KR101761714B1 - Manufacturing method of multi-functional fine particles having ultraviolet-proof and antibiotic functions and the multi-functional fine particles manufactured therefrom - Google Patents
Manufacturing method of multi-functional fine particles having ultraviolet-proof and antibiotic functions and the multi-functional fine particles manufactured therefrom Download PDFInfo
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- KR101761714B1 KR101761714B1 KR1020150091428A KR20150091428A KR101761714B1 KR 101761714 B1 KR101761714 B1 KR 101761714B1 KR 1020150091428 A KR1020150091428 A KR 1020150091428A KR 20150091428 A KR20150091428 A KR 20150091428A KR 101761714 B1 KR101761714 B1 KR 101761714B1
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- 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
- A61K8/27—Zinc; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- 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
- A61K8/29—Titanium; Compounds thereof
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- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
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Abstract
It is harmless to the human body and has antibacterial properties by adding silane to the metal oxide nanoparticles to give a functional group and then adding a silver compound to give an antibacterial function by chelating reaction and then bonding an organic UV-blocking agent to the UV- The present invention also relates to a method for producing an antibacterial / ultraviolet blocking multi-functional fine particle which provides excellent multi-functional fine particles having a high light fastness to a dye and a multi-functional fine particle prepared therefrom.
Description
The present invention relates to a metal oxide nanoparticle, which is obtained by adding a silane group to a metal oxide nanoparticle to give a functional group, and then adding a silver compound to the metal oxide nanoparticle to chelate and thereby impart an antimicrobial function. The present invention relates to a method for producing an antibacterial / ultraviolet blocking multi-functional fine particle which provides a multi-functional fine particle which is excellent in antibacterial activity and light fastness to a dye, and to a multi-functional fine particle prepared therefrom.
Ultraviolet light should play an important role in reducing collagen synthesis if severe collagen reduction in skin that has been exposed to UV rays for a long time (photoaged skin) is the main cause of wrinkles. Recent studies have shown that when irradiated with ultraviolet light on human skin, the synthesis of collagen is reduced through a complex signal pathway and the expression of matrix metalloproteinases (MMPs), a degradation enzyme of extracellular matrix proteins including collagen, is increased.
In 1993, the US FDA proposed a final monograph for an ultraviolet screening agent in OTC medicines, which contains available UV absorbers and formulation limits. In Japan, the ultraviolet absorber that can be incorporated into the ultraviolet screening agent is described in the classification approval standard. When the compounding amount exceeds 10%, it is required to apply with the safety data, and in order to develop ultraviolet absorber, safety and functionality In addition, solubility and stability in cosmetic bases are also important factors.
At present, ultraviolet light absorbers are ultraviolet absorbers, which are organic compounds such as benzophenone, cinnamic acid, salicylic acid and para-aminobenzoic acid (PABA).
In recent years, titanium oxide and zinc oxide based on inorganic compounds have been listed as ultraviolet absorptive and scattering agents. However, they have different wavelength regions to be scattered due to changes in particle size or shape, and are not well soluble in water or oil in cosmetic bases, Dispersing technology is important.
It is also used as a preservative for parabens which is used as a preservative for cosmetics. It is used as a preservative for cosmetics. Combination limit due to preservative is 0.4% (as an acid) for a single ingredient and 0.8% (as an acid) for a mixed ingredient (In Europe, the paraben content is 0.19% or less because of the harmfulness.) Parabens are preservatives that are used in the food, pharmaceutical and personal care products industries. Controversy is a controversial ingredient. Estrogen ) And the endocrine system (endocrine) has been reported to be possible. Studies have also shown that methylparaben has a detrimental effect on the aging and differentiation of skin cells.
Methylchloroisothiazolinone (MCI) is a chemical that is widely used today as a sterilization preservative in personal care products, including cosmetics and shampoos. For example, young, infant wipes, and disposable diapers are among the personal care products used by MIT and MCI. However, research findings suggesting that MIT and MCI may cause allergic skin disease are likely to trigger a sensitive response from consumers.
Dr. Mark R. Petekoff, MD, a team at the Mayo Clinic in Rochester, Minnesota, USA, reports in a June issue of the Archives of Dermatology, an academic journal published by the American Medical Association (AMA) He said. The subject of this report is the 'Danger of Moist Toilet Paper'. The main point of the study was that during the 6-month study at the Mayo Clinic, among the subjects who used the baby wipes containing MIT, 4 adults The patients were found to have severe perianal and perineal allergic contact dermatitis. In addition, the team was able to observe cases of allergies among subjects using MCI, the team added.
