylene glycol, and xanthan gum, wherein the mass ratio of methylene bis-benzotriazolyl tetramethyl butylphenol in the composite coated sunscreen agent is 55%, the added methylene bis-benzotriazolyl tetramethyl butylphenol is subtracted from water, and other conditions are the same as in example 1.
Example 8
The difference between the present example and example 1 is that the composite inorganic sunscreen agent is composed of titanium dioxide, polydimethylsiloxane, hexyl laurate, PEG-10 polydimethylsiloxane, polyglycerol-4 isostearate, stearic acid and alumina, wherein the mass ratio of the titanium dioxide in the composite inorganic sunscreen agent is 35%, the reduced titanium dioxide is supplemented by the polydimethylsiloxane, and other conditions are the same as those in example 1.
Example 9
The difference between this example and example 1 is that the composite inorganic sunscreen agent is composed of titanium dioxide, polydimethylsiloxane, hexyl laurate, PEG-10 polydimethylsiloxane, polyglycerol-4 isostearate, stearic acid, and alumina, wherein the mass of titanium dioxide in the composite inorganic sunscreen agent accounts for 45%, and the extra titanium dioxide is deducted from polydimethylsiloxane, and the other conditions are the same as those in example 1.
Comparative example 1
The comparative example differs from example 1 in that no organic sunscreen agent is included, the weight reduction is supplemented with water, and the other conditions are the same as in example 1.
Comparative example 2
The difference between the comparative example and the example 1 is that the composite coated organic sunscreen agent is not contained, the reduced weight is supplemented by water, and the rest conditions are the same as the example 1.
Comparative example 3
The difference between the comparative example and the example 1 is that the composite inorganic sunscreen agent is not contained, the weight reduction is supplemented by water, and the rest conditions are the same as the example 1.
Comparative example 4
The comparative example differs from example 1 in that it does not contain an organic sunscreen agent, the reduced weight is supplemented by a composite coated organic sunscreen agent, and the remaining conditions are the same as in example 1.
Comparative example 5
The comparative example differs from example 1 in that the composite coated organic sunscreen was not included, the weight reduction was complemented by the organic sunscreen, and the remaining conditions were the same as in example 1.
Comparative example 6
The difference between this comparative example and example 1 is that the composite inorganic sunscreen agent is not included, the reduced weight is supplemented by the organic sunscreen agent, and the rest of the conditions are the same as those in example 1.
Comparative example 7
This comparative example differs from example 1 in that the anti-allergy relief agent is not present, the weight reduction is supplemented with water, and the other conditions are the same as in example 1.
Comparative example 8
The comparative example differs from example 1 in that: the composite inorganic sun-screening agent is replaced by titanium dioxide, the dosage of the titanium dioxide is 1.2%, and the reduced weight is supplemented by water.
Test example 1
Test items: the stability accelerated test, the experimental method is as follows:
the test sample is placed in a 50g PET bottle and sealed, and is respectively placed in a room at 25 ℃, a constant temperature air blast drying box at 45 ℃, a refrigerator at-18 ℃, a refrigerator at 4 ℃ and an alternating test box at 25-45 ℃ to-18 ℃ for 3 months, and the stability of the sample is observed after the temperature is restored to room temperature (25 ℃).
The evaluation methods and evaluation criteria are shown in Table 1:
TABLE 1
The results of the stability acceleration experiment are shown in table 2:
TABLE 2
Test example 2
Test items: the stimulation test evaluation and the chick embryo chorioallantoic membrane stimulation experiment comprise the following steps:
selecting chick embryo chorioallantoic membranes (CAM) which are incubated for 10 days, recording the condition of the chorioallantoic membranes by using photographing equipment, covering a polytetrafluoroethylene resin ring with a layer of preservative film, keeping the preservative film flat, and adhering the preservative film to the polytetrafluoroethylene resin ring without falling. Transferring 40 mul of sample to be tested by a liquid transfer gun, uniformly coating the sample on a polytetrafluoroethylene resin ring with a preservative film, covering the polytetrafluoroethylene resin ring on a CAM film to ensure that the tested object is directly contacted with the CAM, recording the contact time of the tested object and the CAM, covering a gas chamber with a wetting preservative, and transferring the chick embryo into a constant temperature and humidity box to culture for 30 min. And taking out the polytetrafluoroethylene resin ring with the preservative film, photographing the tested area, observing the degree of vascular injury, and grading according to the degree of vascular injury. And performing ten groups of parallel control experiments on each sample to be detected, removing the highest score and the lowest score, and finally calculating the average score NC.
