CN117205096A - Bentonite composition with sun-proof and repairing effects, and preparation method and application thereof - Google Patents
Bentonite composition with sun-proof and repairing effects, and preparation method and application thereof Download PDFInfo
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- CN117205096A CN117205096A CN202310935767.2A CN202310935767A CN117205096A CN 117205096 A CN117205096 A CN 117205096A CN 202310935767 A CN202310935767 A CN 202310935767A CN 117205096 A CN117205096 A CN 117205096A
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- bentonite
- tremella
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- 239000000440 bentonite Substances 0.000 title claims abstract description 189
- 229910000278 bentonite Inorganic materials 0.000 title claims abstract description 189
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 title claims abstract description 189
- 239000000203 mixture Substances 0.000 title claims abstract description 130
- 230000000694 effects Effects 0.000 title claims abstract description 99
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 241001506047 Tremella Species 0.000 claims abstract description 131
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000003756 stirring Methods 0.000 claims abstract description 48
- 239000007788 liquid Substances 0.000 claims abstract description 40
- 239000006185 dispersion Substances 0.000 claims abstract description 34
- UBFRDALTOGELDQ-UHFFFAOYSA-L manganese(2+) 2-methoxyphenol dichloride Chemical compound [Cl-].[Mn+2].C=1(C(O)=CC=CC1)OC.[Cl-] UBFRDALTOGELDQ-UHFFFAOYSA-L 0.000 claims abstract description 25
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims abstract description 15
- 239000002537 cosmetic Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
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- 229940091557 ethylbisiminomethylguaiacol manganese chloride Drugs 0.000 claims description 40
- YUZJJFWCXJDFOQ-UHFFFAOYSA-K manganese(3+);2-methoxy-6-[2-[(3-methoxy-2-oxidophenyl)methylideneamino]ethyliminomethyl]phenolate;chloride Chemical compound [Cl-].[Mn+3].COC1=CC=CC(C=NCCN=CC=2C(=C(OC)C=CC=2)[O-])=C1[O-] YUZJJFWCXJDFOQ-UHFFFAOYSA-K 0.000 claims description 40
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- 238000000034 method Methods 0.000 claims description 19
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- 238000002386 leaching Methods 0.000 claims description 8
- KQXNSIFXSLHNSG-UHFFFAOYSA-L [Cl-].C(C)C1=C(C(=C(C(=C1)OC)O)C=N)C=N.[Mn+2].[Cl-] Chemical compound [Cl-].C(C)C1=C(C(=C(C(=C1)OC)O)C=N)C=N.[Mn+2].[Cl-] KQXNSIFXSLHNSG-UHFFFAOYSA-L 0.000 claims description 7
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- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 3
- GTTSNKDQDACYLV-UHFFFAOYSA-N Trihydroxybutane Chemical compound CCCC(O)(O)O GTTSNKDQDACYLV-UHFFFAOYSA-N 0.000 claims description 3
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- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 2
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- LHGVFZTZFXWLCP-UHFFFAOYSA-N guaiacol Chemical compound COC1=CC=CC=C1O LHGVFZTZFXWLCP-UHFFFAOYSA-N 0.000 description 12
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- 229910021380 Manganese Chloride Inorganic materials 0.000 description 6
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- 229930003268 Vitamin C Natural products 0.000 description 6
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- 230000001476 alcoholic effect Effects 0.000 description 6
- 239000001963 growth medium Substances 0.000 description 6
- 229960001867 guaiacol Drugs 0.000 description 6
- 239000011565 manganese chloride Substances 0.000 description 6
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- 239000011718 vitamin C Substances 0.000 description 6
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
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- AXHWIVKRWPJSOF-UHFFFAOYSA-N 2-methoxyphenol;hydrochloride Chemical compound Cl.COC1=CC=CC=C1O AXHWIVKRWPJSOF-UHFFFAOYSA-N 0.000 description 1
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- 108010014258 Elastin Proteins 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 206010040829 Skin discolouration Diseases 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 206010042496 Sunburn Diseases 0.000 description 1
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Landscapes
- Cosmetics (AREA)
Abstract
The invention belongs to the technical field of cosmetic raw materials, and discloses a bentonite composition with sun-screening and repairing effects, and a preparation method and application thereof. The preparation method of the bentonite composition comprises the following steps: adding bentonite into water, and uniformly dispersing to obtain bentonite dispersion liquid; adding the tremella solution into bentonite dispersion liquid, heating and stirring to obtain viscous liquid to obtain mixed dispersion liquid; adding the ethyl diiminomethyl guaiacol manganese chloride into the polyhydric alcohol, uniformly mixing to obtain an ethyl diiminomethyl guaiacol manganese chloride solution, adding the ethyl diiminomethyl guaiacol manganese chloride solution into the mixed dispersion liquid, and uniformly stirring to obtain the bentonite composition with sun-screening and repairing effects. The bentonite composition prepared by the invention has the synergistic effect of bentonite, tremella solution and ethyl diiminomethyl guaiacol manganese chloride, so that the prepared composition has good sun-screening and repairing effects.
Description
Technical Field
The invention belongs to the technical field of cosmetic raw materials, and particularly relates to a bentonite composition with sun protection and repair effects, and a preparation method and application thereof.
Background
Sun protection is an indispensable step in daytime skin care, and sun protection products are necessary for people who pursue skin lightening, especially for their home travel. The sun-screening products are mainly used for protecting UVA (long-wave ultraviolet) and UVB (medium-wave ultraviolet), skin cells can be damaged after the skin is exposed to ultraviolet rays, the skin barrier function is weakened, and skin inflammation and burn can be caused; destroying the moisturizing function of the skin and drying the skin; the tyrosinase can be activated, the pigment synthesis is accelerated, and skin sunburn is generated; can promote reduction of elastin and collagen in dermis layer, and loss of supporting force of skin, and wrinkles. The index of the detection of the sun protection ability of cosmetics is specified in the technical Specification for cosmetic safety (2015): UVA protection index (PFA number) determination, and sun protection index (SPF number) determination.
Some merchants often add excessive physical sunscreens to improve the SPF value and the PA value, and although the sunscreens can improve the sun protection index of the product, the excessive physical sunscreens can deposit into thicker white layers on the skin surface, so that pores are easy to be blocked, and the normal secretion of sebaceous glands and sweat glands is influenced. In addition, excessive physical sunscreens are prone to falling off the skin surface, causing the phenomenon of mud or powder lifting. The long-term use of the pseudo high sun-screening emulsion can inhibit the normal metabolism of skin epidermal cells, so that the loss of skin percutaneous moisture is increased, and the epidermal barrier function of the skin is weakened.
