CN108977024B - Low-VOC (volatile organic compound) double-component solvent-based finish paint and preparation method thereof - Google Patents
Low-VOC (volatile organic compound) double-component solvent-based finish paint and preparation method thereof Download PDFInfo
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- CN108977024B CN108977024B CN201810726094.9A CN201810726094A CN108977024B CN 108977024 B CN108977024 B CN 108977024B CN 201810726094 A CN201810726094 A CN 201810726094A CN 108977024 B CN108977024 B CN 108977024B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
Abstract
The invention provides a low VOC bi-component solvent-based finish paint, which consists of a component A and a component B with equal weight; the component A comprises the following components in parts by weight: 20-40 parts of titanium dioxide, 0.5-3 parts of wetting dispersant, 0.1-1 part of anti-settling agent, 50-60 parts of acrylic resin, 0.1-1 part of acrylate leveling agent, 0.05-0.3 part of organic silicon leveling agent, 0.01-0.05 part of drier, 1-5 parts of butyl acetate and 5-10 parts of propylene glycol methyl ether acetate; the component B comprises the following components in parts by weight: 50-70 parts of isocyanate, 10-20 parts of butyl acetate and 10-30 parts of propylene glycol methyl ether acetate. The invention also provides a preparation method of the low VOC bi-component solvent-based finish paint. The low-VOC bi-component solvent-based finish paint provided by the invention has lower VOC content and viscosity and higher drying speed.
Description
Technical Field
The invention relates to a bi-component solvent-based finish paint, in particular to a low-VOC bi-component solvent-based finish paint and a preparation method thereof.
Background
The solvent type acrylic paint has excellent weather resistance and high mechanical performance, and is a kind of paint which is developed quickly at present. The solvent-based acrylic paint can be classified into a self-drying type acrylic paint (thermoplastic type) and a crosslinking curing type acrylic paint (thermosetting type), the former being a non-conversion type coating and the latter being a conversion type coating. The cross-linking curing type acrylic coating is generally of a two-component type, mainly comprises acrylic amino paint, acrylic polyurethane paint, acrylic alkyd paint, radiation curing acrylic coating and the like, and is widely applied to the aspects of automobile coating, electric appliance coating, wood coating, building coating and the like. The cross-linking curing type acrylic paint generally has high solid content, can obtain a thick coating film by one-time coating, has excellent mechanical property, and can be prepared into paint with high weather resistance, high fullness, high elasticity and high hardness.
Chinese patent with application number CN201510479204.2 provides a bi-component acrylic acid high-gloss weather-resistant ultraviolet-resistant finish paint which comprises a component A and a component B; the component A comprises: 30-60 parts of acrylic resin, 8-15 parts of solvent, 2-8 parts of pigment, 8-15 parts of nano cerium dioxide and 35-50 parts of auxiliary agent; the component B comprises: 15-25 parts of low molecular weight polyamide and 1-3 parts of phenol. The patent has problems that the VOC content and viscosity are high and the drying speed is slow.
Disclosure of Invention
The invention aims to provide a low-VOC bi-component solvent-based finish paint which has lower VOC content and viscosity and higher drying speed.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a low VOC bi-component solvent-based finish paint is composed of a component A and a component B which are equal in weight; the component A comprises the following components in parts by weight: 20-40 parts of titanium dioxide, 0.5-3 parts of wetting dispersant, 0.1-1 part of anti-settling agent, 50-60 parts of acrylic resin, 0.1-1 part of acrylate leveling agent, 0.05-0.3 part of organic silicon leveling agent, 0.01-0.05 part of drier, 1-5 parts of butyl acetate and 5-10 parts of propylene glycol methyl ether acetate; the component B comprises the following components in parts by weight: 50-70 parts of isocyanate, 10-20 parts of butyl acetate and 10-30 parts of propylene glycol methyl ether acetate.
Further, the invention consists of a component A and a component B which are equal in weight; the component A comprises the following components in parts by weight: 30 parts of titanium dioxide, 0.8 part of wetting dispersant, 0.3 part of anti-settling agent, 55 parts of acrylic resin, 0.5 part of acrylate leveling agent, 0.1 part of organic silicon leveling agent, 0.05 part of drier, 4 parts of butyl acetate and 9.15 parts of propylene glycol methyl ether acetate; the component B comprises the following components in parts by weight: 60 parts of isocyanate, 15 parts of butyl acetate and 25 parts of propylene glycol methyl ether acetate.
