A method for preparing a sunscreen agent using attapulgite as a carrier and the sunscreen agent

Abstract

The present invention provides a method for preparing a sunscreen with attapulgite as a carrier and the sunscreen. The sunscreen with attapulgite as a carrier consists of a sunscreen, attapulgite, a modifier and a connector. The preparation method of the present invention makes full use of the advantages of attapulgite, which is abundant in reserves, cheap and easy to obtain, safe and non-toxic, and large in specific surface area and pore volume. The natural mineral attapulgite is used as a carrier, and the sunscreen is loaded in the pores of the attapulgite or fixed on the outer surface, thereby improving the dispersibility and stability of the sunscreen, reducing the irritation of the sunscreen, improving its safety, and improving the quality of the sunscreen. The preparation method of the sunscreen with attapulgite as a carrier of the present invention is simple, has abundant raw material sources, does not require high temperature and high pressure, and is convenient for large-scale industrial production.

Description

Technical Field

[0001] The invention belongs to the technical field of cosmetics, and particularly relates to a sunscreen agent using attapulgite as a carrier and a preparation method thereof. Background Art

[0002] Ultraviolet rays can cause great damage to human skin. High-intensity or long-term outdoor activities will expose the skin to ultraviolet rays for a long time, which will inevitably cause damage to skin tissue and cause many skin problems, and even lead to skin cancer. Sunscreen cosmetics refer to cosmetics that have added sunscreens that can block or absorb ultraviolet rays to prevent the skin from being tanned or sunburned. Sunscreens can be divided into physical sunscreens, chemical sunscreens and natural sunscreens. Physical sunscreens are highly safe, but their sunscreen efficiency is affected by conditions such as their particle size and dispersibility. Their poor dispersibility often reduces the sunscreen efficiency of sunscreens. In order to improve the sunscreen ability, a higher addition amount is usually required, but as the amount of physical sunscreen added increases, the product will turn white, the skin feel will decrease, and the stability of the sunscreen will be reduced. Chemical sunscreens have a strong ability to absorb ultraviolet rays, but their stability is poor. They are also somewhat irritating to the skin, and high amounts added can cause the product to feel greasy. Natural sunscreens can reduce the damage of ultraviolet rays to the skin through antioxidant or anti-free radical effects and have good safety, but their effects are generally not as good as chemical sunscreens, and it is difficult to produce an effective sunscreen product when used alone.

[0003] Attapulgite, also known as palygorskite, is a natural chain-layered magnesium-aluminum silicate clay mineral. The single crystal of attapulgite is rod-shaped, has a unique multi-level pore structure, a large specific surface area, and a negative charge on the surface. It is an adsorbent and carrier material with excellent performance. Attapulgite also has good dispersion, high temperature resistance, salt and alkali resistance, and has certain water retention properties. At the same time, attapulgite has been included in the latest version of the cosmetic raw material catalog and has been used in cosmetics, such as sunscreen cream (CN101579300A), lipstick (CN111281828B), etc.

[0004] In view of the performance defects of existing sunscreens, the present invention utilizes the unique pore structure of attapulgite as a carrier to load the sunscreen, so as to solve the application problems of poor dispersibility, low sunscreen efficiency and easy residue of existing sunscreens. At the same time, attapulgite can also enhance the water retention performance of the product and improve the skin feel of sunscreen cosmetics. Summary of the invention

[0005] The purpose of the present invention is to overcome the defects of existing sunscreens and to provide a method for preparing a sunscreen using attapulgite as a carrier and the sunscreen.

[0006] In a first aspect, the present invention discloses a method for preparing a sunscreen agent using attapulgite as a carrier, the method comprising the following steps:

[0007] Step A: sieving attapulgite soil with a 100-800 mesh sieve to obtain sieved attapulgite, adding the sieved attapulgite to an appropriate amount of the first solvent, treating it with ultrasound at a power of 10-30kHz at 10-80°C for 0.2-1h, and then stirring it at a speed of 100-1000r / min for 0.5-3h to obtain an attapulgite carrier slurry A with a mass content of 1-50%;

[0008] Step B: weighing the sunscreen according to a mass ratio of 1:1-99 between the sunscreen and the attapulgite in the attapulgite carrier slurry A, dissolving or dispersing the sunscreen in an appropriate amount of a second solvent, treating with ultrasound at a power of 10-20 kHz for 0.2-1 h at 30-80° C., and then stirring at a speed of 100-800 r / min for 0.5-3 h to obtain a sunscreen slurry B with a mass content of 1-80%;

[0009] Step C: under a specific gas atmosphere, adding the sunscreen slurry B to the attapulgite carrier slurry A to form a mixed slurry, stirring the mixed slurry at 10-80° C. and 100-1000 r / min for 10-30 min, adding a connector with a mass ratio of 0.1-10%, continuing to stir for 30-90 min, and then adding a modifier with a mass ratio of 0.1-10%, continuing to stir for 30-120 min; after the reaction is completed, filtering the mixed slurry and washing 1-3 times to obtain a filter cake, and then vacuum drying the filter cake at room temperature for 5-24 h to obtain a sunscreen with attapulgite as a carrier.

