CN110938283A - Thermochromic non-wood fiber melamine powder - Google Patents

Thermochromic non-wood fiber melamine powder Download PDF

Info

Publication number
CN110938283A
CN110938283A CN201910919923.XA CN201910919923A CN110938283A CN 110938283 A CN110938283 A CN 110938283A CN 201910919923 A CN201910919923 A CN 201910919923A CN 110938283 A CN110938283 A CN 110938283A
Authority
CN
China
Prior art keywords
fiber
percent
melamine
drying
hours
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910919923.XA
Other languages
Chinese (zh)
Inventor
严明亮
邱涛
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang Liancheng Amino Material Co Ltd
Original Assignee
Zhejiang Liancheng Amino Material Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhejiang Liancheng Amino Material Co Ltd filed Critical Zhejiang Liancheng Amino Material Co Ltd
Priority to CN201910919923.XA priority Critical patent/CN110938283A/en
Publication of CN110938283A publication Critical patent/CN110938283A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/14Glass
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L61/00Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
    • C08L61/20Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
    • C08L61/26Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
    • C08L61/28Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2237Oxides; Hydroxides of metals of titanium
    • C08K2003/2241Titanium dioxide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/14Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/16Fibres; Fibrils

Abstract

The heat discoloration resistant non-wood fiber melamine powder is characterized in that the molding compound for melamine tableware comprises the following components in percentage by mass: 60-70% of melamine formaldehyde resin, 20-30% of fiber, 0.1-0.5% of curing agent, 3-10% of dispersing agent, 1.0-1.5% of titanium dioxide and the balance of pigment, wherein the components are one hundred percent by mass; the fiber is composed of at least one of glass fiber, cotton fiber and fibrilia, the manufacturing process is simple, the effect is good, the product is attractive, elegant, stable and durable in use, all natural materials are used in the manufacturing process, no pollution is caused, and the manufactured product meets the national standard, even is up to the national standard.