Further, the titanium dioxide is rutile titanium dioxide.
Further, the wetting dispersant of the invention is BYK-110.
Further, the anti-settling agent is degussa R972 fumed silica.
Further, the acrylic resin is high-solid low-viscosity acrylic resin.
Further, the drier provided by the invention comprises an organotin drier and zinc fatty acid in a weight ratio of 2:1, and the preparation step of the zinc fatty acid comprises the following steps:
A1. placing okra seeds in a drying oven at 60 ℃ for drying to constant weight, taking out and crushing, sieving with a 50-mesh sieve to obtain okra seed powder, adding the okra seed powder into petroleum ether with the weight being 10 times that of the okra seed powder, placing the okra seed powder in a microwave oven with the power of 600W, performing microwave extraction for 10 minutes to obtain an extracting solution, performing suction filtration on the extracting solution to obtain a filtrate, concentrating the filtrate under reduced pressure, and drying at 100 ℃ to constant weight to obtain fatty acid;
A2. and D, adding the fatty acid obtained in the step A1 and 1, 4-dioxane into a reaction bottle, stirring and heating to 75 ℃, adding zinc oxide into the reaction bottle, heating to 110 ℃, preserving heat and reacting for 3.5 hours to obtain a reactant, distilling the reactant under reduced pressure, and drying at 100 ℃ to constant weight to obtain the zinc fatty acid.
Further, the isocyanates according to the invention consist of equal amounts by weight of HDI and IPDI.
The invention also aims to provide a preparation method of the low-VOC bi-component solvent-based finish paint.
In order to solve the technical problems, the technical scheme is as follows:
a preparation method of a low VOC bi-component solvent-based finish paint comprises the following preparation steps:
B1. weighing the components in parts by weight, adding butyl acetate and propylene glycol monomethyl ether acetate into a stirring kettle, and stirring for 3-5 minutes at the rotating speed of 390-;
B2. adding the wetting dispersant into a stirring kettle, and stirring for 3-5 minutes at the rotating speed of 390-;
B3. adding acrylic resin into a stirring kettle, and stirring for 3-5 minutes at the rotating speed of 390-;
B4. adding titanium dioxide and an anti-settling agent into a stirring kettle, stirring at the rotating speed of 1390-;
B5. adding other components into a stirring kettle, and stirring for 10 minutes at the rotating speed of 390 plus 410 rpm to obtain a component A;
the preparation steps of the component B are as follows:
C1. weighing the components in parts by weight, adding butyl acetate and propylene glycol monomethyl ether acetate into a stirring kettle, and stirring for 3-5 minutes at the rotating speed of 390-;
C2. adding isocyanate into a stirring kettle, and stirring for 15 minutes at the rotating speed of 590-610 rpm to obtain the component B.
Compared with the prior art, the invention has the following beneficial effects:
1) the invention selects the proper wetting dispersant, can effectively improve the dispersion efficiency, reduce the viscosity of the finish paint, has low construction viscosity during paint preparation, does not need to add a diluent for spraying, and can also effectively reduce the VOC content.
2) The invention selects the high-solid low-viscosity hydroxyl acrylic resin and the high-solid low-viscosity isocyanate to match, can further reduce the content of VOC with high viscosity (less than or equal to 420g/L), and has high solid content.
3) The invention selects the proper drier-organic tin catalyst and fatty acid zinc, can effectively improve the drying speed, improves the drying speed by more than 30 percent compared with the conventional low VOC coating, and has good paint film appearance and high fullness.
4) The zinc fatty acid used in the invention is prepared by drying and crushing okra seeds, taking petroleum ether as an extraction solvent, preparing fatty acid through microwave assistance, and reacting the fatty acid with zinc oxide, so that the drying speed can be improved, and the compatibility among other components can be improved, thereby further reducing the VOC content; in addition, the sunflower seeds are food waste, and the invention recycles the sunflower seeds as a raw material to prepare the finish paint, thereby having good environmental protection and economic value.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, and the exemplary embodiments and descriptions thereof herein are provided to explain the present invention but not to limit the present invention.