Although MIT and MCI have been constantly following the safety debate over the past decade, it has been known that cases of side effects were rarely reported in academia. MCI has excellent antibacterial and antifungal activity and is used as a disinfectant in various personal care products with MIT. "Patients with dermatitis have relieved their symptoms by stopping the use of wipes," Dr. Felekov said. Accordingly, development of antibacterial and UV-screening agents that are stable to the skin is required.
Also, in the field of textiles, many products using antibacterial fiber materials are made, but organic inorganic antibacterial agents are required to exhibit fastness to laundering by attaching to fibers. However, since the fastness to washing is low, antibacterial property tends to be remarkably decreased by washing several times.
Furthermore, in summer and in the tropics, not only skin aging due to ultraviolet rays but also low color fastness of the dye tends to discolor the fibers. Accordingly, it is necessary to develop a material having excellent antimicrobial activity and light fastness to a fiber.
Functionality is particularly emphasized in recent cosmetics. With the advancement of dermatology, interest in improving the effect of cosmetics on skin and hair, such as whitening, wrinkle prevention and hair growth, is increasing. Particularly, UV protection products are aimed at consumers as a whole regardless of age, and demand for spring and summer is high. However, products for four seasons are increasing. In addition, the number of products with the body make-up function increases, and cosmetic effects and the effect that the skin looks beautiful. Lipcream market is small, but demand is increasing as interest in UV shielding increases.
It is expected that the present invention will have an import substitution effect of 50 billion won, which is 10% of functional cosmetics imports, and an export increase of 10 billion won, 10% of functional cosmetics exports, which will minimize the damage of human body due to harmful substances The skin trouble due to cosmetics can be avoided. In addition, the development of materials such as antimicrobial materials which do not contain preservatives derived from natural materials, materials which do not cause side effects of skin, and ultraviolet ray materials are expected to increase the number of additional functional products such as cosmetic and skin- .
Parabens preservatives used as cosmetic preservatives, ie parabens preservatives, are a typical preservative used in the food, pharmaceutical and personal care products industries. There are frequent controversies about the harmfulness. In the summer and the tropical regions, as well as aging of the skin caused by ultraviolet rays, It is necessary to develop a material having excellent antimicrobial and light fastness because the color of the fiber is discolored due to low fastness. Therefore, it is an excellent material which is harmless to human body, excellent in antimicrobial property and can increase the fastness to light of dye, and can be applied to various fields such as cosmetics, fibers and films, and a method for producing multi- Development of fine particles is necessary.
Parabens preservatives, which are used as preservatives in cosmetics, are a typical preservative used in the food, pharmaceutical and personal care products industries. There are many controversies about harmfulness. In summertime and tropical regions, not only the aging of skin caused by UV rays, There was a problem that the fiber was discolored due to low light fastness.
The present invention solves the above problems and provides a method for producing antibacterial / ultraviolet blocking multi-functional fine particles which can be applied to various fields such as cosmetics, fibers and films by improving harmlessness to the human body, It is an object of the present invention to provide the prepared multi-functional fine particles.
In order to achieve the above object,
The present invention relates to a method of manufacturing a metal oxide nanoparticle comprising: (S10) preparing metal oxide nanoparticles of titanium oxide (TiO 2 ) or zinc oxide (ZnO);
30 to 70 wt% of the metal oxide nanoparticles prepared in the step (S10)
Aminosilane or methyltrimethoxysilane selected from aminopropyltrimethoxysilane, aminoethylaminopropyltrimethoxysilane, aminopropyltriethoxysilane and aminoethylaminopropyltriethoxysilane, hexylthio (TEOS) The alkyl silane selected from among hexyltrimethoxysilane, octyltrimethoxysilane, dodecyltrimethoxysilane, methyltriethoxysilane, hexyltriethoxysilane, octyltriethoxysilane, and dodecyltriethoxysilane (S20) mixing 30 to 70 wt% of any one kind or more of the silanes, and imparting functional groups to the metal oxide nanoparticles;
A silver compound is added to the metal oxide nanoparticles after the step (S20), and a silver compound having a molar ratio of 1/4 to 1/32 mol of the aminosilane or alkylsilane is added and the compound is chelated at a temperature of 80 ° C to 80 ° C (S30) of imparting an antibacterial function;
The metal oxide nanoparticles that have undergone the above step (S30) may further contain at least one selected from the group consisting of ethylhexyl methoxycinnamate, octyl methoxycinnamate, phenylbenzimidazole sulfonic acid, avobenzone, oxybenzone, benzophenone, oxanilide, cinnamate, (S40) of bonding at least one or two or more organic UV-blocking agents selected from the group consisting of aminosilane and alkylammonium, To thereby provide an antibacterial / ultraviolet blocking multi-functional fine particle production method.