[0010] Specifically, the first solvent and the second solvent are one or a mixture of two or more solvents in any proportion, such as water, ethanol, methanol, etc.

[0011] Specifically, the sunscreen is one or more of a physical sunscreen, a chemical sunscreen, and a natural sunscreen.

[0012] Specifically, the physical sunscreen is zinc oxide and titanium dioxide particles, preferably zinc oxide and titanium dioxide with a particle size of 5-100 nm.

[0013] Specifically, the chemical sunscreen is one or more of ethylhexyl methoxycinnamate, 4-methylbenzyl camphor, bis-ethylhexyloxyphenol methoxyphenyl triazine, isopentyl p-methoxycinnamate, diethylaminohydroxybenzoyl hexyl benzoate, cinnamate derivatives, salicylic acid derivatives, butyl methoxydibenzoylmethane, benzophenone, methylene dibenzotriazole tetramethylbutylphenol, and anthranilate, preferably ethylhexyl methoxycinnamate.

[0014] Specifically, the natural plant sunscreen is one or more extracts of tea, aloe, tomato, orange, tangerine peel, birch bark, Polygonum multiflorum, kiwi fruit, cucumber, sea buckthorn, scutellaria baicalensis, broccoli, etc., preferably aloe and tea extracts.

[0015] Specifically, the specific gas atmosphere is air or nitrogen;

[0016] Specifically, the linking agent is one or more of vinyl tri(β-methoxyethoxy)silane, γ-aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane, 3-aminopropyl trimethoxysilane, γ-(2,3-epoxypropyloxy)propyl trimethoxysilane, and γ-methacryloxypropyl trimethoxysilane.

[0017] Specifically, the modifier is one or more of an amino acid modifier or a lecithin modifier. The lecithin modifier includes soybean hydrogenated lecithin, soybean acylated lecithin, and soybean hydroxylated lecithin; the amino acid modifier includes sodium cocoyl glutamate, sodium lauroyl glutamate, and potassium cocoyl glycinate.

[0018] In a second aspect, the present invention further discloses a sunscreen agent using attapulgite as a carrier, wherein the sunscreen agent is prepared according to the above-mentioned method for preparing a sunscreen agent using attapulgite as a carrier. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 This is the SEM picture of the attapulgite prepared in the present invention before and after the sunscreen is adsorbed.

[0020] Figure 2A This is the adsorption-desorption isotherm diagram of the attapulgite prepared in the present invention before and after the adsorption of the sunscreen agent.

[0021] Figure 2B This is the pore size distribution diagram of the attapulgite prepared in the present invention before and after the sunscreen agent is adsorbed.

[0022] Figure 3 The ultraviolet absorption curve of the sunscreen prepared with attapulgite as a carrier according to the present invention. DETAILED DESCRIPTION

[0023] In order to enable those skilled in the art to better understand the present invention, the technical solution of the present invention will be clearly and completely described below in conjunction with the accompanying drawings and specific embodiments.

[0024] Example 1

[0025] Step A: sieve the attapulgite soil with a 400-mesh sieve, weigh 10 g of the sieved attapulgite and add it to 90 g of ethanol solvent, treat it with ultrasound at a power of 10 kHz at 30° C. for 0.5 h, and then stir it at a speed of 1000 r / min for 1 h to obtain an attapulgite carrier slurry A with a mass content of 10%;

[0026] Step B: 2.5 g of nano zinc oxide powder with an average particle size of 20 nm was weighed according to a mass ratio of sunscreen to attapulgite in slurry A of 1:4, dispersed in 22.5 g of ethanol, and subjected to ultrasonic treatment at a power of 10 kHz for 0.5 h at 30° C., and then stirred at a speed of 800 r / min for 1 h to obtain a sunscreen slurry B with a mass content of 10%;

[0027] Step C: under a nitrogen atmosphere, adding the sunscreen slurry B to the slurry A, stirring at 30° C. and 1000 r / min for 10 min, adding 0.5 g of γ-aminopropyl triethoxysilane, continuing to stir and react for 60 min, and then adding 0.3 g of sodium cocoyl glutamate, continuing to stir and react for 60 min; after the reaction, filtering the slurry and washing it 3 times to obtain a filter cake, and vacuum drying the filter cake at room temperature for 24 h to obtain a sunscreen with attapulgite as a carrier.

