CN111057416A - Color paste with low odor, low viscosity and good stability and application thereof - Google Patents
Color paste with low odor, low viscosity and good stability and application thereof Download PDFInfo
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- CN111057416A CN111057416A CN201911352984.9A CN201911352984A CN111057416A CN 111057416 A CN111057416 A CN 111057416A CN 201911352984 A CN201911352984 A CN 201911352984A CN 111057416 A CN111057416 A CN 111057416A
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- color paste
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- dispersant
- acrylate
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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
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/003—Pigment pastes, e.g. for mixing in paints containing an organic pigment
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
-
- 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
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
-
- 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
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
- C09D17/005—Carbon black
-
- 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
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
- C09D17/007—Metal oxide
- C09D17/008—Titanium dioxide
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Optical Filters (AREA)
Abstract
The invention belongs to the field of materials, and discloses color paste with low odor, low viscosity and good stability, which comprises the following components in parts by weight: 55-80 parts of monomer, 3-15 parts of dispersant and 15-30 parts of pigment; the monomer is at least one of acrylate, vinyl ether or acryloyl morpholine; the dispersing agent is at least one selected from polyethylene glycol acrylate polymer, oxidized polyethylene wax, ethylene-acrylic acid copolymer or ethylene-vinyl acetate copolymer. According to the invention, by selecting a proper monomer and a proper dispersant and selecting a proper component dosage ratio, the prepared color paste has good stability, can resist the circulating treatment at the temperature of 60 ℃ and minus 10 ℃, is not layered and settled, and has the characteristics of low odor, low viscosity, high pigment content and good filtering performance. The process of preparing the color paste adopts a high-speed grinding mode to ensure that the pigment can be uniformly and stably dispersed in the color paste, thereby integrally improving the stability and the filtering performance of the color paste.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to color paste with low odor, low viscosity and good stability and application thereof.
Background
The color paste is widely applied to various inks or coatings, wherein the inks for digital printing have high requirements on the performance of the color paste.
One of the problems of the color paste in the prior art is that the pigment content in the color paste is low, so that a large amount of color paste is needed when preparing ink, and if the pigment content in the color paste is too high, the stability of the color paste is poor. In addition, the color paste in the prior art has the defects of high viscosity, poor filtering performance, large smell, poor stability particularly in storage and incapability of enduring treatment in high-temperature and low-temperature environments.
Therefore, it is desirable to provide a color paste which has the characteristics of low odor, low viscosity, high pigment content, good filtration performance and good stability.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides the color paste with low odor, low viscosity and good stability, which has the characteristics of low odor, low viscosity, high pigment content and good filtering performance, particularly good stability, can resist the cyclic treatment at the temperature of 60 ℃ and minus 10 ℃, and still does not delaminate and settle.
The color paste with low odor, low viscosity and good stability comprises the following components in parts by weight:
monomer 55-80
3-15 parts of dispersant
15-30 parts of pigment;
the monomer is selected from at least one of acrylate, vinyl ether or acryloyl morpholine;
the dispersant is a polymeric dispersant.
Preferably, the acrylate is at least one selected from the group consisting of ethoxyethoxyethyl acrylate, cyclotrimethylolpropane formal acrylate, 2-ethyleneoxyethoxy ethyl acrylate, hydroxypropyl acrylate and hydroxyethyl methacrylate.
Preferably, the vinyl ether is selected from at least one of triethylene glycol divinyl ether, or divinyl-1, 4-butanediol ether.
Preferably, the acryloyl morpholine is selected from 4-acryloyl morpholine and/or N-acryloyl morpholine.
Preferably, the dispersant is at least one selected from polyethylene glycol acrylate polymers, oxidized polyethylene wax, ethylene-acrylic acid copolymers or ethylene-vinyl acetate copolymers.
Preferably, the polyethylene glycol acrylate polymer is selected from at least one of polyethylene glycol (300) diacrylate, polyethylene glycol (200) -methacrylate, polyethylene glycol (400) -methacrylate or polyethylene glycol (600) -methacrylate.