Also provided are antibacterial and ultraviolet blocking multi-functional fine particles which are manufactured through such a manufacturing process and used for cosmetics, fibers and plastic films.
The present invention relates to a technique for producing inorganic fine particles and imparting antimicrobial and ultraviolet barrier properties to the surface of particles and applying the same to cosmetics, fibers and films to provide physically stable, stable human body, The present invention provides a composite functional particle having improved spreadability and improved cosmetic persistence as well as improved cohesion prevention of powder and prevention of collapse of makeup caused by sebum, and also provides antibacterial particles having a washing fastness over 30 times The present invention has the advantage that it can be widely used as a preservative for films, fibers and cosmetics and as an ultraviolet screening agent.
The present invention can provide a product that is safe and has excellent light fastness to fiber antimicrobial agents and dyes by producing a new formulation replacing the existing ultraviolet screening agent, thereby contributing to expansion of the film, textile and cosmetic market, It has an advantage that it can be utilized as a catalyst or dye for a solar cell.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a view showing a process for producing multipurpose antibacterial and ultraviolet blocking multi-functional fine particles according to the present invention. FIG.
2 (A) to 2 (F) show antibacterial test results on Staphylococcus aureus polylylene film to which the multi-functional fine particles according to the present invention are applied.
3 (A) to 3 (F) show antibacterial test results of a polyethylene film to which the multi-functional fine particles according to the present invention are applied, against E. coli.
4 is a photograph of the result of culturing a polylysine film (control piece) not treated with the multifunctional fine particles according to the present invention and a polyethylene film (sample piece) treated with the multifunctional fine particles for Staphylococcus aureus. A) to F)
5 is a photograph of the result of culturing a polylysine film (control sample) not treated with the multifunctional fine particles according to the present invention and a polyethylene film (sample piece) treated with the multifunctional fine particles with respect to E. coli. (Sample (A) (F))
As described above, the method for producing an antibacterial / ultraviolet screening composite functional fine particle for cosmetics and fibers according to the present invention is characterized in that a metal oxide nanoparticle of titanium oxide (TiO 2 ) or zinc oxide (ZnO) (S10);
30 to 70 wt% of the metal oxide nanoparticles prepared in the step (S10)
Aminosilane or methyltrimethoxysilane selected from aminopropyltrimethoxysilane, aminoethylaminopropyltrimethoxysilane, aminopropyltriethoxysilane and aminoethylaminopropyltriethoxysilane, hexylthio (TEOS) The alkyl silane selected from among hexyltrimethoxysilane, octyltrimethoxysilane, dodecyltrimethoxysilane, methyltriethoxysilane, hexyltriethoxysilane, octyltriethoxysilane, and dodecyltriethoxysilane (S20) mixing 30 to 70 wt% of any one kind or more of the silanes, and imparting functional groups to the metal oxide nanoparticles;
A silver compound is added to the metal oxide nanoparticles after the step (S20), and a silver compound having a molar ratio of 1/4 to 1/32 mol of the aminosilane or alkylsilane is added and the compound is chelated at a temperature of 80 ° C to 80 ° C (S30) of imparting an antibacterial function;
The metal oxide nanoparticles that have undergone the above step (S30) may further contain at least one selected from the group consisting of ethylhexyl methoxycinnamate, octyl methoxycinnamate, phenylbenzimidazole sulfonic acid, avobenzone, oxybenzone, benzophenone, oxanilide, cinnamate, (S40) of bonding at least one or two or more organic UV-blocking agents selected from the group consisting of aminosilane and alkylammonium, .
Hereinafter, specific details of each of the above-described technical configurations will be described.
[Metal oxide nanoparticle preparation step (
S10
)]
The titanium oxide (TiO 2 ) The fine particles can be produced by hydrolyzing titania sulfate to produce titanium hydroxide, which is then heated and aged in hydrochloric acid to produce titanium oxide (TiO 2 ) particles having a rutile crystal structure of nanoparticles. At this time, titanium oxide (TiO 2 ) is sol-ized and its particle size is 15 to 40 nm.
The zinc oxide (ZnO) fine particles were prepared by adding zinc chloride (1%) in water / alcohol (2/8) mixed solution of zinc isopropoxide and aging for 24 hours to prepare zinc oxide sol The size is 15 to 30 nm.
