CN112741775B - Preparation method of composite mica powder with oil control performance for cosmetics - Google Patents
Preparation method of composite mica powder with oil control performance for cosmetics Download PDFInfo
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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
- A61K8/26—Aluminium; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- 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
- A61K8/24—Phosphorous; 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
- A61K8/27—Zinc; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/008—Preparations for oily skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
- A61K2800/30—Characterized by the absence of a particular group of ingredients
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
- A61K2800/592—Mixtures of compounds complementing their respective functions
- A61K2800/5922—At least two compounds being classified in the same subclass of A61K8/18
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
Abstract
The invention provides composite mica powder with oil control performance for cosmetics and a preparation method thereof. The composite mica powder is prepared by coating zinc oxide and hydroxyapatite on the surface of cosmetic-grade mica powder, wherein the weight ratio of the zinc oxide to the hydroxyapatite to the cosmetic-grade mica powder is (1-30): (1-30): 100. the invention takes the large-size and high-diameter-thickness ratio sheet-shaped structural material mica as a carrier, and coats a zinc oxide and hydroxyapatite composite layer on the carrier to form a multifunctional composite material with stable structure, which has the selective adsorption capacity of high-strength unsaturated fatty acid (the main component of grease in human sweat) without adsorbing other grease substances in the formula of cosmetics; rapidly solidifying unsaturated fatty acid in sebum; the color is not dark after oil absorption, and the like. Thereby making the makeup more permanent.
Description
Technical Field
The invention relates to composite mica powder with oil control performance for cosmetics and a preparation method thereof, belonging to the technical field of cosmetic raw materials.
Background
In contemporary society, almost every woman and some men make up before going out or engaging in important activities. However, as the time after makeup is extended, it is difficult to keep the makeup as it is. The reason for this is that the skin surface of a human body naturally secretes oil, and particularly in summer, excessive sebum causes makeup falling and affects the makeup effect, so that the cosmetic system needs an oil control function, otherwise, the cosmetic system has dark color and poor greasiness, floating powder and other adverse phenomena, so people usually use fixed makeup powder such as pressed powder or loose powder to adsorb the oil on the skin surface.
In various makeup powders appearing in the market at present, the oil control function is mostly realized by using porous functional powder, such as porous silicon dioxide, porous polymethyl methacrylate or metal salts with strong oil absorption capacity. However, all oil-absorbing materials suffer from makeup removal and "shine" phenomena when sebum is excessively secreted, while porous silica absorbs not only oil but also moisture, and therefore drying of the skin is inevitable; the porous polymethyl methacrylate has poor oil absorption performance due to small pore diameter; metal salts and the like have problems that spreadability is insufficient, and that peeling easily occurs due to rough feel when applied to the skin or poor water resistance.
Zinc oxide is mainly used as a physical sun-screening agent and an astringent in cosmetics and skin care products, and blister has partial effects of fungus preparation and drying and has certain covering power. Nanometer zinc oxide is an important and widely used physical sun-screening agent in cosmetics, and the principle of screening ultraviolet rays is to absorb and scatter the ultraviolet rays. It is known that, in cosmetics, except for differences in brand formulas, most of BB cream, foundation, CC cream, sunscreen cream (also sunscreen cream), anti-radiation cream, and the like are zinc oxide. Relevant experimental data show that the ultraviolet shielding capacity of the nano zinc oxide is higher than that of the commonly used nano titanium dioxide within the wavelength of 355-380 nm. Due to this characteristic, nano zinc oxide is gradually applied to cosmetics.
Therefore, the use of monomer free non-nano zinc oxide and nano zinc oxide in cosmetics is increasingly limited and faces the risk of gradual elimination
The hydroxyapatite is calcium apatite (Ca)5(PO4)3(OH)) natural minerals. Consists of hydroxyl and apatite. Is the main inorganic component of human and animal bones. Is in hexagonal crystal form, has specific gravity of 3.08 and Mohs hardness of 5. Simple hydroxyapatite is generally used as a bone substitute materialThe calcium supplement is widely applied to the preparation of new advanced materials of artificial teeth or bone components at present.