The pigment is selected from at least one of organic pigment or inorganic pigment.
Preferably, the pigment is at least one selected from cinnabar, carbon black, realgar, malachite green, wollastonite, barite powder, talcum powder, mica powder, kaolin, alizarin red, indigo, titanium white, lithopone, lead chrome yellow, iron blue, phthalocyanine blue, quinacridone violet ER02, quinacridone red 122A (the pigment quinacridone violet ER02 and quinacridone red 122A are commercially available organic pigments), quinacridone violet 19, pigment yellow 3, pigment yellow 93 and pigment red 53: 1.
Preferably, the mass ratio of the pigment to the dispersant is 1: (0.1-1).
Preferably, when the pigment is a black pigment, the mass ratio of the pigment to the dispersant is 1: (0.6-0.8).
Preferably, when the pigment is a cyan pigment, the mass ratio of the pigment to the dispersant is 1: (0.4-0.6).
Preferably, when the pigment is a yellow pigment, the mass ratio of the pigment to the dispersant is 1: (0.8-1.0).
Preferably, when the pigment is a white pigment, the mass ratio of the pigment to the dispersant is 1: (0.1-0.2).
Preferably, the size of the pigment is 10 to 100. mu.m.
Preferably, the color paste with low odor, low viscosity and good stability comprises the following components in parts by weight:
monomer 65-78
3-10 parts of dispersant
15-25 parts of pigment.
Further preferably, the color paste with low odor, low viscosity and good stability comprises the following components in parts by weight:
monomer 75
5 portions of dispersant
And 20 parts of pigment.
A preparation method of color paste with low odor, low viscosity and good stability comprises the following steps:
(1) weighing the components according to the formula ratio, stirring and mixing the monomer and the dispersant at the stirring speed of 300-500 r/min to prepare a mixture A for later use;
(2) adding pigment into the mixture A prepared in the step (1), stirring at the stirring speed of 1000-.
Preferably, the stirring time in step (1) is 20 to 40 minutes,
preferably, the stirring time in step (2) is 50 to 70 minutes.
Preferably, the grinding conditions in the step (2) are that the diameter of zirconium beads used for grinding is 0.2-0.4mm, the filling rate of the zirconium beads is 60-80%, the linear speed of grinding is 10-12m/s, the cavity pressure is less than 0.04MPa, the discharging temperature of grinding is less than 40 ℃, and the discharging flow rate is 800-.
Preferably, the time for milling in step (2) is 2 to 12 hours.
Preferably, the grinding process further comprises a filtration process, wherein the filtration process uses a filter membrane for filtration, and the pore diameter of the filter membrane is 100-300 nm.
The high-speed grinding in the step (2) is beneficial to the uniformity of the pigment particle size, the pigment is better dispersed in the dispersing agent and the monomer, and the stability and uniformity of the color paste are improved.
The invention selects the monomer with excellent pigment wettability and the auxiliary dispersant to ensure that the pigment is wetted and wrapped to be optimal, thereby reducing the viscosity of the color paste and improving the filterability and the stability of the color paste.
The ink comprises the color paste.
The ink is applied to the printing process, and the phenomena of blockage and ink break are not easy to occur.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, by selecting a proper monomer and a proper dispersant and selecting a proper component dosage ratio, the prepared color paste has good stability, can resist the circulating treatment at the temperature of 60 ℃ and minus 10 ℃, is not layered and settled, and has the characteristics of low odor, low viscosity, high pigment content and good filtering performance.
(2) The process of preparing the color paste adopts a high-speed grinding mode to ensure that the pigment can be uniformly and stably dispersed in the color paste, thereby integrally improving the stability and the filtering performance of the color paste.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The pigments in the following examples may be Mitsubishi carbon black MA7, Kabot carbon black ML, Kabot carbon black ME, Bassfield titanium cyan 7110F, DuPont titanium dioxide R996; the dispersants used in the examples below may be lubotun 32000, lubotun 35000, lubotun 36000, lubotun 38000, lubotun J180, BYK9152, BYK9151, basf EFKA4701 (these dispersants are all polymer-based dispersants).