Examples 1 to 4
Preparing a component A of the finishing paint according to the proportion (in parts by weight) in the table 1, preparing a component B of the finishing paint according to the proportion (in parts by weight) in the table 2, wherein the weight ratio of the component A to the component B is 1:
TABLE 1
Wherein the drier consists of organotin drier and fatty acid zinc in a weight ratio of 2: 1. The preparation method of the fatty acid zinc comprises the following steps:
A1. placing okra seeds in a drying oven at 60 ℃ for drying to constant weight, taking out and crushing, sieving with a 50-mesh sieve to obtain okra seed powder, adding the okra seed powder into petroleum ether with the weight being 10 times that of the okra seed powder, placing the okra seed powder in a microwave oven with the power of 600W, performing microwave extraction for 10 minutes to obtain an extracting solution, performing suction filtration on the extracting solution to obtain a filtrate, concentrating the filtrate under reduced pressure, and drying at 100 ℃ to constant weight to obtain fatty acid;
A2. and D, adding the fatty acid obtained in the step A1 and 1, 4-dioxane into a reaction bottle, stirring and heating to 75 ℃, adding zinc oxide into the reaction bottle, heating to 110 ℃, preserving heat and reacting for 3.5 hours to obtain a reactant, distilling the reactant under reduced pressure, and drying at 100 ℃ to constant weight to obtain the zinc fatty acid.
The preparation of the component A of example 1 comprises the following steps:
B1. weighing the components in parts by weight, adding butyl acetate and propylene glycol monomethyl ether acetate into a stirring kettle, and stirring for 4 minutes at the rotating speed of 400 revolutions per minute;
B2. adding the wetting dispersant into a stirring kettle, and stirring for 4 minutes at the rotating speed of 400 revolutions per minute;
B3. adding acrylic resin into a stirring kettle, and stirring for 4 minutes at the rotating speed of 400 revolutions per minute;
B4. adding titanium dioxide and an anti-settling agent into a stirring kettle, stirring at the rotating speed of 1400 revolutions per minute for 30 minutes until the fineness of the mixed material is lower than 15 mu m, and stopping stirring;
B5. adding other components into a stirring kettle, and stirring at the rotating speed of 400 rpm for 10 minutes to obtain a component A.
The preparation procedure for the a component of example 2 differs from example 1 in that: the rotating speeds in the steps B1, B2 and B3 are all 390 rpm, and the stirring time is 5 minutes; the rotating speed in the step B4 is 1390 rpm, and the stirring time is 40 minutes; the rotation speed in step B5 was 390 rpm.
The preparation procedure for the a component of example 3 differs from example 1 in that: the rotating speeds in the steps B1, B2 and B3 are all 410 r/min, and the stirring time is all 3 minutes; the rotating speed in the step B4 is 1410 rpm, and the stirring time is 20 minutes; the rotation speed in step B5 was 410 rpm.
The preparation procedure for the a component of example 4 differs from example 1 in that: the rotating speeds in the steps B1, B2 and B3 are all 395 rpm, and the stirring time is all 4.5 minutes; the rotating speed in the step B4 is 1395 rpm, and the stirring time is 35 minutes; the rotation speed in step B5 was 395 rpm.
TABLE 2
Wherein the isocyanate consists of HDI and IPDI in equal weight.
The preparation steps of the component B of the embodiment 1 are as follows:
C1. weighing the components in parts by weight, adding butyl acetate and propylene glycol monomethyl ether acetate into a stirring kettle, and stirring for 4 minutes at the rotating speed of 400 revolutions per minute;
C2. adding isocyanate into a stirring kettle, and stirring for 15 minutes at the rotating speed of 600 revolutions per minute to obtain a component B.
The preparation procedure for the b component of example 2 differs from that of example 1 in that: the rotating speed in the step C1 is 390 rpm, and the stirring time is 5 minutes; the rotation speed in step C2 is 590 rpm.
The preparation procedure for the b component of example 3 differs from example 1 in that: the rotating speed in the step C1 is 410 r/min, and the stirring time is 3 minutes; the rotation speed in step C2 was 610 rpm.
The preparation procedure for the b component of example 4 differs from example 1 in that: the rotating speed in the step C1 is 395 rpm, and the stirring time is 4.5 minutes; the rotation speed in step C2 was 595 rpm.
Reference example 1
The wetting dispersant used was a general polyester-based dispersant, and other components and preparation method were the same as in example 1.
Reference example 2
The high-solid low-viscosity acrylic resin is replaced by the common acrylic resin, and other components and the preparation method are the same as those of the example 1.