Hydroxyapatite has calcium ion (Ca) due to its special structure2+) Easily bond with carboxyl (ROO-) in unsaturated fatty acid (main oil component of human sweat) to form stable chemical bond, thereby selectively absorbing the unsaturated fatty acid. The structure and the mechanism of selective adsorption of unsaturated fatty acid by hydroxyapatite are shown in figure 1:
in recent years, some patent publications describe a sebum gelation technique using particulate zinc oxide, which has adsorbability to free fatty acids, diglycerides, triglycerides and the like, and which effectively avoids "oily finish" by forming a zinc salt thereof to coagulate sebum. The prior art mainly has the following problems:
1. after the mica powder, the hydroxyapatite and the zinc oxide are directly physically mixed at a high speed, the selective absorption capacity to unsaturated fatty acid is not available, and the mixture can not be solidified and solidified after oil absorption.
2. The particle size of the fine zinc oxide particle is extremely fine, the original particle exists in a nano form, the fine zinc salt particle formed by the fine zinc oxide particle and sebum has certain solubility in grease, and the gelation effect is greatly weakened. With the risk that the nanoparticles are easily inhaled.
3. The superfine particle size of the zinc oxide belongs to free zinc oxide, is restricted by more and more laws and regulations in the main cosmetic application market (such as European Union and southeast Asia), and belongs to a product which is gradually eliminated.
Therefore, there is a need to develop a new zinc oxide preparation method, which can fix and deposit zinc oxide particles on a large-sized carrier, reduce the inhalation hazard of the zinc oxide particles, and solve the legal and regulatory risks of zinc oxide in the cosmetic field.
Disclosure of Invention
The invention aims to solve the technical problem of providing composite mica powder for cosmetics with oil control performance and a preparation method thereof, wherein the method takes a large-size and high-diameter-thickness ratio sheet-shaped structural material mica as a carrier, and a zinc oxide and hydroxyapatite composite layer is coated on the carrier to form a multifunctional composite material with a stable structure, and the multifunctional composite material has the selective adsorption capacity of high-strength unsaturated fatty acid (the main component of oil in human sweat) and cannot adsorb other oil substances in a cosmetic formula; rapidly solidifying unsaturated fatty acid in sebum; the color is not dark after oil absorption. Thereby making the makeup more permanent. The preparation method adopts the zinc oxide, the hydroxyapatite with good biocompatibility, the natural and nontoxic mica and the like to be matched for use, avoids using the surfactant and the organic reagent, meets the system requirement of the cosmetics, and has better product safety performance. Meanwhile, the zinc oxide is chemically deposited on the surface of the mica, is not in a free state, is not easy to absorb and has no related risks of laws and regulations. According to the invention, the scanning X-ray diffraction (XRD) is used for confirming the result that zinc oxide and hydroxyapatite are deposited on the surface of mica through chemical reaction in the technical route of the invention, and the appearance observation of the composite mica powder is carried out through an electron microscope (SEM), so that the result that zinc oxide and hydroxyapatite are chemically deposited on the surface of mica is also verified.
The above purpose is realized by the following technical scheme:
the composite mica powder for cosmetics with oil control performance is prepared by coating zinc oxide and hydroxyapatite on the surface of cosmetic-grade mica powder, wherein the weight ratio of the zinc oxide to the hydroxyapatite to the cosmetic-grade mica powder is (1-30): (1-30): 100.
The cosmetic composite mica powder with oil control performance has the particle size of 1-60 mu m.
The mica powder is one or more of sericite, muscovite, phlogopite and artificially synthesized fluorophlogopite.
The preparation method of the composite mica powder with oil control performance for cosmetics comprises the following steps:
(1) weighing mica powder for cosmetics, sodium carbonate and water, mixing and stirring;
(2) weighing anhydrous calcium chloride and dissolving the anhydrous calcium chloride in water;
(3) weighing diammonium hydrogen phosphate, dissolving in water, and adjusting the pH value to 10 by using sodium hydroxide;
(4) weighing zinc nitrate hexahydrate and dissolving in water;
(5) weighing sodium hydroxide and dissolving in water;
(6) slowly adding the calcium chloride solution obtained in the step (2) into the reaction system in the step (1), and stirring for reaction;
(7) slowly adding the diammonium hydrogen phosphate solution obtained in the step (3) into the reaction system in the step (6), and stirring for reaction;
(8) transferring the mixed solution obtained in the step (7) into a specific closed container, and carrying out hydrothermal reaction at 100-200 ℃ for 1-100 hours;
(9) cooling the mixed solution obtained in the step (8) to be below 100 ℃, and adding the zinc nitrate solution obtained in the step (4) into a reaction system;
(10) slowly adding the sodium hydroxide solution obtained in the step (5) into the mixed solution obtained in the step (9), and carrying out hydrothermal reaction at 100-200 ℃ for 1-100 hours;
(11) and (5) washing and filtering the mixed solution obtained in the step (8), collecting a filter cake and drying to obtain the composite mica powder with the oil control function for cosmetics.