Description

Thermochromic non-wood fiber melamine powder
Technical Field
The invention relates to a heat discoloration resistant non-wood fiber melamine powder, belonging to the field of molding compound manufacture.
Background
Common melamine tableware is attractive and well liked by people, but due to the existence of a large amount of wood fibers, the tableware can slowly become yellow when being used at high temperature for a long time, so that the beautiful appearance of the tableware is lost, and the service life of the tableware is shortened.
The invention content is as follows:
the invention aims to overcome the defects in the prior art and provide the thermal discoloration resistant non-wood fiber melamine powder, and the molding compound for melamine tableware comprises the following components in percentage by mass:
Figure BDA0002217253680000011
the components are based on one hundred mass percent; the fiber is composed of at least one of glass fiber, cotton fiber and hemp fiber.
Preferably, the molding compound for melamine tableware comprises the following components in percentage by mass:
Figure BDA0002217253680000012
the components are based on one hundred mass percent; the fiber is composed of at least one of glass fiber, cotton fiber and hemp fiber.
The preparation method comprises the following steps:
(1) adding a formaldehyde solution into a reaction kettle, and adding sodium hydroxide to adjust the pH value to 7-10;
(2) starting to heat, adding melamine, heating to 80-100 ℃ and reacting;
(3) and (3) reaction end point: the resin was tested for white precipitate with 4 ℃ water.
(4) Adding triethanolamine, adjusting pH, terminating the reaction, and cooling to 70 deg.C;
(5) kneading: and adding the fiber, the dispersing agent, the curing agent and the prepared resin by using a Z-type low-speed kneader, kneading, and stirring uniformly by changing the stirring direction at regular time.
(6) And (3) drying: a multi-section mesh belt hot air oven is adopted, hot air drying is carried out at the temperature of 80-85 ℃, the drying is uniform, the moisture content is controlled to be below 3.5 percent, and the drying time is about 3-4 hours.
(7) Crushing and ball-milling: the materials are crushed and then enter a ball mill for ball milling for 3-8 hours, and dispersing agents, curing agents, pigments and the like are added in the process to meet the requirements of material densification, color matching, curing fluidity control and the like. The ball mill jacket needs to be cooled by cooling water, and the material temperature is not higher than 50 ℃.
(8) Packaging: packaging the ground material with 25Kg lining film paper bag after passing through a 60-mesh screen, and storing the finished product in a cool and dry place.
Preferably, the method comprises the following steps:
in the step (1), the pH value is adjusted to 8.5 by adding sodium hydroxide;
in the step (2), melamine is added, and the temperature is raised to 85 ℃ for reaction;
in the step (6), drying: a multi-section mesh belt hot air oven is adopted, hot air drying is carried out at 83.5 ℃, the drying is uniform, the water content is controlled to be below 3.5 percent, and the drying time is about 3.5 hours;
in the step (7), crushing and ball milling: the materials are crushed and then enter a ball mill for ball milling for 6 hours.
The invention has the advantages of simple manufacturing process, good effect, beautiful and elegant appearance, stability and durability of the product, no pollution caused by pure natural materials used in the manufacturing process, and the manufactured product conforms to the national standard even to the national standard.
Detailed Description
1. The present invention will be described in detail below: the heat discoloration resistant non-wood fiber melamine powder is characterized in that the melamine tableware molding compound consists of the following components in percentage by mass:
Figure BDA0002217253680000021
the components are based on one hundred mass percent; the fiber is composed of at least one of glass fiber, cotton fiber and hemp fiber.
The molding compound for melamine tableware specifically comprises the following components in percentage by mass:
Figure BDA0002217253680000022
Figure BDA0002217253680000031
the components are based on one hundred mass percent; the textile fiber is composed of at least one of glass fiber, cotton fiber and hemp fiber.
The preparation method comprises the following steps:
(1) adding a formaldehyde solution into a reaction kettle, and adding sodium hydroxide to adjust the pH value to 7-10;
(2) starting to heat, adding melamine, heating to 80-100 ℃ and reacting;
(3) and (3) reaction end point: the resin was tested for white precipitate with 4 ℃ water.
(4) Adding triethanolamine, adjusting pH, terminating the reaction, and cooling to 70 deg.C;
(5) kneading: and adding the fiber, the dispersing agent, the curing agent and the prepared resin by using a Z-type low-speed kneader, kneading, and stirring uniformly by changing the stirring direction at regular time.
(6) And (3) drying: a multi-section mesh belt hot air oven is adopted, hot air drying is carried out at the temperature of 80-85 ℃, the drying is uniform, the moisture content is controlled to be below 3.5 percent, and the drying time is about 3-4 hours.
(7) Crushing and ball-milling: the materials are crushed and then enter a ball mill for ball milling for 3-8 hours, and dispersing agents, curing agents, pigments and the like are added in the process to meet the requirements of material densification, color matching, curing fluidity control and the like. The ball mill jacket needs to be cooled by cooling water, and the material temperature is not higher than 50 ℃.
(8) Packaging: packaging the ground material with 25Kg lining film paper bag after passing through a 60-mesh screen, and storing the finished product in a cool and dry place. In the step (1), the pH value is adjusted to 8.5 by adding sodium hydroxide;
in the step (2), melamine is added, and the temperature is raised to 85 ℃ for reaction;
in the step (6), drying: a multi-section mesh belt hot air oven is adopted, hot air drying is carried out at 83.5 ℃, the drying is uniform, the water content is controlled to be below 3.5 percent, and the drying time is about 3.5 hours;
in the step (7), crushing and ball milling: the materials are crushed and then enter a ball mill for ball milling for 6 hours.
The first embodiment is as follows: glass fiber
Figure BDA0002217253680000032
Figure BDA0002217253680000041
(1) Adding a formaldehyde solution into a reaction kettle, and adding sodium hydroxide to adjust the pH value to 7-10;
(2) starting to heat, adding melamine, heating to 80-100 ℃ and reacting;
(3) and (3) reaction end point: the resin was tested for white precipitate with 4 ℃ water.
(4) Adding triethanolamine, adjusting pH, terminating the reaction, and cooling to 70 deg.C;
(5) kneading: and (3) kneading the glass fiber, the dispersing agent, the curing agent and the prepared resin by using a Z-type low-speed kneader, and stirring uniformly by changing the stirring direction at regular time.
(6) And (3) drying: a multi-section mesh belt hot air oven is adopted, hot air drying is carried out at the temperature of 80-85 ℃, the drying is uniform, the moisture content is controlled to be below 3.5 percent, and the drying time is about 3-4 hours.