Disclosure of Invention
In order to overcome the disadvantages and shortcomings of the prior art, a primary object of the present invention is to provide a method for preparing a bentonite composition having sun protection and repair effects.
It is another object of the present invention to provide a bentonite composition having sun protection and repair effects prepared by the above method.
It is a further object of the present invention to provide the use of the bentonite composition having sunscreen and repair effects described above.
The aim of the invention is achieved by the following scheme:
a method for preparing a bentonite composition having sun protection and repair effects, comprising the steps of:
(1) Adding bentonite into water, and uniformly dispersing to obtain bentonite dispersion liquid;
(2) Adding the tremella solution into bentonite dispersion liquid, heating and stirring to obtain viscous liquid to obtain mixed dispersion liquid;
(3) Adding the ethyl bis (iminomethyl) guaiacol manganese chloride into the polyalcohol, and uniformly mixing to obtain an ethyl bis (iminomethyl) guaiacol manganese chloride solution;
(4) And (3) adding the ethyl diiminomethyl guaiacol manganese chloride solution into the mixed dispersion liquid in the step (2), and uniformly stirring to obtain the bentonite composition with sun protection and repair effects.
Physical sunscreens are typically metal oxides, with zinc oxide, titanium dioxide, zirconium oxide, silicon dioxide, ferric oxide, and the like being the primary inorganic sunscreens. The silica, commonly called as "white carbon black", is prepared based on bentonite at high temperature, acidizing, filtering and washing, and has certain waterproof capability in a sun-proof product. However, after the bentonite is refined and extracted, the silica lacks the strong water-absorbing swelling capacity of the original bentonite, and the skin problems of pore blockage, mud rubbing or floating powder can be caused while the sun-screening efficacy is reduced. The natural bentonite has the advantages of strong water absorbability, adsorptivity, water cohesiveness, no toxicity and the like, and can protect skin from excessive dryness during sun-screening and reduce the phenomenon of floating powder.
The tremella is edible and medicinal fungus, and the tremella polysaccharide is used as a main component, has excellent moisturizing performance, and can form a layer of soft film on the epidermis to keep the moisture content of the skin.
The antioxidant enzyme small molecule ethyl diiminomethyl guaiacol manganese chloride (EUK) is a synthetic superoxide dismutase (SOD)/catalase mimic, has high-efficiency antioxidant activity, has catalase and cytoprotective activity and SOD activity, and the molecular weight of EUK is 416.74, belongs to a small molecule compound, and can directly enter the skin to play a role.
The bentonite composition prepared by combining natural bentonite, tremella solution and antioxidant enzyme small-molecule ethyl diiminomethyl guaiacol manganese chloride has good sun-screening and repairing effects. The bentonite composition prepared by the invention can block ultraviolet rays and increase the antioxidation function at the same time, thereby achieving the purpose of protecting the skin in all directions. The bentonite composition prepared by lacking any one of bentonite, tremella solution or ethyl diiminomethyl guaiacol manganese chloride or replacing the components thereof has poor sun-screening and repairing effects.
In some embodiments, the bentonite of step (1) has a particle size of 2-8 μm; preferably 3 μm.
In some embodiments, the bentonite is present in the bentonite composition having sunscreen and repair efficacy in a mass percentage of 6-15%; preferably 10%.
In some embodiments, the water of step (1) is present in the bentonite composition having sun protection and repair efficacy in a mass percentage of 20-60%; preferably 45%.
In some embodiments, the operation of step (1) of homogenizing is a shear homogenizing treatment at a rotational speed of 5000-8000rpm for a period of 20-60min; preferably, the rotation speed of the shearing homogenization treatment is 7000rpm, and the time of the shearing homogenization treatment is 40min.
In some embodiments, the tremella solution in step (2) is at least one of tremella extract, tremella fermentation broth, tremella polysaccharide solution; the mass percentage of the tremella solution in the bentonite composition with sun protection and repair effects is 8-16%; preferably, the tremella solution is tremella fermentation liquor; the mass percentage of the tremella fermentation liquid in the bentonite composition with sun-proof and repairing effects is 12%.
In some embodiments, the tremella extract is prepared by the following steps: mixing the dried tremella powder with water, leaching, and filtering to obtain tremella extract.
Further, the mass ratio of the dry tremella powder to the water is 1:5-15, preferably 1:10.
Further, the leaching temperature is 50-90 ℃, and the leaching time is 1-6h; preferably, the temperature of the leaching is 70℃and the time of leaching is 3 hours.
In some embodiments, the tremella fermentation broth is prepared by: and adding the bacillus seed liquid into a tremella fermentation medium, fermenting, culturing and filtering to obtain tremella fermentation liquid.
Further, the bacillus seed solution has a concentration of 10 7 -10 9 cfu/mL; preferably 10 8 cfu/mL。
Further, the tremella fermentation medium comprises 0.5-2% of dry tremella powder, 1-3% of glucose, 0.5-2% of ammonium chloride, 0.5-2% of soybean peptone and the balance of water, wherein the percentages refer to mass percent; preferably, the tremella fermentation medium comprises 1% of dry tremella powder, 2% of glucose, 1% of ammonium chloride, 1% of soybean peptone and 95% of water.
Further, the temperature of the fermentation culture is 28-33 ℃, and the time of the fermentation culture is 36-60 hours; preferably, the temperature of the fermentation culture is 30 ℃, and the time of the fermentation culture is 48 hours.
Further, the filtration is diatomite filtration or microfiltration membrane filtration.
In some embodiments, the tremella polysaccharide solution is a tremella polysaccharide solution with a mass fraction of 0.5-3%; the molecular weight of the tremella polysaccharide is 500000-1500000 Da.
In some embodiments, the temperature of the heating and stirring in step (2) is 50-80 ℃, the speed of the heating and stirring is 150-500rpm, and the time of the heating and stirring is 2-10h; preferably, the heating and stirring temperature is 60 ℃, the heating and stirring speed is 350rpm, and the heating and stirring time is 6h.
In some embodiments, the tremella solution of step (2) is added at a rate of 0.5-5mL/min; preferably 2mL/min.
In some embodiments, the mass percentage of the ethyldiiminomethyl guaiacol manganese chloride in step (3) in the bentonite composition having sun protection and repair efficacy is 0.5 to 2%, preferably 1%.
In some embodiments, the polyol of step (3) is at least one of butanediol, butanetriol, pentaerythritol, hexanediol, sorbitol, xylitol; butanediol is preferred.
In some embodiments, the mass percentage of the polyol of step (3) in the bentonite composition having sun protection and repair efficacy is 20-50%, preferably 32%.
In some embodiments, the step (3) of uniformly mixing is uniformly stirring, the stirring speed is 100-300rpm, and the stirring time is 2-10 hours; preferably, the stirring temperature in the step (3) is 25 ℃, the stirring speed is 200rpm, and the stirring time is 3 hours.