The preparation method of the cosmetic composite mica powder with oil control performance comprises the following steps of: 100:(200-600): (0.5-16):(0.6-17):(0.4-12):(3.6-110):(1-30).
According to the preparation method of the composite mica powder with oil control performance for cosmetics, the molar concentration of the sodium carbonate solution, the calcium chloride solution, the diammonium phosphate solution and the zinc nitrate solution is 0.1-2 mol/L.
According to the preparation method of the composite mica powder for cosmetics with the oil control performance, the washing water in the step (11) is pure water with the conductivity of less than or equal to 10 mu S/cm, and the conductivity of the mixed solution of the washed composite mica powder is less than or equal to 50 mu S/cm, so that the product is ensured not to contain other free ions.
According to the preparation method of the composite mica powder with the oil control performance for cosmetics, the filter cake is dried and broken up at the temperature of 100-300 ℃.
The invention has the beneficial effects that:
(1) according to the invention, cosmetic-grade mica powder is used as a matrix, hydroxyapatite and zinc oxide are deposited on the surface of the mica powder, and the composite material fully utilizes the flaky characteristic of high aspect ratio of mica, so that the zinc oxide is fixed on a large-size carrier, the solubility of the zinc oxide is reduced, and the suction hazard is reduced;
(2) the mica surface is coated with zinc oxide and hydroxyapatite to form a multifunctional composite material with a stable structure, and the multifunctional composite material is applied to cosmetics and can directionally and selectively absorb grease secreted by skin and flocculate and solidify the grease, so that the makeup is more durable;
(3) the cosmetic is matched with hydroxyapatite, natural nontoxic mica and the like with good biocompatibility, so that the use of a surfactant and an organic reagent is avoided, and the safety requirement of a cosmetic system is met;
(4) reagents used in the preparation process are common medicines, the price is low, the reagents are easy to obtain, the preparation process is simple, safe and reliable, the product has good potential application value in other related scientific fields, and the cost performance is high.
Drawings
FIGS. 1(a), (b) and (c) are a structural diagram of hydroxyapatite, a structural diagram of unsaturated fatty acid (oleic acid), and a mechanism diagram of hydroxyapatite selectively adsorbing unsaturated fatty acid, respectively, which are introduced in the background of the present invention;
fig. 2 is an XRD spectrum of the composite mica powder obtained according to the method of example 1, and from the XRD spectrum of fig. 2, mica, sodium carbonate, anhydrous calcium chloride, diammonium hydrogen phosphate, zinc nitrate hexahydrate and sodium hydroxide are mixed according to the method and ratio of example 1 to form composite mica powder of hydroxyapatite, zinc oxide particles and mica;
FIG. 3 is an SEM photograph of the composite mica powder obtained by the method of example 1, wherein a is the SEM image magnified 1000 times; b1 and b2 are photographs of SEM at 2000 x magnification, respectively; c1 and c2 are photographs at 5000 × SEM magnification, respectively; d is a SEM picture magnified by 10000 times, and the SEM picture clearly shows that hydroxyapatite and zinc oxide particles produced by reaction are deposited on the surface of the flaky mica;
fig. 4 is an oil absorption capacity test of the composite mica powder obtained according to the method of example 1 in oleic acid, white oil, silicone oil, glycerin, squalane, 2EHP, respectively, wherein fig. 4(a) shows a photograph of the composite mica powder obtained according to the method of example 1 as soon as oleic acid, white oil, silicone oil, glycerin, squalane, 2EHP are added; fig. 4(b) shows a photograph of the composite mica powder obtained by the method of example 1, which is added into oleic acid, white oil, silicone oil, glycerol, squalane, and 2EHP, respectively, shaken fully for 60 times, and left to stand for 60 seconds; fig. 4(c) shows a photograph of the composite mica powder obtained according to the method of example 1, which was added to oleic acid, white oil, silicone oil, glycerol, squalane, and 2EHP, respectively, shaken well for 60 times, left for 60 seconds, and transferred to a glass petri dish. The above pictures show that the composite mica powder of the invention has significant selective oil absorption on oleic acid, and can be rapidly solidified after absorption, without absorbing 26# white oil, silicone oil (polydimethylsiloxane, 20CS), glycerol, squalane and 2EHP (isooctyl palmitate).
