CN104725957B - A kind of self-crosslinking fire-resistant coating for steel structure and preparation method thereof - Google Patents
A kind of self-crosslinking fire-resistant coating for steel structure and preparation method thereof Download PDFInfo
- Publication number
- CN104725957B CN104725957B CN201510119086.4A CN201510119086A CN104725957B CN 104725957 B CN104725957 B CN 104725957B CN 201510119086 A CN201510119086 A CN 201510119086A CN 104725957 B CN104725957 B CN 104725957B
- Authority
- CN
- China
- Prior art keywords
- parts
- fire
- self
- steel structure
- crosslinking
- 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.)
- Active
Links
Classifications
-
- 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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- 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
Abstract
The invention belongs to fireproof coating technical field, it particularly relates to arrive a kind of self-crosslinking fire-resistant coating for steel structure and preparation method thereof.Calculate in parts by mass, the self-crosslinking fire-resistant coating for steel structure include 12 28 parts water-borne Self-Crosslinked Acrylic emulsion, 15 parts of pigment, 39 62 parts of fire proofing additive, 7 17 parts of fire resistant infilling, 0.1 0.5 parts of thickening agent, the deionized water of 0.1 0.4 parts of coalescents and 10 18 parts；The fire proofing additive includes dehydrant APP, tripolycyanamide, charcoal agent tetramethylolmethane and expanded graphite；The thickening agent is cellulose.Compared with prior art, the compactness of self-crosslinking fire-resistant coating for steel structure of the present invention is good with fire resistance, and adhesive force is strong, and high-temperature expansion effect is good, and its preparation method process is simple, low cost, flameproof effect are good, applied range.
Description
Technical field
The invention belongs to fireproof coating technical field, it particularly relates to arrive a kind of self-crosslinking fire-resistant coating for steel structure and
Its preparation method.
Background technology
In the 10min that fire occurs, fire scene temperature can reach 700 DEG C or so, therefore when steel local or surface are subjected to
During fire effect, heat can be transmitted inside steel rapidly, and total or member temperature will be caused drastically to raise, structure is caused
Intensity decreases completely lose bearing capacity.Under fire effect, as temperature is raised, the increase of atom kinetic energy, atom leaves flat
The room that weighing apparatus point is formed is increased, and weakens interatomic adhesion；On the other hand, under load effect, room is easily formed should
Power is concentrated, therefore under the collective effect of fire and load, steel start destruction from empty place first, and gradually radiate out
It is very short the time required to by local to overall destruction, therefore fire endurance is very low.
Fire-resistant coating for steel structure has two big class, non-expansion type fire-resistant coating for steel structure and expanding fire-proof paint.It is unexpansive
Formed steel construction fireproof coating plays fire-proof and thermal-insulation effect typically by adding inorganic fire proof material and is prevented fires, but due to fire prevention effect
It is really undesirable gradually to be eliminated.And expansion steel-structure fireproofing coating is preferably widely used due to fire protecting performance, according to painting
Material form can be divided into water type, three class of oil type and powder-type, and due to oil paint solvent volatilization easily pollution environment, therefore consumption exists
Gradually decrease, and the thin coated type steel structure fire-proof paint of most widely used aqueouss, the dirt of solvent volatilization is reduced with water as solvent
Dye.Existing scumbling expansion steel-structure fireproofing coating is with APP, tripolycyanamide, tetramethylolmethane and part inorganic material group
Into film forming matter mainly adopts aqueous polymer emulsion (styrene-acrylic emulsion, polyacrylate dispersion, vinyl acetate emulsion, chlorine acrylic emulsion
Deng), preparation technology is to disperse at a high speed aqueous polymer emulsion and fire proofing material, auxiliary agent, pigment, filler etc., grind, adjusting viscosity
Form.By to the thin coated type steel structure fire-proof paint fire resistance lot of experiments of existing aqueouss on market, it is found that coating is being passed through
Easy crackle and come off after high-temperature expansion, it is unfavorable to insulating refractory.
The content of the invention
To solve above-mentioned technical problem, the invention provides a kind of compactness is good with fire resistance, and high-temperature expansion effect
Really good self-crosslinking fire-resistant coating for steel structure and preparation method thereof.