In some embodiments, the adding of step (4) is a dropwise addition, at a rate of 0.5-5mL/min; the stirring speed is 100-300rpm, and the stirring time is 2-10h; preferably, the dropping rate is 2mL/min, and the stirring speed is 200rpm; the stirring time was 6h.
A bentonite composition having sun-screening and repairing effects prepared by the above method.
The bentonite composition with sun protection and repair effects is applied to the field of cosmetics, and particularly to the preparation of cosmetics with sun protection effects.
The bentonite composition with sun protection and repair effects can be used in an amount of 0.1-30% by mass percent in cosmetics.
Compared with the prior art, the invention has the following advantages:
(1) The bentonite composition with sun-proof and repairing effects is prepared by a specific process, and the synergistic effect of bentonite, tremella solution and ethyl diiminomethyl guaiacol manganese chloride in the composition enables the prepared composition to have good sun-proof and repairing effects.
(2) The tremella solution in the bentonite composition with sun-proof and repairing effects can avoid agglomeration of bentonite and improve the stability of the bentonite composition while enhancing the sun-proof and repairing effects of the composition.
(3) When the bentonite composition with sun-screening and repairing effects prepared by the method is applied to cosmetics, the bentonite composition not only has good sun-screening effect, but also has better sun-screening effect than the sun-screening milk obtained by the method. In addition, when the bentonite composition with sun protection and repair effects is applied to sun protection milk, normal metabolism of skin epidermal cells is not affected, after the sun protection milk is used, the percutaneous moisture loss value of skin is reduced, the evaporation of the moisture of the skin is reduced, and the epidermal barrier function is enhanced.
(4) The bentonite composition with sun protection and repair effects has simple preparation process and is suitable for industrial production.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The bacillus used in the invention is BNCC221996 bacillus and is purchased from Beijing North Innovative biological technology institute.
The nutrient gravy culture medium used in the invention is a common nutrient gravy culture medium in the prior art, and the preparation method comprises (taking preparation of 1L as an example): beef extract 3.0g, peptone 10.0g, naCl 5.0g, distilled water added to the culture medium volume of 1L, mixing uniformly, sterilizing at 121deg.C for 15min, and cooling.
The percentages appearing in the examples, unless explicitly indicated, refer to mass percent.
Example 1
The natural bentonite is crushed and ground by a ball mill to obtain bentonite with the particle size of 3 mu m, 10g of bentonite with the particle size of 3 mu m is added into 45g of deionized water, and the bentonite is dispersed for 40min at 7000rpm by a high-shear homogenizing emulsifying machine to obtain bentonite dispersion liquid. And (3) dripping 12g of tremella fermentation liquor into the bentonite dispersion liquor at a dripping rate of 2mL/min at uniform speed, stirring for 6h to a viscous liquid at a rotating speed of 350rpm under a water bath condition at 60 ℃ after the dripping is finished, and cooling to 25 ℃ to obtain a mixed dispersion liquor. 1g of ethyl bis iminomethyl guaiacol manganese chloride was added to 32g of butanediol, and stirred at a rotation speed of 200rpm and 25℃for 3 hours to obtain an ethyl bis iminomethyl guaiacol manganese chloride alcoholic solution. And (3) dripping the ethyl diiminomethyl guaiacol manganese chloride alcohol solution into the mixed dispersion at a dripping rate of 2mL/min, and stirring for 6 hours at the rotating speed of 200rpm and at the temperature of 25 ℃ after the dripping is finished to obtain the bentonite composition with sun-proof and repairing effects.
The preparation method of the tremella fermentation liquid comprises the following steps:
(1) Inoculating Bacillus to nutrient broth culture medium via inoculating loop, and culturing at 30deg.C for 24 hr to obtain strain with concentration of about 10 8 cfu/mL of bacillus seed solution.
(2) Mixing 1% dry tremella powder, 2% glucose, 1% ammonium chloride, 1% soybean peptone and 95% water uniformly, sterilizing at 121deg.C for 20min to obtain tremella culture medium.
(3) Inoculating the bacillus seed liquid into a tremella culture medium, culturing for 48 hours at 30 ℃, and filtering by a diatomite filter to obtain tremella fermentation broth.
Example 2
The bentonite composition having sun-screening and repairing effects was obtained by changing 10g of bentonite of 3 μm in example 1 to bentonite of 6g of 3 μm in mass and properly adjusting the mass of deionized water to 49g so that the total mass was 100g and the rest was unchanged.
Example 3
The bentonite composition having sun-screening and repairing effects was obtained by changing 10g of bentonite of 3 μm in example 1 to 15g of bentonite of 3 μm and properly adjusting the mass of deionized water to 40g so that the total mass was 100g, and the rest was unchanged.
Example 4
12g of tremella fermentation broth in example 1 is changed into 12g of tremella extract, and the rest is unchanged, so that the bentonite composition with sun protection and repair effects is obtained.
The preparation method of the tremella extract comprises the following steps:
10g of dry tremella powder is added into 100g of deionized water, and is leached for 3 hours at 70 ℃, and the filtrate obtained after filtration is tremella extract.
Example 5
12g of tremella fermentation liquor in example 1 is changed into 12g of tremella polysaccharide solution with mass fraction of 1% (the molecular weight of tremella polysaccharide is 500000-1500000 Da), and the rest is unchanged, so that the bentonite composition with sun-screening and repairing effects is obtained.
Example 6
The mass of deionized water was properly adjusted to 49g by changing the tremella fermentation broth of 12g in example 1 to the tremella fermentation broth of 8g so that the total mass was 100g, and the rest was unchanged, to obtain a bentonite composition with sun-screening and repairing effects.
Example 7
The white fungus fermentation broth of 12g in example 1 was changed to the white fungus fermentation broth of 16g, and the mass of deionized water was properly adjusted to 41g so that the total mass was 100g, and the rest was unchanged, to obtain a bentonite composition having sun-screening and repairing effects.
Example 8
1g of ethyl bis iminomethyl guaiacol manganese chloride in example 1 was changed to 0.5g of ethyl bis iminomethyl guaiacol manganese chloride, and the mass of deionized water was appropriately adjusted to 45.5g so that the total mass was 100g, and the balance was unchanged, to obtain a bentonite composition having sun-screening and repairing effects.
Example 9
1g of ethyl bis iminomethyl guaiacol manganese chloride in example 1 was changed to 2g of ethyl bis iminomethyl guaiacol manganese chloride, and the mass of deionized water was appropriately adjusted to 44g so that the total mass was 100g, and the balance was unchanged, to obtain a bentonite composition having sun-screening and repairing effects.