Example 1
The color paste with low odor, low viscosity and good stability comprises the following components in parts by weight:
75 parts of ethoxy ethyl acrylate
Lubo run 320005 parts
Marigold MA 720 parts.
The color paste is black color paste.
Example 2
The color paste with low odor, low viscosity and good stability comprises the following components in parts by weight:
75 parts of cyclotrimethylolpropane methylal acrylate
Lubo run 320005 parts
And 20 parts of BASF titanium cyan 7110F.
The color paste is blue color paste.
Example 3
The color paste with low odor, low viscosity and good stability comprises the following components in parts by weight:
75 parts of 4-acryloyl morpholine
Lubo run 350005 parts
And 20 parts of cinnabar.
The color paste is red color paste.
Example 4
The color paste with low odor, low viscosity and good stability comprises the following components in parts by weight:
75 parts of triethylene glycol divinyl ether
Luobu Rui J1805 parts
20 parts of lead chrome yellow.
The color paste is yellow color paste.
Example 5
The color paste with low odor, low viscosity and good stability comprises the following components in parts by weight:
75 parts of 2-ethyleneoxy ethoxy ethyl acrylate
Lubo run 360005 parts
And (4) 99620 parts of Dupont titanium dioxide.
The color paste is white color paste.
The color pastes of the above examples 1-5 were prepared according to the following steps:
(1) weighing the components according to the formula ratio, stirring and mixing the monomer and the dispersant at the stirring speed of 400 revolutions per minute for 30 minutes to prepare a mixture A for later use;
(2) adding pigment into the mixture A prepared in the step (1), stirring at the stirring speed of 1200 rpm to prepare a mixture B, and then adding the mixture B into a sand mill for grinding under the grinding conditions that the diameter of zirconium beads used for grinding is 0.3mm, the filling rate of the zirconium beads is 60%, the linear speed of grinding is 10m/s, the pressure of a cavity is 0.02MPa, the discharging temperature of grinding is less than 40 ℃, and the discharging flow is 800-.
Example 6
The color paste with low odor, low viscosity and good stability comprises the following components in parts by weight:
55 parts of hydroxypropyl acrylate
Ethylene-vinyl acetate copolymer 15 parts
30 parts of phthalocyanine blue;
the preparation method of the color paste comprises the following steps:
(1) weighing the components according to the formula ratio, stirring and mixing hydroxypropyl acrylate and ethylene-vinyl acetate copolymer at the stirring speed of 500 revolutions per minute for 20 minutes to prepare a mixture A for later use;
(2) adding pigment into the mixture A prepared in the step (1), stirring at the stirring speed of 1400 revolutions per minute for 50 minutes to prepare a mixture B, and then adding the mixture B into a sand mill for grinding under the conditions that the diameter of zirconium beads used for grinding is 0.2mm, the filling rate of the zirconium beads is 80%, the linear speed of grinding is 12m/s, the pressure of a cavity is 0.03MPa, the discharging temperature of grinding is less than 40 ℃, and the discharging flow rate is 800-inch and 1000kg/h to prepare the color paste.
Example 7
The color paste with low odor, low viscosity and good stability comprises the following components in parts by weight:
n-acryloyl morpholine 75
Polyethylene glycol (400) -methacrylate 5 parts
20 parts of indigo.
The preparation method of the color paste comprises the following steps:
(1) weighing the components according to the formula ratio, stirring and mixing the N-acryloyl morpholine and polyethylene glycol (400) -methacrylate at the stirring speed of 300 revolutions per minute for 25 minutes to prepare a mixture A for later use;
(2) adding pigment into the mixture A prepared in the step (1), stirring at the stirring speed of 1200 rpm for 60 minutes to prepare a mixture B, and then adding the mixture B into a sand mill for grinding under the conditions that the diameter of zirconium beads used for grinding is 0.4mm, the filling rate of the zirconium beads is 60%, the linear speed of grinding is 11m/s, the pressure of a cavity is 0.01MPa, the discharging temperature of grinding is less than 40 ℃, and the discharging flow rate is 800-class and 1000kg/h to prepare the color paste.