[0028] Example 2

[0029] Step A: sieve the attapulgite soil with a 600-mesh sieve, weigh 10 g of the sieved attapulgite, add it to 40 g of methanol-water (volume ratio 1:1) solvent, treat it with ultrasound at a power of 10 kHz for 0.5 h at 30° C., and then stir it at a speed of 1000 r / min for 0.5 h to obtain an attapulgite carrier slurry A with a mass content of 20%;

[0030] Step B: 10 g of titanium dioxide powder with an average particle size of 100 nm was weighed according to a mass ratio of sunscreen to attapulgite in slurry A of 1:1, dispersed in 90 g of ethanol, and subjected to ultrasonic treatment at a power of 10 kHz for 0.5 h at 30° C., and then stirred at a speed of 800 r / min for 1 h to obtain a sunscreen slurry B with a mass content of 10%;

[0031] Step C: Under a nitrogen atmosphere, slurry B is added to slurry A, and after stirring at 30° C. and 1000 r / min for 10 min, 0.5 g of γ-aminopropyltriethoxysilane is added, and the stirring reaction is continued for 60 min, and then 0.3 g of sodium cocoyl glutamate is added, and the stirring reaction is continued for 60 min. After the reaction is completed, the slurry is filtered and washed 3 times to obtain a filter cake, and the filter cake is vacuum dried at room temperature for 24 h to obtain a sunscreen agent with attapulgite as a carrier.

[0032] Example 3

[0033] Step A: sieve the attapulgite soil with a 600-mesh sieve, weigh 10 g of the sieved attapulgite, add it to 40 g of ethanol solvent, treat it with ultrasound at a power of 10 kHz at 30° C. for 0.5 h, and then stir it at a speed of 1000 r / min for 0.5 h to obtain an attapulgite carrier slurry A with a mass content of 20%;

[0034] Step B: 5 g of zinc oxide particles with an average particle size of 20 nm and 5 g of aloe extract were weighed according to a mass ratio of sunscreen to attapulgite in slurry A of 1:1, dispersed in 90 g of ethanol, and subjected to ultrasonic treatment at a power of 10 kHz for 0.5 h at 30° C., and then stirred at a speed of 800 r / min for 1 h to obtain a sunscreen slurry B with a mass content of 10%;

[0035] Step C: Under a nitrogen atmosphere, slurry B is added to slurry A, and after stirring at 30° C. and 1000 r / min for 100 min, 0.5 g of γ-aminopropyltriethoxysilane is added, and the stirring reaction is continued for 60 min. Then, 0.3 g of soybean hydroxylated phospholipid is added, and the stirring reaction is continued for 60 min. After the reaction is completed, the slurry is filtered and washed 3 times to obtain a filter cake, and the filter cake is vacuum dried at room temperature for 12 h to obtain a sunscreen agent with attapulgite as a carrier.

[0036] Example 4

[0037] Step A: sieve the attapulgite soil with a 600-mesh sieve, weigh 10 g of the sieved attapulgite, add it to 90 g of ethanol solvent, treat it with ultrasound at a power of 10 kHz at 30° C. for 0.5 h, and then stir it at a speed of 1000 r / min for 0.5 h to obtain an attapulgite carrier slurry A with a mass content of 10%;

[0038] Step B: 10 g of zinc oxide particles with an average particle size of 20 nm were weighed according to a mass ratio of sunscreen to attapulgite in slurry A of 1:1, dispersed in 90 g of ethanol, and subjected to ultrasonic treatment at a power of 10 kHz for 0.5 h at 30° C., and then stirred at a speed of 800 r / min for 1 h to obtain a sunscreen slurry B with a mass content of 10%;

[0039] Step C: Under a nitrogen atmosphere, slurry B is added to slurry A, and after stirring at 20° C. and 1000 r / min for 100 min, 0.5 g of γ-aminopropyltriethoxysilane is added, and the stirring reaction is continued for 60 min. Then, 0.3 g of soybean hydroxylated phospholipid is added, and the stirring reaction is continued for 60 min. After the reaction is completed, the slurry is filtered and washed 3 times to obtain a filter cake, and the filter cake is vacuum dried at room temperature for 12 h to obtain a sunscreen agent with attapulgite as a carrier.