[Metal oxide nanoparticles
Functional
(
S20
)]
(TiO 2 ) or zinc oxide (ZnO) is mixed with the metal oxide nanoparticles (TiO 2 ) or zinc oxide (ZnO) while stirring at room temperature, the step of adding functional groups to the metal oxide nanoparticles, For 30 to 70 wt%
Aminosilane or methyltrimethoxysilane selected from aminopropyltrimethoxysilane, aminoethylaminopropyltrimethoxysilane, aminopropyltriethoxysilane and aminoethylaminopropyltriethoxysilane, hexylthio (TEOS) The alkyl silane selected from among hexyltrimethoxysilane, octyltrimethoxysilane, dodecyltrimethoxysilane, methyltriethoxysilane, hexyltriethoxysilane, octyltriethoxysilane, and dodecyltriethoxysilane And 30 to 70 wt% of at least one kind of silane.
If the amount of the metal oxide nanoparticles used is less than 30 wt%, there is a problem that ultraviolet light is blocked by the reflection effect of the inorganic blockade agent. When the amount is more than 70 wt%, the absorption ability of the organic ultraviolet screening agent can not be expected. The use amount of the oxide nanoparticles is preferably limited within a range of 30 to 70 wt%.
[Antimicrobial function imparting step (
S30
)]
A silver compound is added to the metal oxide nanoparticles after the step (S20), and a silver compound having a molar ratio of 1/4 to 1/32 mol of the aminosilane or alkylsilane is added and the compound is chelated at a temperature of 80 ° C to 80 ° C As a step of imparting an antimicrobial function, metal oxide nanoparticles are dispersed in water and then mixed with a silver compound of silver nitrate or silver oxide at room temperature to 80 ° C with stirring to prepare metal oxide nanoparticles having antimicrobial properties.
If the addition amount of the silver compound is less than 1/4 of the number of moles of the aminosilane or the alkylsilane in the chelating step, the metal may remain and the chelate may be formed, / 32, there is a problem that the antibacterial activity is lowered. Therefore, the amount of the silver compound to be added is preferably limited within a range of 1/4 mol to 1/32 mol of the number of moles of aminosilane or alkylsilane.
When the reaction temperature is kept below room temperature, there is a problem that a chelate is not formed. When the reaction temperature exceeds 80 ° C, there is a problem of discoloring. Therefore, the reaction temperature is preferably kept within a range of room temperature to 80 ° C Do.
[The step of imparting the ultraviolet shielding function (
S40
)]
The step of imparting an ultraviolet shielding function to the metal oxide nanoparticles to which the antibacterial property is imparted through the steps,
The metal oxide nanoparticles are selected from the group consisting of ethylhexyl methoxycinnamate, octylmethoxycinnamate, phenylbenzimidazole sulfonic acid, avobenzone, oxybenzone, benzophenone, oxanilide, cinnamate, salicylate, Any one or two or more kinds of organic ultraviolet screening agents are bound, but are bound to the equimolar to 1/2 mol of the moles of aminosilane or alkylsilane.
At this time, when the organic UV blocking agent is not used in the same molar amount as the silane, the amine of the aminosilane may remain to stimulate the skin, so that it is preferable to use an aminosilane equivalent to the aminosilane.
Specific examples 1 to 3 according to the method for producing the antibacterial / UV-shielding multi-functional fine particles of the present invention are as follows.
[
Example
One]
Titanium oxide (TiO 2 ) fine particles were prepared by adding 100 g of titania sulfate to 900 g of water and hydrolyzing the mixture at room temperature for 24 hours to prepare titanium hydroxide. The resulting mixture was heated at 70 ° C in
70 g of aminopropyltrimethoxysilane (Z-6011) and 30 g of MTMS (Methyltrimethoxysilane) were added, and 5 g of ammonia water was added thereto. The reaction mixture was reacted at room temperature for 24 hours To prepare a titanium oxide particle into which an amino group is introduced. 6.7 g of nitric acid was added thereto and reacted at room temperature for 2 hours. Next, 86 g of 2-phenyl-benzimidazole-5 sulphonic acid soduim salt (HS), which is an ultraviolet absorber, is dissolved in 500 g of water and added to the reaction mixture to prepare ultraviolet and antibacterial titanium oxide composite fine particles (Table 1).
[Examples 2 to 3]
The composite fine particles were prepared in the same manner as in Example 1 except that the addition amount was as shown in Table 1 below (Table 1).
MTMS (g)
(Parsol 1789)
(g) **
(탆)
70/30
* MCA: Methoxycinnamic acid
** BMBM (Parsol 1789): Butyl Methoxydibensol methane
Hereinafter, characteristics of the multi-functional fine particles produced through such steps will be described.