(7) Crushing and ball-milling: the materials are crushed and then enter a ball mill for ball milling for 3-8 hours, and dispersing agents, curing agents, pigments and the like are added in the process to meet the requirements of material densification, color matching, curing fluidity control and the like. The ball mill jacket needs to be cooled by cooling water, and the material temperature is not higher than 50 ℃.
(8) Packaging: packaging the ground material with 25Kg lining film paper bag after passing through a 60-mesh screen, and storing the finished product in a cool and dry place. The second specific embodiment is as follows: adding fibrilia
Figure BDA0002217253680000042
(1) Adding a formaldehyde solution into a reaction kettle, and adding sodium hydroxide to adjust the pH value to 7-10;
(2) heating, adding melamine, and heating to 80-100 ℃ for reaction;
(3) and (3) reaction end point: the resin was tested for white precipitate with 4 ℃ water.
(4) Adding triethanolamine, adjusting pH, terminating the reaction, and cooling to 70 deg.C;
(5) kneading: adding the fibrilia, the dispersing agent, the curing agent and the prepared resin into a Z-type low-speed kneader, kneading, changing the stirring direction at regular time, and stirring until the mixture is uniform.
(6) And (3) drying: a multi-section mesh belt hot air oven is adopted, hot air drying is carried out at the temperature of 80-85 ℃, the drying is uniform, the moisture content is controlled to be below 3.5 percent, and the drying time is about 3-4 hours.
(7) Crushing and ball-milling: the materials are crushed and then enter a ball mill for ball milling for 3-8 hours, and dispersing agents, curing agents, pigments and the like are added in the process to meet the requirements of material densification, color matching, curing fluidity control and the like. The ball mill jacket needs to be cooled by cooling water, and the material temperature is not higher than 50 ℃.
(8) Packaging: packaging the ground material with 25Kg lining film paper bag after passing through a 60-mesh screen, and storing the finished product in a cool and dry place.
The third concrete embodiment: adding cotton fiber
Figure BDA0002217253680000051
(1) Adding a formaldehyde solution into a reaction kettle, and adding sodium hydroxide to adjust the pH value to 7-10;
(2) starting to heat, adding melamine, heating to 80-100 ℃ and reacting;
(3) and (3) reaction end point: the resin was tested for white precipitate with 4 ℃ water.
(4) Adding triethanolamine, adjusting pH, terminating the reaction, and cooling to 70 deg.C;
(5) kneading: and (3) adding the cotton fiber, the dispersing agent, the curing agent and the prepared resin into a Z-type low-speed kneader, kneading, changing the stirring direction at regular time, and stirring uniformly.
(6) And (3) drying: a multi-section mesh belt hot air oven is adopted, hot air drying is carried out at the temperature of 80-85 ℃, the drying is uniform, the moisture content is controlled to be below 3.5 percent, and the drying time is about 3-4 hours.
(7) Crushing and ball-milling: the materials are crushed and then enter a ball mill for ball milling for 3-8 hours, and dispersing agents, curing agents, pigments and the like are added in the process to meet the requirements of material densification, color matching, curing fluidity control and the like. The ball mill jacket needs to be cooled by cooling water, and the material temperature is not higher than 50 ℃.
(8) Packaging: packaging the ground material with 25Kg lining film paper bag after passing through a 60-mesh screen, and storing the finished product in a cool and dry place.
The method of the specific embodiment four: adding hemp fiber and cotton fiber
Figure BDA0002217253680000052
(1) Adding a formaldehyde solution into a reaction kettle, and adding sodium hydroxide to adjust the pH value to 7-10;
(2) starting to heat, adding melamine, heating to 80-100 ℃ and reacting;
(3) and (3) reaction end point: the resin was tested for white precipitate with 4 ℃ water.
(4) Adding triethanolamine, adjusting pH, terminating the reaction, and cooling to 70 deg.C;
(5) kneading: adding wood fiber, cotton fiber, a dispersing agent, a curing agent and the prepared resin into a Z-type low-speed kneader, kneading, changing the stirring direction at regular time, and stirring uniformly.
(6) And (3) drying: a multi-section mesh belt hot air oven is adopted, hot air drying is carried out at the temperature of 80-85 ℃, the drying is uniform, the moisture content is controlled to be below 3.5 percent, and the drying time is about 3-4 hours.
(7) Crushing and ball-milling: the materials are crushed and then enter a ball mill for ball milling for 3-8 hours, and dispersing agents, curing agents, pigments and the like are added in the process to meet the requirements of material densification, color matching, curing fluidity control and the like. The ball mill jacket needs to be cooled by cooling water, and the material temperature is not higher than 50 ℃.
(8) Packaging: packaging the ground material with 25Kg lining film paper bag after passing through a 60-mesh screen, and storing the finished product in a cool and dry place.
Whiteness testing experiments:
1. directly putting the wood fiber, the hemp fiber and the cotton fiber into a 130 ℃ oven, carrying out high-temperature treatment for different times, and then carrying out whiteness test by using a whiteness tester. The results are as follows:
whiteness value Wood fiber Fibrilia Cotton fiber
Initial whiteness 89.2 79.4 88.9
Whiteness after 7h 81.1 75.2 82.5
Whiteness after 14h 76.4 72.3 79.7
Whiteness after 24h 72 69.1 76.4
After 24 hours of high-temperature treatment, the whiteness value of the wood fiber is reduced by 19.3 percent, the whiteness value of the hemp fiber is reduced by 12.9 percent, and the whiteness value of the cotton fiber is reduced by 14.1 percent.
2. At least one of wood fiber, cotton fiber and hemp fiber is made into melamine product, which is put into a 130 ℃ oven for high temperature treatment at different time and then whiteness test is carried out by a whiteness meter. The results are as follows:
Figure BDA0002217253680000061
after 24 hours of high-temperature treatment, the whiteness value of the wood fiber melamine product is reduced by 19.7 percent, the whiteness value of the wood fiber and cotton fiber melamine product is reduced by 14.4 percent, and the whiteness value of the cotton fiber and hemp fiber melamine product is reduced by 10.0 percent
The tests show that: the glass fiber is not easy to be fully fused with the resin, so that the melamine product has a rough surface, and the beauty and the use are influenced; the effect of the wood fiber is poor, although the fibrilia has the best effect at high temperature, the initial whiteness of the fibrilia is low, the whiteness of a melamine product cannot meet the requirement of a client, and the effect of the cotton fiber is second to that of the fibrilia, and the whiteness value of the cotton fiber is also high, so that the mixture of the fibrilia and the cotton fiber is selected to meet the requirement on whiteness, and the fibrilia is not easy to discolor at high temperature.