Example 8
Compared with the example 7, the method also comprises a filtration process after grinding in the example 8, wherein the filtration process adopts a filter membrane for filtration, the pore diameter of the filter membrane is 200nm, and the rest components and the preparation process are the same as the example 7.
Comparative example 1
In comparison with example 7, in comparative example 1, vinyl bis stearamide was used instead of polyethylene glycol (400) -methacrylate, and the remaining components and preparation process were the same as in example 7.
Comparative example 2
In comparison with example 7, the dispersant polyethylene glycol (400) -methacrylate in comparative example 2 was 25 parts, the pigment indigo was 40 parts, and the remaining components and preparation process were the same as in example 7.
Product effectiveness testing
The color pastes prepared in the examples 1-8 and the comparative examples 1-2 are subjected to stability test, and the specific test process is as follows: the color paste is placed at minus 10 ℃ and kept stand for 3 days, then placed at 60 ℃ and kept stand for 3 days, then placed at minus 10 ℃ and kept stand for 3 days, the operation is repeated for 3 times (namely, the color paste is subjected to high-low temperature treatment), whether the color paste is layered or not is observed (the result is shown in table 1), then the color paste is added to prepare UV ink (namely, the ink capable of being cured by ultraviolet light) to be applied to a high-speed printer (the frequency of a printing nozzle of the printer is 30KHz), whether the printing nozzle is blocked or not is observed, whether the ink break phenomenon occurs or not is printed or not is observed.
As can be seen from Table 1, the color pastes prepared in examples 1-8 of the present invention have no delamination after high and low temperature cycle treatment, and the color pastes after high and low temperature treatment are formulated into UV ink for high speed printers without nozzle blockage and ink break. The stability of the color paste prepared by changing the type of the dispersing agent in the comparative example 1 is poor, the dosage of the dispersing agent and the pigment is changed in the comparative example 2, the prepared color paste is not layered after high-temperature and low-temperature treatment, but the UV ink prepared from the color paste after high-temperature and low-temperature treatment has the phenomena of nozzle blockage and ink break when being applied to a high-speed printer.
In addition, the color pastes obtained in examples 1 to 8 and a commercially available white color paste (containing no monomer according to the present invention and having a pigment content of 10% by mass) were tested for odor, average particle diameter, viscosity at 25 ℃ and filtration performance, wherein the filtration performance was tested for a time required for filtration of 200g of the color paste on a polypropylene filter having a filter diameter of 50mm and a pore diameter of 0.45 μm under-0.05 MPa, and the results are shown in Table 2.
Table 2:
as can be seen from Table 2, the color pastes prepared in examples 1-8 of the present invention have low odor, a viscosity at 25 ℃ of not more than 30CP, and excellent filtration performance, which is significantly superior to commercially available white color pastes. The pigment mass content of the color paste prepared in the embodiments 1-8 of the invention is more than or equal to 20 percent.
Claims (10)
1. The color paste is characterized by comprising the following components in parts by weight:
monomer 55-80
3-15 parts of dispersant
15-30 parts of pigment;
the monomer is selected from at least one of acrylate, vinyl ether or acryloyl morpholine;
the dispersant is a polymeric dispersant.
2. The color paste according to claim 1, wherein the acrylate is at least one selected from the group consisting of ethoxyethoxyethyl acrylate, cyclotrimethylolpropane methylal acrylate, 2-ethyleneoxyethoxy ethyl acrylate, hydroxypropyl acrylate and hydroxyethyl methacrylate.
3. The color paste according to claim 1, wherein the vinyl ether is selected from at least one of triethylene glycol divinyl ether, divinyl ether or divinyl-1, 4-butylene glycol ether; the acryloyl morpholine is selected from 4-acryloyl morpholine and/or N-acryloyl morpholine.
4. The color paste according to claim 1, wherein the dispersant is at least one selected from polyethylene glycol acrylate polymers, oxidized polyethylene wax, ethylene-acrylic acid copolymers or ethylene-vinyl acetate copolymers.