Example 10
The natural bentonite is crushed and ground by a ball mill to obtain bentonite with the particle size of 5 mu m, 8g of bentonite with the particle size of 5 mu m is added into 51.2g of deionized water, and the bentonite is dispersed for 60min at 5000rpm by a high-shear homogenizing emulsifying machine to obtain bentonite dispersion. And (3) dropwise adding 10g of tremella fermentation liquor into the bentonite dispersion liquor at a dropwise adding rate of 0.5mL/min at an average speed, stirring at a water bath condition of 50 ℃ for 2 hours at a rotating speed of 500rpm to obtain a viscous liquid, and cooling to 25 ℃ to obtain a mixed dispersion liquor. 0.8g of ethyl bis iminomethyl guaiacol manganese chloride was added to 30g of butanetriol and stirred at a rotation speed of 100rpm and 20℃for 10 hours to obtain an ethyl bis iminomethyl guaiacol manganese chloride alcoholic solution. And (3) dripping the ethyl diiminomethyl guaiacol manganese chloride alcohol solution into the mixed dispersion at a dripping rate of 5mL/min at uniform speed, and stirring for 10 hours at a rotating speed of 100rpm and a temperature of 20 ℃ after the dripping is finished to obtain the bentonite composition with sun protection and repair effects.
The preparation method of the tremella fermentation broth in this embodiment is the same as that in embodiment 1.
Example 11
The natural bentonite is crushed and ground by a ball mill to obtain bentonite with the particle size of 8 mu m, 10g of bentonite with the particle size of 8 mu m is added into 39.8g of deionized water, and the bentonite is dispersed for 20min at 8000rpm by a high-shear homogenizing emulsifying machine to obtain bentonite dispersion. And (3) dripping 14g of tremella fermentation liquor into the bentonite dispersion liquor at a dripping rate of 5mL/min at uniform speed, stirring the tremella fermentation liquor for 10h to a viscous liquid at a rotating speed of 150rpm under a water bath condition at 80 ℃ after the dripping is finished, and cooling the mixed dispersion liquor to 25 ℃ to obtain the mixed dispersion liquor. 1.2g of ethyl bis iminomethyl guaiacol manganese chloride was added to 35g of sorbitol and stirred at a rotation speed of 300rpm at 35℃for 2 hours to obtain an ethyl bis iminomethyl guaiacol manganese chloride alcoholic solution. And (3) dripping the ethyl diiminomethyl guaiacol manganese chloride alcohol solution into the mixed dispersion at a dripping rate of 3mL/min, and stirring for 2 hours at the rotating speed of 300rpm and the temperature of 35 ℃ after the dripping is finished to obtain the bentonite composition with sun protection and repair effects.
Comparative example 1
And (3) dropwise adding 20g of tremella fermentation liquor into 45g of deionized water at a dropwise adding rate of 2mL/min at uniform speed, stirring at a rotating speed of 350rpm for 6h under a water bath condition at 60 ℃ until the thick liquid is obtained after the dropwise adding, and cooling to 25 ℃ to obtain a mixed solution. 3g of ethyl bis iminomethyl guaiacol manganese chloride was added to 32g of butanediol, and stirred at a rotation speed of 200rpm and 25℃for 3 hours to obtain an ethyl bis iminomethyl guaiacol manganese chloride alcoholic solution. And (3) dripping the ethyl diiminomethyl guaiacol manganese chloride alcohol solution into the mixed solution at a dripping rate of 2mL/min at an average speed, and stirring for 6 hours at the rotating speed of 200rpm and the temperature of 25 ℃ after the dripping is finished to obtain the composition.
The tremella fermentation broth of comparative example 1 was prepared in the same manner as in example 1. Comparative example 1 differs from example 1 in that comparative example 1 replaces 10g of bentonite in example 1 with 8g of tremella fermentation broth and 2g of ethyl bis iminomethyl guaiacol manganese chloride.
The total mass of tremella fermentation broth and ethyl bis iminomethyl guaiacol manganese chloride in comparative example 1 was the same as the total mass of bentonite, tremella fermentation broth and ethyl bis iminomethyl guaiacol manganese chloride in example 1.
Comparative example 2
The natural bentonite is crushed and ground by a ball mill to obtain bentonite with the particle size of 3 mu m, 20g of bentonite with the particle size of 3 mu m is added into 45g of deionized water, and the bentonite is dispersed for 40min at 7000rpm by a high-shear homogenizing emulsifying machine to obtain bentonite dispersion liquid. 3g of ethyl bis iminomethyl guaiacol manganese chloride was added to 32g of butanediol, and stirred at a rotation speed of 200rpm and 25℃for 3 hours to obtain an ethyl bis iminomethyl guaiacol manganese chloride alcoholic solution. And (3) dripping the ethyl diiminomethyl guaiacol manganese chloride alcohol solution into the bentonite dispersion liquid at a dripping rate of 2mL/min at an average speed, and stirring for 6 hours at the rotating speed of 200rpm and the temperature of 25 ℃ after the dripping is finished to obtain the composition.
Comparative example 2 differs from example 1 in that 10g of bentonite and 2g of ethyldiiminomethyl guaiacol manganese chloride were used in comparative example 2 instead of 12g of tremella fermentation broth in example 1.
The total mass of bentonite and ethyldiiminomethyl guaiacol manganese chloride in comparative example 2 was the same as the total mass of bentonite, tremella fermentation broth and ethyldiiminomethyl guaiacol manganese chloride in example 1.
Comparative example 3
The natural bentonite is crushed and ground by a ball mill to obtain bentonite with the particle size of 3 mu m, 10.5g of bentonite is added into 45g of deionized water, and the bentonite is dispersed for 40min at 7000rpm by a high-shear homogenizing emulsifying machine to obtain bentonite dispersion. And (3) dripping 12.5g of tremella fermentation liquor into the bentonite dispersion liquor at a dripping rate of 2mL/min at an average speed, stirring for 6h to a viscous liquid at a rotating speed of 350rpm under a water bath condition at 60 ℃ after the dripping is finished, and cooling to 25 ℃ to obtain a mixed dispersion liquor. 32g of butanediol was stirred at 200rpm and 25℃for 3 hours, and the butanediol solution was added dropwise to the mixed dispersion at a dropping rate of 2mL/min at a uniform rate, and after the completion of the addition, stirring was maintained at 200rpm and 25℃for 6 hours to obtain a composition.
The preparation method of the tremella fermentation broth is the same as in example 1.
Comparative example 3 differs from example 1 in that comparative example 3 replaces 1g of ethyl bis iminomethyl guaiacol manganese chloride in example 1 with 0.5g of bentonite and 0.5g of tremella fermentation broth.