Fig. 5 is a comparison graph of a test of a formula in which the composite mica powder of the present invention is added to a cosmetic, the formula having a stronger absorption capacity for oleic acid than the formula in which the composite mica powder of the present invention is not added, wherein fig. 5(a) is a diffusion diameter of oleic acid after 15 seconds, fig. 5(b) is a diffusion diameter of oleic acid after 5 minutes, fig. 5(c) is a diffusion diameter of oleic acid after 15 minutes, and fig. 5(d) is a diffusion diameter of oleic acid after 30 minutes, and it can be seen from fig. 5 that the formula in which the composite mica powder of the present invention is added to a cosmetic has a significant oil control effect than the formula in which the composite mica powder of the present invention is not added.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1:
a preparation method of composite mica powder with oil control performance for cosmetics comprises the following specific steps:
weighing 1000g of cosmetic-grade synthetic mica powder and 53g of sodium carbonate, adding 2500ml of water, and uniformly stirring;
weighing 55g of anhydrous calcium chloride, dissolving the anhydrous calcium chloride in 500ml of water, slowly dripping the anhydrous calcium chloride into the mica mixed solution under stirring, and continuously stirring for 1 hour;
weighing 40g of diammonium hydrogen phosphate, dissolving in 500ml of water, adjusting the pH value to 10 by using sodium hydroxide, slowly dropping into the mica mixed solution under stirring, and continuously stirring for 1 hour;
transferring the mica mixed solution into a specific closed container, reacting at high temperature and high pressure for 24 hours, and cooling to below 100 ℃;
365g of zinc nitrate hexahydrate is weighed and dissolved in 1000ml of water;
weighing 98g of sodium hydroxide, dissolving in 500ml of water, slowly dripping into the mica mixed solution under stirring, continuously stirring for 1 hour, and reacting for 4 hours under high temperature and high pressure;
and filtering the obtained mixed solution, washing the mixed solution by using pure water until the conductivity is less than or equal to 10 mu S/cm, collecting a filter cake, drying the filter cake at 280 ℃, and scattering the filter cake to obtain the composite mica powder for cosmetics with the oil control function.
Examples test methods for the samples obtained:
(1) x-ray diffraction (XRD) test method
The test is carried out according to SY/T5163-2018X-ray diffraction analysis method for clay minerals and common non-clay minerals in sedimentary rocks. The test results are shown in fig. 2.
(2) Electron Microscope (SEM) testing method
The test photograph is shown in FIG. 3 according to GB/T36422-2018 scanning electron microscopy for measuring the microstructure and diameter of the chemical fiber.
(3) Oil absorption test method
Weighing 5g of sample, placing on a flat glass, dripping refined linseed oil (or oleic acid), pressing and grinding by using a knife adjustment in the process to enable the oil to permeate into the sample until the sample forms a paste with uniform consistency. The greater the oil absorption test data, the greater the oil absorption capacity, and the test data are shown in table 1:
TABLE 1 oil absorption and oil absorption set time
Remarks are as follows: the proportions of hydroxyapatite, zinc oxide and mica powder in the mixed sample are the same as those in the embodiment, and the mixing method comprises the following steps: the speed of rotation is 3000 rpm, the mixing time is 25 minutes.
(4) Selective oil absorption capacity and oil absorption setting time
Weighing 2g of powder at the room temperature of 30 ℃, adding the powder into a transparent glass container containing 6g of distilled water and 12g of oil phase, sealing, fully swinging and vibrating for 60 times, standing, inclining the glass container, observing whether the oleic acid and the powder are solidified or not and the solidification time, and transferring a sample in the transparent glass bottle to a glass culture dish for observation. This example uses oleic acid, 26# white oil, silicone oil (20 CS), glycerin, squalane, 2EHP (isooctyl palmitate) six cosmetic commonly used oil phases to verify the selective absorption capacity of the oil phase, using 6g distilled water +12g oleic acid to simulate unsaturated fatty acids and moisture in human sweat. And (3) testing the oil absorption solidification time, wherein the shorter the solidification time is, the stronger the oil absorption solidification capability is. The test results are shown in fig. 4.