[0040] Example 5

[0041] Step A: sieve the attapulgite soil with a 400-mesh sieve, weigh 10 g of the sieved attapulgite, add it to 40 g of ethanol solvent, treat it with ultrasound at a power of 10 kHz at 30° C. for 0.5 h, and then stir it at a speed of 1000 r / min for 0.5 h to obtain an attapulgite carrier slurry A with a mass content of 20%;

[0042] Step B: 5 g of ethylhexyl methoxycinnamate and 5 g of aloe extract were weighed according to a mass ratio of sunscreen to attapulgite in slurry A of 1:4, dispersed in 90 g of ethanol-water system (volume ratio of 1:1), and subjected to ultrasonic treatment at a power of 10 kHz for 0.5 h at 30° C., and then stirred at a speed of 800 r / min for 1 h to obtain a sunscreen slurry B with a mass content of 10%;

[0043] Step C: Under a nitrogen atmosphere, slurry B is added to slurry A, and after stirring at 40° C. and a speed of 1000 r / min for 100 min, 0.5 g of vinyl tri(β-methoxyethoxy)silane is added, and the stirring reaction is continued for 60 min, and then 0.3 g of sodium cocoyl glutamate is added, and the stirring reaction is continued for 60 min; after the reaction is completed, the slurry is filtered and washed 3 times to obtain a filter cake, and the filter cake is vacuum dried at room temperature for 12 h to obtain a sunscreen agent with attapulgite as a carrier.

[0044] Figure 1 The following are SEM photos of pure attapulgite and attapulgite loaded with sunscreen prepared in Example 1 of the present invention. Figure 1 It can be seen that the surface of the pure attapulgite carrier is very smooth, and after the sunscreen component is loaded, the sunscreen component is evenly distributed on the surface of the attapulgite, which helps to improve the sunscreen efficiency of the sunscreen component.

[0045] Figure 2A is the adsorption-desorption isotherm curve of attapulgite before and after loading physical sunscreen agent. Figure 2BFigure 2 is the pore size distribution curve of attapulgite before and after loading the physical sunscreen. It can be seen that after the attapulgite carrier adsorbs the sunscreen component, the pore volume is significantly reduced, indicating that the sunscreen component can be loaded in the pores of the attapulgite carrier, so attapulgite has a good dispersion ability for the sunscreen component.

[0046] Figure 3 The UV absorption curve of the attapulgite-loaded sunscreen prepared in Example 1 of the present invention. The UV-visible absorption spectrum of the solid was obtained on a Shimadzu UV-2600 UV / visible spectrophotometer equipped with an integrating sphere under the condition of barium sulfate as the background. As can be seen from the figure, compared with pure attapulgite, the sunscreen prepared with attapulgite as the carrier has obvious absorption in the 300-350nm band, indicating that the sunscreen prepared with attapulgite as the carrier has sunscreen effect.

[0047] Although the embodiments of the present invention have been shown and described above, it is to be understood that the above embodiments are exemplary and are not to be construed as limitations of the present invention. A person skilled in the art may change, modify, replace and vary the above embodiments within the scope of the present invention.

Claims

1. A method for preparing a sunscreen agent using attapulgite as a carrier, the method comprising the following steps: Step A: sieve the attapulgite soil with a 100-800 mesh sieve to obtain sieved attapulgite, weigh 10 g of the sieved attapulgite and add it to the first solvent, treat it with ultrasound at a power of 10-30 kHz at 30-80°C for 0.2-1h, and then stir it at a speed of 100-1000 r / min for 0.5-1h to obtain an attapulgite carrier slurry A with a mass content of 10%; Step B: weighing a sunscreen according to a mass ratio of 1:1-4 between the sunscreen and the attapulgite in the attapulgite carrier slurry A, dispersing the sunscreen in a second solvent, treating the solution with ultrasound at a power of 10-20 kHz at 30-80°C for 0.5-1 h, and then stirring the solution at a speed of 100-800 r / min for 0.5-3 h to obtain a sunscreen slurry B with a mass content of 10%; wherein the sunscreen is a physical sunscreen, and the physical sunscreen is 5-20 nm zinc oxide; Step C: under a nitrogen atmosphere, adding the sunscreen slurry B to the attapulgite carrier slurry A to form a mixed slurry, stirring the mixed slurry at 30-80°C and 100-1000 r / min for 10-30 min, adding 0.5 g of a linker, continuing to stir and react for 30-90 min, and then adding 0.3 g of a modifier, continuing to stir and react for 30-120 min; after the reaction is completed, filtering the mixed slurry, washing 1-3 times to obtain a filter cake, and vacuum drying the filter cake at room temperature for 5-24 h to obtain a sunscreen with attapulgite as a carrier; Wherein, the first solvent described in step A is one or a mixture of two or more solvents in any proportion, water, ethanol or methanol; the second solvent described in step B is ethanol; the linker described in step C is γ-aminopropyl triethoxysilane, and the modifier is sodium cocoyl glutamate or soybean hydroxylated phospholipid.

2. A sunscreen agent using attapulgite as a carrier, characterized in that: The sunscreen is prepared according to the method for preparing a sunscreen using attapulgite as a carrier according to claim 1.

Images