The total mass of bentonite and tremella fermentation broth in comparative example 3 was the same as the total mass of bentonite, tremella fermentation broth and ethylbis iminomethyl guaiacol manganese chloride in example 1.
Comparative example 4
The natural bentonite is crushed and ground by a ball mill to obtain bentonite with the particle size of 3 mu m, 23g of bentonite with the particle size of 3 mu m is added into 45g of deionized water, and the bentonite is dispersed for 40min at 7000rpm by a high-shear homogenizing emulsifying machine to obtain bentonite dispersion liquid. 32g of butanediol was added dropwise to the bentonite dispersion at an average rate of 2mL/min, and stirring was maintained at a rotation speed of 200rpm at 25℃for 6 hours to obtain a composition.
Comparative example 4 differs from example 1 in that comparative example 4 replaces 12g of tremella fermentation broth and 1g of ethylbis iminomethyl guaiacol manganese chloride in example 1 with 13g of bentonite.
The mass of bentonite in comparative example 4 was the same as the total mass of bentonite, tremella fermentation broth and ethyldiiminomethyl guaiacol manganese chloride in example 1.
Comparative example 5
23g of tremella fermentation liquor is added into 45g of deionized water at a dropping rate of 2mL/min at a uniform speed, after the dropping is finished, the tremella fermentation liquor is stirred for 6h to a viscous liquid at a rotating speed of 350rpm under a water bath condition at 60 ℃, and the mixed liquor is obtained after cooling to 25 ℃. 32g of butanediol was added to the mixed solution at a dropping rate of 2mL/min at an average rate, and after the completion of the dropping, the mixture was stirred at a rotation speed of 200rpm at 25℃for 6 hours to obtain a composition.
The preparation method of the tremella fermentation broth is the same as in example 1.
Comparative example 5 differs from example 1 in that comparative example 5 replaces 10g bentonite and 1g ethylbis iminomethyl guaiacol manganese chloride of example 1 with 11g tremella fermentation broth.
The mass of bentonite in comparative example 5 was the same as the total mass of bentonite, tremella fermentation broth and ethyldiiminomethyl guaiacol manganese chloride in example 1.
Comparative example 6
15g of ethyl bis iminomethyl guaiacol manganese chloride was added to 32g of butanediol, and stirred at a rotation speed of 200rpm and 25℃for 3 hours to obtain an ethyl bis iminomethyl guaiacol manganese chloride alcoholic solution. The ethyl bis iminomethyl guaiacol manganese chloride alcohol solution is added into 53g of deionized water at a dropping rate of 2mL/min at a uniform speed, and after the dropping is completed, the mixture is kept stirring for 6 hours at a rotating speed of 200rpm and a temperature of 25 ℃ to obtain a composition.
The maximum amount of manganese chloride of ethyldiiminomethyl guaiacol added was 15g. When the content of the manganese chloride of the ethyldiiminomethyl guaiacol exceeds 15g, the obtained composition is a turbid liquid and has a layering phenomenon, and an efficacy test experiment cannot be performed.
In comparison with example 1, comparative example 6 does not add bentonite and tremella broth.
Comparative example 7
The natural bentonite is crushed and ground by a ball mill to obtain bentonite with the particle size of 3 mu m, 10g of bentonite with the particle size of 3 mu m, 45g of deionized water, 12g of tremella fermentation liquor, 1g of ethyl bis iminomethyl guaiacol manganese chloride and 32g of butanediol are uniformly mixed to obtain the composition.
Comparative example 7 differs from example 1 in that comparative example 7 was obtained by directly mixing bentonite, tremella fermentation broth, ethyl bis iminomethyl guaiacol manganese chloride and butanediol without using a process.
Comparative example 8
10g of 3 μm bentonite in example 1 was changed to 4g of 3 μm bentonite, and the mass of deionized water was appropriately adjusted to 51g so that the total mass was 100g, and the rest was unchanged, to obtain a composition.
Comparative example 9
10g of 3 μm bentonite in example 1 was changed to 18g of 3 μm bentonite, and the mass of deionized water was appropriately adjusted to 37g so that the total mass was 100g, and the rest was unchanged, to obtain a composition.
Comparative example 10
Titanium dioxide was pulverized and ground by a ball mill to obtain titanium dioxide having a particle size of 3. Mu.m.
10g of 3 μm bentonite in example 1 was replaced with 10g of 3 μm titanium dioxide, the remainder being unchanged, to obtain a composition.
Comparative example 11 (Aloe extract instead of Tremella fermentation broth)
The tremella fermentation broth of example 1 with a mass of 12g was changed to aloe extract with a mass of 12g, and the rest was unchanged, to obtain a composition.
Comparative example 11 differs from example 1 in that comparative example 11 uses aloe extract instead of tremella fermentation broth to obtain a composition.
The preparation method of the aloe extract comprises the following steps:
selecting fresh aloe vera, cleaning, peeling, and sterilizing under 60W ultraviolet lamp for 30min; cutting the sterilized aloe mesophyll into small pieces, crushing and squeezing according to the mass ratio of the aloe mesophyll to deionized water of 1:2 to obtain a crude aloe extract; filtering the crude aloe extract for 3 times, stirring with 2% active carbon powder for 8 hr, decolorizing, and removing active carbon to obtain aloe extract.
Comparative example 12
1g of ethyl bis iminomethyl guaiacol manganese chloride in example 1 was changed to 1g of vitamin C, and the rest was unchanged, to obtain a composition.
Comparative example 12 differs from example 1 in that comparative example 12 uses vitamin C instead of ethyldiiminomethyl guaiacol manganese chloride to obtain a composition.
Comparative example 13 (substitution of 1, 3-propanediol for butanediol)
The composition was obtained by changing 32g of butanediol in example 1 to 32g of 1, 3-propanediol and the remainder unchanged.
Comparative example 13 differs from example 1 in that comparative example 13 uses 1, 3-propanediol instead of butanediol to obtain a composition.
Test example 1 storage stability test
After the samples of examples 1 to 11 and comparative examples 1 to 13 were left to stand at room temperature for one month, two months and three months, the appearance state and smell of the samples were observed, respectively, and the storage stability of the samples was tested.
TABLE 1 storage stability test results for samples (at room temperature) of examples 1-11 and comparative examples 1-13
Comparative example 1 and comparative examples 1 to 6 show that the addition of bentonite, tremella fermentation broth and ethylbis iminomethyl guaiacol manganese chloride plays a very important role in the stability of the composition. The stability of the obtained product is poor because the composition is prepared by lacking one or only one of bentonite, tremella fermentation broth or ethyl diiminomethyl guaiacol manganese chloride.