5. The color paste according to claim 1, wherein the pigment is at least one selected from the group consisting of cinnabar, carbon black, realgar, malachite green, wollastonite, barite powder, talc, mica powder, kaolin, alizarin red, indigo, titanium white, lithopone, lead chrome yellow, iron blue, phthalocyanine blue, quinacridone violet ER02, quinacridone red 122A, quinacridone violet 19, pigment yellow 3, pigment yellow 93 and pigment red 53: 1.
6. The method for preparing the color paste according to any one of claims 1 to 5, which is characterized by comprising the following steps:
(1) weighing the components according to the formula ratio, and stirring and mixing the monomer and the dispersant to prepare a mixture A for later use;
(2) adding the pigment into the mixture A prepared in the step (1), stirring at the stirring speed of 1000-.
7. The preparation method as claimed in claim 6, wherein the grinding conditions in step (2) are that the diameter of zirconium beads used for grinding is 0.2-0.4mm, the filling rate of zirconium beads is 60-80%, the linear speed of grinding is 10-12m/s, the pressure in the cavity is less than 0.04MPa, the discharge temperature of grinding is less than 40 ℃, and the discharge flow rate is 800-.
8. The method according to claim 6, wherein the grinding in step (2) is followed by a filtration process, and the filtration process uses a filter membrane for filtration, and the pore size of the filter membrane is 100-300 nm.
9. An ink, characterized in that it comprises a paste according to any one of claims 1 to 5.
10. Applying the ink of claim 9 to a printing process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911352984.9A CN111057416A (en) | 2019-12-25 | 2019-12-25 | Color paste with low odor, low viscosity and good stability and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911352984.9A CN111057416A (en) | 2019-12-25 | 2019-12-25 | Color paste with low odor, low viscosity and good stability and application thereof |
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| CN111057416A true CN111057416A (en) | 2020-04-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114163875A (en) * | 2021-11-05 | 2022-03-11 | 深圳市墨库图文技术有限公司 | Red nano color paste and preparation method and application thereof |
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| CN102190907A (en) * | 2010-03-12 | 2011-09-21 | 富士胶片株式会社 | Pigment dispersion, ink composition using the same, and printed material |
| CN107304318A (en) * | 2016-04-25 | 2017-10-31 | 珠海赛纳打印科技股份有限公司 | 3D ink composition for ink-jet printing, ink group and preparation method thereof |
| CN109206980A (en) * | 2018-10-31 | 2019-01-15 | 传美讯电子科技（珠海）有限公司 | A kind of UV ink-jet white ink |
| CN109401439A (en) * | 2018-10-31 | 2019-03-01 | 传美讯电子科技（珠海）有限公司 | A kind of UV ink-jet ink dispersible pigment color paste and preparation method thereof |
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2019
- 2019-12-25 CN CN201911352984.9A patent/CN111057416A/en active Pending
Patent Citations (5)
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| CN101646730A (en) * | 2007-03-28 | 2010-02-10 | 富士胶片株式会社 | Pigment dispersion composition, photocurable composition, color filter, and method for producing color filter |
| CN102190907A (en) * | 2010-03-12 | 2011-09-21 | 富士胶片株式会社 | Pigment dispersion, ink composition using the same, and printed material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114163875A (en) * | 2021-11-05 | 2022-03-11 | 深圳市墨库图文技术有限公司 | Red nano color paste and preparation method and application thereof |
| CN114163875B (en) * | 2021-11-05 | 2023-08-08 | 深圳市墨库图文技术有限公司 | Red nanometer color paste and preparation method and application thereof |
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| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: 519050 No. 3 Langyong Road, Nanshui Town, Jinwan District, Zhuhai City, Guangdong Province Applicant after: Zhuhai Dongchang Color Technology Co.,Ltd. Address before: 519050 No. 3 Langyong Road, Nanshui Town, Jinwan District, Zhuhai City, Guangdong Province Applicant before: ZHUHAI DONGCHANG PIGMENT Co.,Ltd. |
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| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200424 |