Reference example 3
The isocyanate used TDI, the other components and the preparation method were the same as those of example 1.
Reference example 4
The drier does not include zinc fatty acid, and other components and preparation method are the same as example 1.
Comparative example
The comparative example is example 1 of the chinese invention having application number CN 201510479204.2.
The first experimental example: VOC content testing
The VOC content of each topcoat was tested by gas chromatography according to industry standard HJ/T201-2005 and the test results are shown in Table 3.
TABLE 3
As is apparent from Table 3, inventive examples 1-4 all have lower VOC levels than the comparative example, with example 1 having the lowest VOC level. Some of the components of reference examples 1 to 4 were different from those of example 1 in that the VOC contents of reference examples 1 to 4 were increased to various degrees, indicating that the VOC contents of the wetting dispersant BYK-110, the high-solid low-viscosity acrylic resin, the isocyanate composed of HDI and IPDI in equal amounts by weight, and the zinc fatty acid were all effectively reduced.
Experiment example two: viscosity measurement
The viscosity of each topcoat was measured in a 25 ℃ circulating water bath using a rotational viscometer and the results are shown in table 4:
| viscosity (mPa. s) | |
| Example 1 | 706 |
| Example 2 | 709 |
| Example 3 | 713 |
| Example 4 | 710 |
| Reference example 1 | 728 |
| Reference example 2 | 733 |
| Reference example 3 | 730 |
| Reference example 4 | 711 |
| Comparative example | 787 |
TABLE 4
As is apparent from Table 4, the viscosities of inventive examples 1-4 are all lower than the comparative example, with example 1 having the lowest viscosity. The compositions of reference examples 1 to 4 are partially different from those of reference example 1, in which the viscosities of reference examples 1 to 3 are increased to different extents, and thus it is demonstrated that the wetting dispersant BYK-110, the high-solid low-viscosity acrylic resin, and the isocyanate composed of HDI and IPDI in equal amounts by weight are effective in reducing the viscosities; the viscosity of reference example 4 was comparable to examples 1-4, indicating that zinc fatty acid had no effect on viscosity.
Experiment example three: drying speed test
The surface drying time of each finish paint is tested by referring to GB/T1725-1979, the shorter the surface drying time is, the faster the drying speed is, and the test results are shown in Table 5:
| open time (minutes) | |
| Example 1 | 16 |
| Example 2 | 19 |
| Example 3 | 17 |
| Example 4 | 18 |
| Reference example 1 | 16 |
| Reference example 2 | 19 |
| Reference example 3 | 18 |
| Reference example 4 | 28 |
| Comparative example | 39 |
TABLE 5
As is apparent from Table 5, the tack-free times for inventive examples 1-4 are all shorter than for the comparative example, indicating that the invention has a faster drying rate, with example 1 being the fastest. The partial compositions of reference examples 1 to 4 are different from example 1 in that the tack-free time of reference example 4 is increased by a large amount, indicating that zinc fatty acid is effective in increasing the drying rate; the tack-free times of reference examples 1 to 3 are comparable to those of examples 1 to 4, and show that the wetting dispersant BYK-110, the high-solids low-viscosity hydroxy acrylic resin, and the isocyanate composed of equal amounts by weight of HDI and IPDI have no influence on the drying rate.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (5)
1. A low VOC bi-component solvent-based finish paint is characterized in that: consists of a component A and a component B with equal weight; the component A comprises the following components in parts by weight: 20-40 parts of titanium dioxide, 0.5-3 parts of wetting dispersant, 0.1-1 part of anti-settling agent, 50-60 parts of acrylic resin, 0.1-1 part of acrylate leveling agent, 0.05-0.3 part of organic silicon leveling agent, 0.01-0.05 part of drier, 1-5 parts of butyl acetate and 5-10 parts of propylene glycol methyl ether acetate; the component B comprises the following components in parts by weight: 50-70 parts of isocyanate, 10-20 parts of butyl acetate and 10-30 parts of propylene glycol methyl ether acetate; the wetting dispersant is BYK-110; the isocyanate consists of HDI and IPDI in equal weight; the acrylic resin is high-solid low-viscosity hydroxyl acrylic resin; the drier consists of organotin drier and zinc fatty acid in a weight ratio of 2:1, and the preparation method of the zinc fatty acid comprises the following steps:
A1. placing okra seeds in a drying oven at 60 ℃ for drying to constant weight, taking out and crushing, sieving with a 50-mesh sieve to obtain okra seed powder, adding the okra seed powder into petroleum ether with the weight being 10 times that of the okra seed powder, placing the okra seed powder in a microwave oven with the power of 600W, performing microwave extraction for 10 minutes to obtain an extracting solution, performing suction filtration on the extracting solution to obtain a filtrate, concentrating the filtrate under reduced pressure, and drying at 100 ℃ to constant weight to obtain fatty acid;
A2. and D, adding the fatty acid obtained in the step A1 and 1, 4-dioxane into a reaction bottle, stirring and heating to 75 ℃, adding zinc oxide into the reaction bottle, heating to 110 ℃, preserving heat and reacting for 3.5 hours to obtain a reactant, distilling the reactant under reduced pressure, and drying at 100 ℃ to constant weight to obtain the zinc fatty acid.