Comparative examples 1 and 7 show that the preparation process has a great influence on the stability of the composition, and that comparative example 7 directly mixes the respective substances in the composition, and the resulting composition is not a clear liquid but a slightly cloudy state after the preparation is completed. Furthermore, the composition of comparative example 7 was not only cloudy after 1-3 months of standing, but also was very unstable with the generation of a rancid taste.
Comparative examples 1-3 and comparative examples 8-9 show that the addition of bentonite in the composition affects the stability of the final product. Under three months of stability investigation, the product exhibited a clear appearance at room temperature with no obvious odor change. When the addition amount of bentonite is 4% and 18%, the appearance of the product is turbid liquid under the investigation of three months stability, and the product has a harshness taste and poor stability. Therefore, the addition amount of the bentonite selected by the invention is 6-15%.
Comparative examples 1 and comparative examples 10 to 13 show that the dispersibility of titanium dioxide is inferior to bentonite, compared to the use of titanium dioxide (comparative example 10), aloe extract (comparative example 11), vitamin C (comparative example 12) and 1, 3-propanediol (comparative example 13) instead of the corresponding components in the bentonite composition having sun protection and repair effects; the viscosity and film forming property of aloe extract are different from those of tremella solution; vitamin C has poor stability and oxidation resistance is easy to decay, so that the composition prepared by taking the substances as active components has poor stability. In the embodiment 1 of the invention, bentonite, tremella fermentation broth and ethyl bis (iminomethyl) guaiacol manganese chloride are adopted to interact, butanediol is used for dissolving the ethyl bis (iminomethyl) guaiacol manganese chloride to prepare an alcohol solution, and the finally prepared composition with sun protection and repair effects has the best stability.
Test example 2-sun protection index SPF value test:
the SPF value test samples of the sun protection index are examples 1-11 and comparative examples 1-13, the test method adopts a human body efficacy evaluation test, and the detection index is the SPF value of the sun protection index. The test subjects were 270 men or women with healthy, insensitive skin aged 18-50 years, with a 1:1 ratio of men to women, no obvious injury to the test site, no recent medication or cosmetic treatment, and no recent administration of hormonal medications. The experimenters were randomly divided into 27 groups of 10 persons each. The test environment is 20-22 ℃,40% -60% RH.
Test sample: examples 1 to 11, comparative examples 1 to 13, and commercial sun-block emulsions (Mistine brand small yellow cap sun-block), wherein the formulations of the sun-block emulsions, titanium dioxide sun-block emulsions, and blank sun-block emulsions prepared in examples 1 to 11, comparative examples 1 to 13 are shown in Table 2 below:
table 2 formulations of examples 1 to 11, and comparative examples 1 to 13, as well as of sun-block emulsions, titanium dioxide sun-block emulsions, and blank sun-block emulsions
Examples 1-11, comparative examples 1-13 were prepared as follows:
(1) Prefabricating phase A: adding the components except water in the phase A into water, heating to 85 ℃, homogenizing at 8000rpm until the components are uniformly dispersed to obtain a mixed solution 1, and preserving heat for later use;
(2) Adding the B phase component into the mixed solution 1, stirring at 1000rpm until the B phase component is completely dissolved, and preserving heat for 30 minutes to obtain a mixed solution 2, and preserving heat for later use;
(3) Prefabricating phase C: homogenizing the components of the phase C at 8000rpm, and uniformly dispersing the components to obtain a mixed solution 3 for later use;
(4) Adding the components of the D phase into the mixed solution 3, stirring at 1000rpm until the components of the D phase are completely dissolved, adding the components of the E phase, stirring at 1000rpm until the components of the E phase are completely dissolved, obtaining a mixed solution 4, heating to 85 ℃, and preserving heat for later use;
(5) Adding the mixed solution 4 into the mixed solution 2, homogenizing and emulsifying for 10min at 5000rpm, cooling to 70 ℃, adding the F phase component, stirring at 1000rpm, and mixing uniformly to obtain a mixed solution 5;
(6) And cooling the mixed solution 5 to 60 ℃, adding the G-phase material which is dissolved uniformly in advance, stirring uniformly at 1000rpm, and cooling to room temperature to obtain the sun-proof emulsion.
The test steps are as follows:
(1) Test instrument: SIV 6500 type SPF IN VIVO multiband solar protection coefficient human body measurement system;
(2) The subject's minimal erythema dose MED is predicted. Minimum Erythema Dose (MED): causing a clearly visible erythema of the skin in the range of the minimum dose (J/m) or minimum time (seconds) of uv irradiation required to irradiate a large part of the area of the spot.
a. The coating area of the sample is not less than 30cm 2 。
b. Sample amount and coating method: according to (2.00+/-0.05) mg/cm 2 The amount of the sample is weighed, and the latex finger stall is used for uniformly coating the sample in a test area for 15-30 minutes.
c. Predicting the MED of the subject: an irradiation area was selected on the skin of the back of the subject, and the results were observed after 24 hours by irradiating 6 spots with different doses of ultraviolet rays. The MED of the normal skin of the subject is taken as the lowest irradiation dose or the shortest irradiation time at which the erythema appears on the skin.
(3) Test of SPF value
Selecting two irradiation areas on the skin of the back of the subject, wherein one is a negative control area, namely an unprotected skin area; one is the sample area. The two areas are irradiated on the same day, and the MED value selected by irradiation is the predicted MED value. The shortest irradiation time for erythema of the skin was recorded as MED results for this area of normal skin of the subject.
( Remarks: SPF value: the solar protection factor, the factor after the SPF value, refers to a time frame in which the irradiation of ultraviolet rays does not harm the skin. )
(4) SPF value calculation
Individual SPF value = sample guard skin MED/negative control guard skin MED
Sample SPF value = sum of all individual SPF values/sample size
Wherein, the higher the SPF value, the better the sun-proof effect
TABLE 3 results of SPF value test of sun protection index of application examples 1 to 11, application comparative examples 1 to 13, titanium dioxide sun protection milk, blank sun protection milk, commercially available sun protection milk (Mistine brand small yellow cap sun protection milk)
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From the above results, it is understood that the compositions prepared in examples 1 to 11 and comparative examples 1 to 13 each have a sunscreen effect. The sun protection effect of the sun protection emulsions of examples 1 to 11 was superior to that of the sun protection emulsions of comparative examples 1 to 13, and the sun protection effect of the sun protection emulsions of examples 1 to 11 was superior to that of commercially available sun protection emulsions.
Comparative examples 1 and comparative examples 1 to 6 show that the bentonite composition with sun protection and repair effects finally prepared by using bentonite, tremella fermentation broth and ethylbis iminomethyl guaiacol manganese chloride as the active material in example 1 of the present invention has a higher SPF value than the composition lacking one of bentonite (comparative example 1), tremella fermentation broth (comparative example 2) or ethylbis iminomethyl guaiacol manganese chloride (comparative example 3), or using one of bentonite alone (comparative example 4), tremella fermentation broth (comparative example 5) or ethylbis iminomethyl guaiacol manganese chloride (comparative example 6) as the active material.