The scoring criteria are shown in table 3:
TABLE 3
The irritation evaluation criteria are shown in table 4:
TABLE 4
The experimental records and results are shown in table 5:
TABLE 5
As can be seen from the above test data, the irritativeness of the full band UV sunscreens prepared in examples 1-9 and comparative examples 1-6 was manifested as a stressful stimulus, while the full band UV sunscreens prepared in comparative example 7 were manifested as a slight stimulus. The experiments prove that the anti-allergy soothing agent can obviously improve the mildness of the sun-block emulsion.
Test example 3
Test items: sunscreen efficacy test
The test method comprises the following steps: the samples were smeared on Gafchromic film and placed in a dark box simulating high sunlight for irradiation. The charge number in the film is used for measuring the performance change of the material after being irradiated by rays, and then the irradiated film is analyzed and processed by FilmQAPRO software under a standard curve.
Gafchromic film: approximately skin tissue equivalence, medical grade precision, average effective nuclear charge number Zeff 6.8, human skin Zeff 7.4. The change of the performance of the material after being irradiated by the ray is measured by the charge number in the film and is analyzed by a system. The film is classified into two types, HD-V2 (for testing SPF value) and EBT-3 (for testing PA value).
Standard curve chart: the analysis of the sun protection value of the sample is carried out under the UVA/UVB standard curve, and the value of optical density < cGy > corresponding to the analysis value "Raverage" of the reading software is recorded, which is the value of optical density after irradiation of the sample.
The specific test results are shown in table 6:
TABLE 6
| Sample name | SPF value | PA value |
| Example 1 | 58.55 | PA+++(8.17) |
| Example 2 | 67.96 | PA+++(8.35) |
| Example 3 | 53.51 | PA+++(8.33) |
| Example 4 | 45.67 | PA+++(8.12) |
| Example 5 | 46.7 | PA+++(8.41) |
| Example 6 | 48.11 | PA+++(8.2) |
| Example 7 | 46.25 | PA+++(8.11) |
| Example 8 | 47.35 | PA+++(8.78) |
| Example 9 | 46.3 | PA+++(8.43) |
| Comparative example 1 | 27.58 | PA+++(8.11) |
| Comparative example 2 | 34.89 | PA++(6.29) |
| Comparative example 3 | 35.45 | PA++(4.56) |
| Comparative example 4 | 30.55 | PA+++(8.17) |
| Comparative example 5 | 37.11 | PA+++(8.17) |
| Comparative example 6 | 36.55 | PA+++(8.17) |
| Comparative example 7 | 50.55 | PA+++(8.17) |
| Comparative example 8 | 40.5 | PA++(7.11) |
From the above test data, it can be seen that the SPF values of the full-band UV sunscreens prepared in examples 1-9 and comparative example 7 are above 45, and the PA value is PA + + +. The components of the full-wave-band ultraviolet sunscreen emulsion are matched with each other, the synergy is realized, the protection range covers UVB and UVA wavelength regions, and the effect of effectively blocking ultraviolet rays can be realized. While the sunscreen emulsions prepared in comparative examples 1-3 (lacking any component of the sunscreen agent) have a certain sunscreen effect, they are far less effective than the full-band ultraviolet sunscreen emulsions prepared in examples 1-9; comparative examples 4-6 and comparative example 8 (any group of sunscreens is replaced by equal mass ratio) the sunscreen effect of the sunscreen emulsion prepared by the method is improved compared with that of comparative examples 1-3, but the sunscreen effect of the sunscreen emulsion prepared by the method is far from that of examples 1-9. The experiment proves that ideal sunscreen effect cannot be achieved by lacking any sunscreen component or replacing any sunscreen component, and the three sunscreen components can obviously play a role in sunscreen synergy when being matched and used at the same time.
The all-band ultraviolet sunscreen emulsion has the advantages of reasonable formula, good stability, low irritation and good sunscreen effect.
The applicant states that the present invention is illustrated by the above examples to describe the full-band ultraviolet sunscreen emulsion and the preparation method thereof, but the present invention is not limited to the above examples, i.e. it does not mean that the present invention must be implemented by the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A full-wave band ultraviolet sunscreen emulsion is characterized in that: comprises the following components in parts by weight:
organic sunscreen agents: 10-20 parts by weight;
compound organic coating sun-screening agent: 1-3 parts by weight;
compound inorganic sunscreen agent: 1-5 parts by weight;
the sun-screening agent in the compound coating organic sun-screening agent is methylene bis-benzotriazolyl tetramethyl butyl phenol, and the content of the methylene bis-benzotriazolyl tetramethyl butyl phenol is 45-55 wt%; the methylene bis-benzotriazolyl tetramethyl butyl phenol is wrapped in the microspheres;
the compound inorganic sun-screening agent consists of titanium dioxide, polydimethylsiloxane, hexyl laurate, PEG-10 polydimethylsiloxane, polyglycerol-4 isostearate, stearic acid and aluminum oxide; the weight ratio of titanium dioxide, polydimethylsiloxane, hexyl laurate, PEG-10 polydimethylsiloxane, polyglycerol-4 isostearate, stearic acid and aluminum oxide is respectively 35-45%, 30-35%, 8-12%, 5-7%, 7-10%, 3-4% and 2-3%.