2. The low VOC, two-component solvent-borne topcoat of claim 1, characterized by: consists of a component A and a component B with equal weight; the component A comprises the following components in parts by weight: 30 parts of titanium dioxide, 0.8 part of wetting dispersant, 0.3 part of anti-settling agent, 55 parts of acrylic resin, 0.5 part of acrylate leveling agent, 0.1 part of organic silicon leveling agent, 0.05 part of drier, 4 parts of butyl acetate and 9.15 parts of propylene glycol methyl ether acetate; the component B comprises the following components in parts by weight: 60 parts of isocyanate, 15 parts of butyl acetate and 25 parts of propylene glycol methyl ether acetate.
3. The low VOC, two-component solvent-borne topcoat of claim 1, characterized by: the titanium dioxide is rutile type titanium dioxide.
4. The low VOC, two-component solvent-borne topcoat of claim 1, characterized by: the anti-settling agent is degussa R972 fumed silica.
5. The method of preparing a low VOC two-component solvent-based topcoat as claimed in any one of claims 1 to 4, wherein: the preparation steps of the component A are as follows:
B1. weighing the components in parts by weight, adding butyl acetate and propylene glycol monomethyl ether acetate into a stirring kettle, and stirring for 3-5 minutes at the rotating speed of 390-;
B2. adding the wetting dispersant into a stirring kettle, and stirring for 3-5 minutes at the rotating speed of 390-;
B3. adding acrylic resin into a stirring kettle, and stirring for 3-5 minutes at the rotating speed of 390-;
B4. adding titanium dioxide and an anti-settling agent into a stirring kettle, stirring at the rotating speed of 1390-;
B5. adding other components into a stirring kettle, and stirring for 10 minutes at the rotating speed of 390-;
the preparation steps of the component B are as follows:
C1. weighing the components in parts by weight, adding butyl acetate and propylene glycol monomethyl ether acetate into a stirring kettle, and stirring for 3-5 minutes at the rotating speed of 390-;
C2. adding isocyanate into a stirring kettle, and stirring for 15 minutes at the rotating speed of 590-610 rpm to obtain the component B.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103013654A (en) * | 2013-01-05 | 2013-04-03 | 湖南奇异生物科技有限公司 | Okra seed oil and extraction method thereof |
| CN103666229A (en) * | 2013-11-29 | 2014-03-26 | 洛阳双瑞防腐工程技术有限公司 | High solid coating for container and preparation method of high solid coating |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103013654A (en) * | 2013-01-05 | 2013-04-03 | 湖南奇异生物科技有限公司 | Okra seed oil and extraction method thereof |
| CN103666229A (en) * | 2013-11-29 | 2014-03-26 | 洛阳双瑞防腐工程技术有限公司 | High solid coating for container and preparation method of high solid coating |
Non-Patent Citations (1)
| Title |
|---|
| 耐酸雨有机硅改性丙烯酸涂料的研制;赵琦等;《中国涂料》;20000830(第4期);第26-27，29页 * |
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Address after: The two district 529700 in Guangdong province Jiangmen city Heshan City, the ancient town of labor three industrial zone Applicant after: Yatu high tech materials Co.,Ltd. Address before: The two district 529700 in Guangdong province Jiangmen city Heshan City, the ancient town of labor three industrial zone Applicant before: YATU ADVANCED MATERIALS Co.,Ltd. |
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| GR01 | Patent grant | ||
| GR01 | Patent grant |