As is clear from comparative examples 1 and 7, the components of the bentonite composition were directly mixed, bentonite and ethyl bis iminomethyl guaiacol manganese chloride could not be well dispersed, and the tremella fermentation broth could not well exert its film forming effect, resulting in poor sun screening effect of the final product.
Comparative examples 1 and comparative examples 10 to 12 show that the composition prepared by using bentonite, tremella fermentation broth and ethyldiiminomethyl guaiacol manganese chloride in example 1 of the present application has a better sun-screening effect than zinc oxide (comparative example 10), aloe extract (comparative example 11) and vitamin C (comparative example 12) instead of the corresponding components in the bentonite composition.
Comparative examples 1 to 3 and comparative examples 8 to 9 show that the addition amount of bentonite varies among the compositions, and the finally produced compositions having sun protection and repair effects vary in sun protection performance. With the increase of the addition amount of bentonite, the SPF value of the sun protection index of the product is firstly increased and then decreased. When the addition amount of bentonite is 10%, the sun protection index SPF value of the product is highest. When the addition amount of bentonite is 4% or 18%, the SPF value of the sun protection index is not as good as that of the bentonite when the addition amount is 6-15%. Therefore, the bentonite selected in the present application is added in an amount of 6 to 15%, with an addition amount of 10% being preferred (example 1).
Comparative examples 1 and examples 4 to 5 show that the types of tremella solutions in the bentonite compositions having sun-screening and repairing effects are different, and the finally prepared compositions having sun-screening and repairing effects are different in sun-screening performance. In examples 1, 4 and 5, the tremella solutions in the bentonite composition with sun protection and repair effects are respectively tremella fermentation liquor, tremella extract and tremella polysaccharide powder dissolved in water, and the results show that the sun protection index SPF value of the product of example 1 is the highest. Therefore, in the application, the tremella fermentation broth is selected as the tremella solution, and the finally prepared composition with sun protection and repair effects has the best sun protection performance (example 1).
As is clear from comparative examples 1, 6 and 7, the addition amounts of the tremella solution in the bentonite compositions having the sun-screening and repairing effects are different, and the finally prepared compositions having the sun-screening and repairing effects are different in sun-screening performance. With the increase of the addition amount of the tremella fermentation liquid, the SPF value of the sun protection index of the product is firstly increased and then decreased. When the addition amount of the tremella fermentation liquid is 12%, the sun protection index SPF value of the product is highest.
Comparative examples 1, 8 and 9 show that the addition of manganese ethyldiiminomethyl guaiacol chloride in bentonite compositions having sunscreen and repair effects affects the sunscreen performance of the final product. With the increase of the addition amount of the manganese chloride of the ethyldiiminomethyl guaiacol, the SPF value of the sun protection index of the product is firstly increased and then decreased. When the addition amount of the manganese chloride of the ethyldiiminomethyl guaiacol is 1 percent, the sun protection index SPF value of the product is the highest.
Test example 3 repair test
The repair test sample comprises the following components: same test example 2
The test method adopts a human body efficacy evaluation experiment, and the detection index is the percutaneous water loss value. The test subjects were 270 healthy men or women aged 18-45 years, with a ratio of 1:1, no obvious injury, no recent medication or cosmetic treatment, and no recent administration of hormonal medications. The group-entering screening standard is that the percutaneous water loss value of the face is not less than 15 g/(hm) 2 ) Qualified subjects were randomized into 27 groups of 10 persons each. The test environment is 20-22 ℃,40% -60% RH.
The test steps are as follows:
(1) The subject's face was not able to use any product (including cosmetics or topical medicines) 2 days prior to testing, and the subject did not apply any product to the face test area prior to testing. The subjects cleaned their faces with a unified cleanser as required, gently wiped dry with dry facial tissues, and rested for 30min in the test environment.
(2) The percutaneous water loss values of the left and right faces of the face of the subject were measured, and the data were recorded.
(3) The subjects pick up the product and use the samples continuously for 4 weeks as required, and the using method is as follows: after the skin care step is finished, a coin-sized sample is taken and uniformly smeared on the whole face. Once daily in the morning for 4 weeks.
(4) Return visit 4 weeks after sample use: the percutaneous water loss values of the left and right faces of the face were measured, and the data were recorded.
(5) Analysis of results: data are recorded in the form of (face left, right face average); comparing the change in the percutaneous moisture loss value before and after using the sample; the change of the percutaneous moisture loss of the used sample and the blank sun block is compared, and the smaller the percutaneous moisture loss is, the better the skin repairing effect is.
Difference = 4 week average used-average before use
Rate of change = (4 week average used-average before use)/average before use 100%
TABLE 4 repair test results for application examples 1-11, application comparative examples 1-13 samples and blank sunscreens
Comparative examples 1 to 3 and comparative examples 8 to 9 show that the addition amount of bentonite varies among the compositions, and the finally produced compositions having sunscreen and repair effects vary in repair properties. As the addition amount of bentonite increases, the repair ability of the bentonite composition having sun protection and repair effects increases and then decreases. When the addition amount of bentonite is 10%, the repairing effect of the bentonite composition having sun-screening and repairing effects is best. When the addition amount of bentonite is 4% or 18%, the repairing effect is inferior to that when the addition amount is 6-15%. Therefore, the bentonite selected in the present invention is added in an amount of 6 to 15%, with an addition amount of 10% being preferred (example 1).
Comparative examples 1 and examples 4 to 5 show that the types of tremella solutions in the bentonite compositions having sun-screening and repairing effects are different, and the finally prepared compositions having sun-screening and repairing effects are different in repairing performance. In examples 1, 4 and 5, the tremella solutions in the compositions are respectively tremella fermentation broth, tremella extract and tremella polysaccharide powder dissolved in water, and the results show that the bentonite composition with sun protection and repair effects in example 1 has the best repair effect. Therefore, in the invention, the tremella solution is selected from tremella fermentation broth, and the composition with sun protection and repair effects finally prepared has the best repair performance (example 1).
As can be seen from comparative examples 1, 6 and 7, the tremella solution added amounts in the compositions were different, and the finally prepared compositions having sun protection and repair effects were different in repair performance. With the increase of the addition amount of the tremella fermentation broth, the repairing capability of the bentonite composition with sun protection and repairing effects is improved and then reduced. When the addition amount of the tremella fermentation liquor is 12%, the bentonite composition with sun protection and repair effects has the best repair effect.