[
Test Example]
[Antimicrobial activity measurement]
The inoculum to Escherichia coli culture solution (O.D600 0.804, 3.7 × 10 8 cells / ㎖), Salmonella typhimurium culture solution (OD 600 1.140, 6.9 × 10 8 cells / ㎖), Shigella sonnei culture solution (OD 600 0.608, 1.36 × 10 8 cells / ml). The bacterial counts of E. coli were adjusted to 7.4% in the culture medium by adding 0.2 ml of the prepared bacterial solution to the medium (9.3 ml) to make the antibacterial / ultraviolet blocking functional fine particles 0.05% 10 6 cells / ㎖, the number of S. typhimurium was 1.38 × 10 7 cells / ㎖, and the number of S. sonnei was 2.72 × 10 6 cells / ㎖) and cultured at 37 ° C for 1 to 2 days with shaking. The culture broth was diluted 10 times with sterile physiological saline and plated on LB agar plate at 0.1 ㎖. After culturing at 37 ℃ for 1 day, the colony forming ability (CFU) was counted. In the control group, the same procedure is followed without the addition of the antibacterial microparticles.
[ UV-rays
Barrier property
Research(
SPF
Index and
PA
Index measurement)]
Cream-type cosmetics were prepared by preparing a cream containing a certain amount of antibacterial / ultraviolet blocking compound-functional fine particles at various composition ratios. The prepared cosmetic sample was applied to a cell and SPF and PA were measured by Optometrics SPF-290S Analyzer. Are shown in Table 2 below.
(wt%)
(wt%)
(wt%)
(wt%)
(wt%)
(10 wt%)
2
One
3
82
(+++)
(10 wt%)
(+++)
(10 wt%)
(+++)
FIGS. 2 to 5 are photographs showing the results of antibacterial test and culture results of applying the antibacterial / ultraviolet blocking multi-functional fine particles prepared according to the present invention to a polyethylene film using Staphylococcus aureus and E. coli. Test results and photographs of the culture results showed 99.99% reduction of Staphylococcus aureus and Escherichia coli compared to the control.
INDUSTRIAL APPLICABILITY The present invention is applicable to various fields such as cosmetics, fibers and plastic films by providing multifunctional fine particles which are harmless to human body, excellent in antimicrobial activity and can enhance the light fastness to dye, and thus are highly industrially applicable.
Claims (3)
30 to 70 wt% of the metal oxide nanoparticles,
Aminosilane or methyltrimethoxysilane selected from aminopropyltrimethoxysilane, aminoethylaminopropyltrimethoxysilane, aminopropyltriethoxysilane and aminoethylaminopropyltriethoxysilane, hexylthio (TEOS) The alkyl silane selected from among hexyltrimethoxysilane, octyltrimethoxysilane, dodecyltrimethoxysilane, methyltriethoxysilane, hexyltriethoxysilane, octyltriethoxysilane, and dodecyltriethoxysilane And 30 to 70 wt% of at least one kind of silane selected from the group consisting of a metal oxide nanoparticle and a metal oxide nanoparticle;
To the metal oxide nanoparticle to which the functional group is imparted, an organic solvent such as ethylhexyl methoxycinnamate, octylmethoxycinnamate, phenylbenzimidazole sulfonic acid, avobenzone, oxybenzone, benzophenone, oxanilide, cinnamate, salicylate, vinyl Amide, wherein the organic UV-blocking agent is bonded to the aminosilane or the alkylsilane at an equimolar to 1/2 mole of the aminosilane or alkylsilane to give an ultraviolet shielding function,
As a subsequent step immediately following the step of imparting functional groups to the metal oxide nanoparticles,
A silver compound is added to the metal oxide nanoparticles to which the functional group is added, and a silver compound having a molar ratio of 1/4 to 1/32 mol of the aminosilane or the alkylsilane is added and the chelating reaction is performed at room temperature to 80 ° C. The method of claim 1, wherein the microparticulate / ultraviolet blocking functional-functional microparticle is prepared by a method comprising the steps of:
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| KR102403343B1 (en) * | 2021-03-12 | 2022-05-30 | 경북대학교 산학협력단 | Composite material comprising silane-based sizing agent and method for preparing thereof |
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| KR100526888B1 (en) | 2004-02-20 | 2005-11-08 | 학교법인조선대학교 | Lignan glucoside compound extracted from Styrax japonica S. et Z. and cosmetic composition containing the same |
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