Claims (4)

1. The heat discoloration resistant non-wood fiber melamine powder is characterized in that the molding compound for melamine tableware comprises the following components in percentage by mass:
60-70% of melamine formaldehyde resin
20 to 30 percent of fiber
0.1 to 0.5 percent of curing agent
3 to 10 percent of dispersant
Titanium dioxide 1.0-1.5%
Pigment replenishment
The components are based on one hundred mass percent; the fiber is composed of at least one of glass fiber, cotton fiber and hemp fiber.
2. The thermochromic non-wood fiber melamine powder according to claim 1, wherein the molding compound for melamine tableware comprises the following components in percentage by mass:
melamine formaldehyde resin 70%
25 percent of fiber
0.1 percent of curing agent
3 percent of dispersant
1.0 percent of titanium dioxide
Pigment replenishment
The components are based on one hundred mass percent; the fiber is composed of at least one of glass fiber, cotton fiber and hemp fiber.
3. A method for preparing the anti-thermochromic non-wood fiber melamine powder according to claim 1 or 2, wherein the method comprises the steps of:
(1) adding a formaldehyde solution into a reaction kettle, and adding sodium hydroxide to adjust the pH value to 7-10;
(2) starting to heat, adding melamine, heating to 80-100 ℃ and reacting;
(3) and (3) reaction end point: testing the resin with water at 4 ℃ to obtain white precipitate;
(4) adding triethanolamine, adjusting pH, terminating the reaction, and cooling to 70 deg.C;
(5) kneading: adding fibers, a dispersing agent, a curing agent and the prepared resin into a Z-type low-speed kneader, kneading, changing the stirring direction at regular time, and stirring uniformly;
(6) and (3) drying: a multi-section mesh belt hot air oven is adopted, hot air drying is carried out at the temperature of 80-85 ℃, the drying is uniform, the moisture content is controlled to be below 3.5 percent, and the drying time is about 3-4 hours;
(7) crushing and ball-milling: the materials are crushed and then enter a ball mill for ball milling for 3-8 hours, and dispersing agents, curing agents, pigments and the like are added in the process to meet the requirements of material densification, color matching, solidification fluidity control and the like, a ball mill jacket needs to be cooled by cooling water, and the temperature of the materials is not higher than 50 ℃;
(8) packaging: packaging the ground material with 25Kg lining film paper bag after passing through a 60-mesh screen, and storing the finished product in a cool and dry place.
4. The method for preparing the anti-thermochromic non-wood fiber melamine powder according to claim 3, wherein:
in the step (1), the pH value is adjusted to 8.5 by adding sodium hydroxide;
in the step (2), melamine is added, and the temperature is raised to 85 ℃ for reaction;
in the step (6), drying: a multi-section mesh belt hot air oven is adopted, hot air drying is carried out at 83.5 ℃, the drying is uniform, the moisture content is controlled to be below 3.5 percent, and the drying time is about 3.5 hours;
in the step (7), crushing and ball milling: the materials are crushed and then enter a ball mill for ball milling for 6 hours.
CN201910919923.XA 2019-09-26 2019-09-26 Thermochromic non-wood fiber melamine powder Pending CN110938283A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910919923.XA CN110938283A (en) 2019-09-26 2019-09-26 Thermochromic non-wood fiber melamine powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910919923.XA CN110938283A (en) 2019-09-26 2019-09-26 Thermochromic non-wood fiber melamine powder