2. The full band ultraviolet sunscreen lotion according to claim 1, characterized by: the organic sunscreen agent is at least one of ethylhexyl methoxycinnamate, ethylhexyl triazone, bis-ethylhexyloxyphenol methoxyphenyl triazine and butyl methoxydibenzoyl methane.
3. The full band ultraviolet sunscreen lotion according to claim 2, characterized by: the organic sunscreen agent is a combination of ethylhexyl methoxycinnamate and ethylhexyl triazone, and the mass ratio of the ethylhexyl methoxycinnamate to the ethylhexyl triazone is 5-9: 1-3;
or the organic sun-screening agent is a combination of ethylhexyl methoxycinnamate and bis-ethylhexyloxyphenol methoxyphenyl triazine, and the mass ratio of the ethylhexyl methoxycinnamate to the bis-ethylhexyloxyphenol methoxyphenyl triazine is 5-9: 2-4;
or the organic sunscreen agent is a combination of ethylhexyl methoxycinnamate and butyl methoxydibenzoylmethane, and the mass ratio of the ethylhexyl methoxycinnamate to the butyl methoxydibenzoylmethane is 5-9: 2-4.
4. The full band ultraviolet sunscreen lotion according to claim 1, characterized by: the composite coated organic sunscreen agent consists of 48-52% of methylene bis-benzotriazolyl tetramethyl butyl phenol, 36.9-45.7% of water, 6-10% of decyl glucoside, 0.2-0.6% of propylene glycol and 0.1-0.5% of xanthan gum.
5. The full band ultraviolet sunscreen lotion according to claim 1, characterized by: comprises the following components:
water: 32 to 66 percent
Emulsifier: 2 to 6 percent
Thickening agent: 0.3 to 1 percent
Grease: 8 to 15 percent of
Organic sunscreen agents: 10 to 20 percent
Compound organic coating sun-screening agent: 1 to 3 percent of
Compound inorganic sunscreen agent: 1 to 5 percent
Polyhydric alcohol humectant: 5-10 percent
Anti-allergy soothing agents: 0.7 to 2 percent
Auxiliary agent: 3 to 6 percent
The sum of the mass percentages of the components is 100 percent.
6. The full band ultraviolet sunscreen lotion according to claim 5, characterized by: the emulsifier is at least one of stearic acid, potassium cetyl phosphate, cetearyl alcohol, glyceryl stearate and PEG-100 stearate; the thickening agent is at least one of xanthan gum, carbomer and acryloyl dimethyl ammonium taurate/VP copolymer; the grease is at least one of C12-15 alcohol benzoate, dioctyl carbonate, polydimethylsiloxane and dimethiconol; the polyalcohol humectant is at least one of glycerol, butanediol and 1, 2-hexanediol.
7. The full band ultraviolet sunscreen lotion according to claim 5, characterized by: the antiallergic agent is at least one of stearyl glycyrrhetinate, bisabolol, and rhizoma Zingiberis recens extract.
8. The full band ultraviolet sunscreen lotion of claim 7 wherein: the anti-allergy soothing agent is a combination of stearyl glycyrrhetinate, bisabolol and ginger root extracts, wherein the mass ratio of the stearyl glycyrrhetinate to the bisabolol to the ginger root extracts is 1-2: 1-2: 1-3.
9. The full band ultraviolet sunscreen lotion according to claim 5, characterized by: the auxiliary agent is at least one of a chelating agent, a pH regulator, a skin conditioner and a preservative.
10. A process for the preparation of a full band uv sunscreen lotion according to any of claims 1 to 9 characterized by: adding the emulsifier, the grease and the organic sunscreen agent into an oil phase reaction kettle according to the proportion, and heating and dissolving the mixture completely until the mixture is transparent and has no insoluble substances; adding water, a thickening agent and a polyol humectant into a vacuum reaction kettle, heating and dissolving until the mixture is transparent and free of insoluble substances; slowly pumping the oil phase and the compound inorganic sunscreen agent into a vacuum reaction kettle, stirring and homogenizing until the oil phase and the compound inorganic sunscreen agent are uniformly mixed, and then, beginning to cool; and sequentially adding the compound organic sunscreen agent, the anti-allergy soothing agent and the auxiliary agent, stirring until the mixture is completely and uniformly mixed, and obtaining the sunscreen emulsion with the full-wave band ultraviolet protection function.
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Application publication date: 20210903 |