Comparative examples 1, 8 and 9 show that the amount of manganese chloride ethyl bis iminomethyl guaiacol added to the composition affects the repair performance of the bentonite composition having the final sunscreen and repair effects. As the addition amount of the manganese chloride of ethyldiiminomethyl guaiacol increases, the repairing ability of the bentonite composition having sun protection and repairing effects increases and then decreases. When the addition amount of the manganese chloride of ethyldiiminomethyl guaiacol is 1%, the bentonite composition having sun protection and repair effects has the best repair effect.
As is clear from comparative examples 1 and comparative examples 1 to 6, the composition having sun-screening and repairing effects finally prepared by using bentonite, tremella fermentation broth, and ethylbis iminomethyl guaiacol manganese chloride as the active material in example 1 of the present application is better in repairing effect than the composition lacking one of bentonite (comparative example 1), tremella fermentation broth (comparative example 2), and ethylbis iminomethyl guaiacol manganese chloride (comparative example 3), or using bentonite (comparative example 4), tremella fermentation broth (comparative example 5), or ethylbis iminomethyl guaiacol manganese chloride alone (comparative example 6, ethylbis iminomethyl guaiacol manganese chloride is excessively added, and cytotoxicity is too great).
Comparative examples 1 and 7 show that the compositions prepared by direct material mixing have poor repairing effect compared with those prepared by the non-process.
Comparative example 1, comparative example 10, comparative example 11, comparative example 12 and comparative example 13 are shown. Compared with zinc oxide (comparative example 10), aloe extract (comparative example 11), vitamin C (comparative example 12) and 1, 3-propanediol (comparative example 13), bentonite, tremella fermentation broth and ethyl bis iminomethyl guaiacol manganese chloride are adopted to interact in the embodiment 1 of the application, and butanediol is used for dissolving the ethyl bis iminomethyl guaiacol manganese chloride to prepare an alcohol solution, so that the composition with sun protection and repair effects is prepared finally, and the repair effect is better.
Compared with deionized water, the composition with sun protection and repair effects prepared finally in the embodiment 1 of the application is better in repair effect by adopting interaction of bentonite, tremella fermentation broth and ethyl diiminomethyl guaiacol manganese chloride as compared with the blank sun protection emulsion matrix in the embodiment 1 of the application.
The above examples are preferred embodiments of the present application, but the embodiments of the present application are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present application should be made in the equivalent manner, and the embodiments are included in the protection scope of the present application.
Claims (10)
1. A method for preparing a bentonite composition with sun protection and repair effects, which is characterized by comprising the following steps:
(1) Adding bentonite into water, and uniformly dispersing to obtain bentonite dispersion liquid;
(2) Adding the tremella solution into the bentonite dispersion liquid, heating and stirring to obtain a viscous liquid to obtain a mixed dispersion liquid;
(3) Adding the ethyl bis (iminomethyl) guaiacol manganese chloride into the polyalcohol, and uniformly mixing to obtain an ethyl bis (iminomethyl) guaiacol manganese chloride solution;
(4) And (3) adding the ethyl diiminomethyl guaiacol manganese chloride solution into the mixed dispersion liquid in the step (2), and uniformly stirring to obtain the bentonite composition with sun protection and repair effects.
2. The method for preparing a bentonite composition having sun protection and repair effects according to claim 1, wherein:
the mass percentage of the bentonite in the step (1) in the bentonite composition with sun protection and repair effects is 6-15%;
the mass percentage of the water in the step (1) in the bentonite composition with sun protection and repair effects is 20-60%;
the mass percentage of the tremella solution in the bentonite composition with sun protection and repair effects in the step (2) is 8-16%;
The mass percentage of the ethyl bis iminomethyl guaiacol manganese chloride in the bentonite composition with sun protection and repair effects in the step (3) is 0.5-2%;
the mass percentage of the polyol in the step (3) in the bentonite composition with sun protection and repair effects is 20-50%.
3. The method for preparing a bentonite composition having sun protection and repair effects according to claim 1, wherein:
the particle size of the bentonite in the step (1) is 2-8 mu m.
4. The method for preparing a bentonite composition having sun protection and repair effects according to claim 1, wherein:
the tremella solution in the step (2) is at least one of tremella extract, tremella fermentation liquor and tremella polysaccharide solution.
5. The method for preparing a bentonite composition having sun protection and repair effect according to claim 4, wherein:
the preparation method of the tremella extract comprises the following steps: mixing the dry tremella powder with water, leaching, and filtering to obtain tremella extract;
the preparation method of the tremella fermentation liquid comprises the following steps: adding bacillus seed liquid into a tremella fermentation medium, fermenting and culturing, and filtering to obtain tremella fermentation liquid;
The tremella polysaccharide solution is 0.5-3% tremella polysaccharide solution by mass fraction.
6. The method for preparing a bentonite composition having sun protection and repair effect according to claim 5, wherein:
in the preparation method of the tremella extract, the mass ratio of the dry tremella powder to the water is 1:5-15, the leaching temperature is 50-90 ℃, and the leaching time is 1-6h;
in the preparation method of the tremella fermentation liquid, the concentration of the bacillus seed liquid is 10 7 -10 9 cfu/mL; the tremella fermentation medium comprises 0.5-2% of dry tremella powder, 1-3% of glucose, 0.5-2% of ammonium chloride, 0.5-2% of soybean peptone and the balance of water; the fermentation temperature is 28-33 ℃, and the fermentation time is 36-60h.
7. The method for preparing a bentonite composition having sun protection and repair effects according to claim 1, wherein:
the polyalcohol in the step (3) is at least one of butanediol, butanetriol, pentaerythritol, hexanediol, sorbitol and xylitol; butanediol is preferred.
8. The method for preparing a bentonite composition having sun protection and repair effects according to claim 1, wherein:
the operation of uniform dispersion in the step (1) is shearing and homogenizing treatment, wherein the rotating speed of the shearing and homogenizing treatment is 5000-8000rpm, and the time of the shearing and homogenizing treatment is 20-60min;
The temperature of heating and stirring in the step (2) is 50-80 ℃, the time of heating and stirring is 2-10h, and the adding speed of the tremella solution is 0.5-5mL/min;
the step (3) of uniformly mixing is that stirring is uniformly carried out, the stirring temperature is 20-35 ℃, the stirring speed is 100-300rpm, and the stirring time is 2-10h;
the step (4) is characterized in that the adding of the ethyl bis iminomethyl guaiacol manganese chloride solution is dropwise adding, the dropwise adding rate is 0.5-5mL/min, and the stirring time is 2-10h.
9. A bentonite composition having sun protection and repair efficacy prepared according to the method of any one of claims 1-8.
10. Use of a bentonite composition with sun protection and repair effects according to claim 9 in the field of cosmetics, in particular in the preparation of cosmetics with sun protection effects.
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