(5) Permeability of oleic acid
The method comprises the following steps: 0.7g of cosmetic formulation powder was weighed and spread evenly over an area of 28cm2The transparent glass plate of (2) was pressed with powder, 15. mu.g of oleic acid was injected onto the surface of the pressed powder using a precision pipette, the dispersion of oleic acid was observed, and the diameter of the dispersed oleic acid was measured. The smaller the oleic acid diffusion diameter, the stronger the adsorption capacity for oleic acid. The cosmetic formulation powder formulations in this test are shown in table 2. Wherein the compound mica powder is not added in the formula A, and the compound mica powder is added in the formula BThe test results of the mother powder are shown in FIG. 5.
TABLE 2 formulation of powder for cosmetic formulation
The technical scheme disclosed by the invention is not limited to the technical means disclosed by the technical characteristics, and also comprises the technical scheme formed by equivalent replacement of the technical characteristics. The present invention is not limited to the details given herein, but is within the ordinary knowledge of those skilled in the art.
Claims (5)
1. A preparation method of cosmetic composite mica powder with oil control performance comprises the following steps of coating zinc oxide and hydroxyapatite on the surface of cosmetic mica powder, wherein the weight ratio of the zinc oxide to the hydroxyapatite to the cosmetic mica powder is (1-30): (1-30): 100; the mica powder is one or a mixture of more than one of sericite, muscovite, phlogopite and artificially synthesized fluorophlogopite; the particle size of the cosmetic-grade mica powder is 1-60 mu m;
the method is characterized in that: the method comprises the following steps:
(1) weighing mica powder for cosmetics, sodium carbonate and water, mixing and stirring;
(2) weighing anhydrous calcium chloride and dissolving in water;
(3) weighing diammonium hydrogen phosphate, dissolving in water, and adjusting the pH value to 10 by using sodium hydroxide;
(4) weighing zinc nitrate hexahydrate and dissolving in water;
(5) weighing sodium hydroxide and dissolving in water;
(6) slowly adding the calcium chloride solution obtained in the step (2) into the reaction system in the step (1), and stirring for reaction;
(7) slowly adding the diammonium hydrogen phosphate solution obtained in the step (3) into the reaction system in the step (6), and stirring for reaction;
(8) transferring the mixed solution obtained in the step (7) into a specific closed container, and carrying out hydrothermal reaction at 100-200 ℃ for 1-100 hours;
(9) cooling the mixed solution obtained in the step (8) to be below 100 ℃, and adding the zinc nitrate solution obtained in the step (4) into a reaction system;
(10) slowly adding the sodium hydroxide solution obtained in the step (5) into the mixed solution obtained in the step (9), and carrying out hydrothermal reaction at 100-200 ℃ for 1-100 hours;
(11) and (4) washing and filtering the mixed solution obtained in the step (8), collecting a filter cake and drying to obtain the composite mica powder with the oil control function for cosmetics.
2. The method for preparing the composite mica powder with oil control performance for cosmetics according to claim 1, which is characterized in that: the cosmetic-grade mica powder, sodium carbonate, water, anhydrous calcium chloride, diammonium hydrogen phosphate, zinc nitrate hexahydrate and sodium hydroxide are in a mass ratio of: 100:(200-600)(0.5-16):(0.6-17):(0.4-12):(3.6-110):(1-30).
3. The method for preparing the composite mica powder with oil control performance for cosmetics according to claim 1, which is characterized in that: the molar concentration of the sodium carbonate, the calcium chloride, the diammonium hydrogen phosphate and the zinc nitrate solution is 0.1-2 mol/L.
4. The washing of the composite mica powder mixed solution for cosmetics according to claim 1, wherein the water for washing in step (11) is pure water with conductivity of 10 μ S/cm or less, and the conductivity of the mixed composite mica powder mixed solution after washing is 50 μ S/cm or less, so as to ensure that the product does not contain other free ions.
5. The method for preparing the composite mica powder with oil control performance for cosmetics according to claim 1, which is characterized in that: the filter cake is dried and broken up at the temperature of 100-300 ℃.
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Address after: 239000, No. 18, Guanghui Road, Yaopu Town, Nanqiao District, Chuzhou City, Anhui Province Applicant after: Anhui Gerui New Material Technology Co.,Ltd. Address before: 239000, No. 18, Guanghui Road, Yaopu Town, Nanqiao District, Chuzhou City, Anhui Province Applicant before: CHUZHOU GREA MINERALS Co.,Ltd. |
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