Publications (1)

Publication Number Publication Date
CN110938283A true CN110938283A (en) 2020-03-31

Family

ID=69906073

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910919923.XA Pending CN110938283A (en) 2019-09-26 2019-09-26 Thermochromic non-wood fiber melamine powder

Country Status (1)

Country Link
CN (1) CN110938283A (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002000429A1 (en) * 2000-06-21 2002-01-03 Agrolinz Melamin Gmbh Fibre composites with excellent dimensional stability, weather resistance and flameproofing properties
JP2006161023A (en) * 2004-07-09 2006-06-22 Nippon Carbide Ind Co Inc Composition for molding melamine-based resin and molded article

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002000429A1 (en) * 2000-06-21 2002-01-03 Agrolinz Melamin Gmbh Fibre composites with excellent dimensional stability, weather resistance and flameproofing properties
JP2006161023A (en) * 2004-07-09 2006-06-22 Nippon Carbide Ind Co Inc Composition for molding melamine-based resin and molded article

Similar Documents

Publication Publication Date Title
CN101654542B (en) High-temperature resistant porcelain imitation material and production method thereof
CN105130378B (en) A kind of artificial color sand colouring agent, artificial color sand and preparation method using the colouring agent
CN105218771A (en) A kind of preparation method of melmac
CN109020528B (en) Low-temperature high-heat-resistance all-ceramic and preparation method thereof
CN109279872A (en) A kind of high temperature ceramic material and preparation method thereof
CN103113759A (en) Red disperse dye composition, and preparation method and application thereof
CN109401190A (en) A kind of anti-bacteria melamine powder
CN110938283A (en) Thermochromic non-wood fiber melamine powder
CN113582686A (en) Preparation method of blue zirconia ceramic
CN104447429B (en) Environment protection acidic can pulling color Yellow dye compound, application and synthetic method
CN105692704A (en) Preparation method of temperature-resistant iron oxide yellow
CN109266041B (en) Preparation method of compact stable ceramic pigment
CN108997839A (en) A kind of preparation method of the brown colorant for ceramic ink jet
CN112174528A (en) Purple blue glaze for preparing Jun pottery and preparation method thereof
CN111170716B (en) High-brightness colorful ceramic product and preparation method thereof
CN106082809B (en) Heat-reflecting insulating coating and preparation method thereof
CN113896878B (en) Macromolecular anti-blue-light auxiliary agent and preparation method thereof
KR102514276B1 (en) Yellow oriental-melon colored pottery and manufacturing method of the same
CN109486239B (en) Disperse dye composition and preparation method and application thereof
CN108341659A (en) A kind of manufacture craft of magnesia dry-pressing ceramic products
CN109279827A (en) A kind of production technology of construction wall composite material
CN104988794A (en) Coating for improving smoothness of coated paper and application
CN104458601B (en) A kind of fibre identification colouring agent and application thereof
CN112358184A (en) High-temperature raw ore red glaze and preparation method and use method thereof
CN115286365B (en) Jade porcelain and manufacturing process thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20200331

RJ01 Rejection of invention patent application after publication