A kind of self-crosslinking fire-resistant coating for steel structure of the present invention, is calculated in parts by mass, and the fireproof coating includes 12-
28 parts of water-borne Self-Crosslinked Acrylic emulsion, the pigment of 1-5 parts, the fire proofing additive of 39-62 parts, the fire resistant infilling of 7-17 parts,
The deionized water of the thickening agent, the coalescents of 0.1-0.4 parts and 10-18 parts of 0.1-0.5 parts；The fire proofing additive includes dehydration
Agent APP, tripolycyanamide, charcoal agent tetramethylolmethane and expanded graphite；The thickening agent is cellulose.
A kind of self-crosslinking fire-resistant coating for steel structure of the present invention, is calculated in parts by mass, and the fire proofing additive includes 17-
The expansion 200 of 80 mesh of 28 parts of APP, the tripolycyanamide of 13-20 parts, the tetramethylolmethane of 8-18 parts and 1-6 parts again with
On expanded graphite；Titanium dioxide of the pigment for 1-5 parts；The fire resistant infilling high-alumina refractory mud and 5-10 parts for 2-7 parts
Ceramic fibre.
A kind of self-crosslinking fire-resistant coating for steel structure of the present invention, the solid of the water-borne Self-Crosslinked Acrylic emulsion contain
Measure as 45%-50%, during moisture evaporation, carry out self-crosslinking solidification at normal temperatures.
A kind of self-crosslinking fire-resistant coating for steel structure of the present invention, Al in the high-alumina refractory mud2O3Content 55%-
85%, fineness is -400 mesh of 200 mesh.
A kind of self-crosslinking fire-resistant coating for steel structure of the present invention, the tetramethylolmethane are monopentaerythritol, double seasons penta
Any one in tetrol or tripentaerythritol.
A kind of self-crosslinking fire-resistant coating for steel structure of the present invention, the APP are II of the degree of polymerization more than 1000
Type APP.
A kind of self-crosslinking fire-resistant coating for steel structure of the present invention, the cellulose adopt methylcellulose, carboxymethyl
Any one in cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose.
A kind of self-crosslinking fire-resistant coating for steel structure of the present invention, the coalescents adopt diethylene glycol monobutyl ether.
A kind of preparation method of self-crosslinking fire-resistant coating for steel structure of the present invention, methods described are specially：By raw material
Proportioning weighs each component, starts dispersion machine and adds water-borne Self-Crosslinked Acrylic emulsion, deionized water, APP, trimerization successively
Cyanamide, tetramethylolmethane, expanded graphite, titanium dioxide and high-alumina refractory mud, then carry out dispersion 15min at a high speed, add ceramic fibre
Dimension, coalescents and cellulose thickener continue dispersion 10min at a high speed, adjust viscosity and are followed by ground, obtain fireproof coating.
Compared with prior art, following excellent of self-crosslinking fire-resistant coating for steel structure of the present invention and preparation method thereof
Point：
1), had as thin type expanding steel structure fire-resisting paint matrix resin using water-borne Self-Crosslinked Acrylic emulsion
Good mechanical property, resistance to water, washing fastness, excellent adhesive force, resistance to impact and pliability, remarkable weatherability and guarantor
Color gloss retention, easy construction, coating are dried rapid, prominent heat resistance.Excellent weather-proof of water-borne Self-Crosslinked Acrylic emulsion
Property, heat resistance can meet the requirement of Intumescent Fire Retardant Coatings for Steel Structure substrate, can also meet when hydro carbons catches fire and be rapidly heated
Requirement, fire endurance is up to more than 120min (coating dry film thickness 2.4mm).
2), in conventionally used APP, tripolycyanamide, tetramethylolmethane, expanded graphite are added as into C catalyst
And foaming agent, improve coating and be heated foaming effect, foaming layer is thickened and closely knit, depth of foam is up to original coating layer thickness
25 times -42 times, the fire endurance of fire resistant coating is improve, in coating, add cellulose thickener to increased dope viscosity, carry
Sagging effect of the high coating to steel beam column, it is ensured that the thickness of single spin coating.
3), simple production process of the present invention, low cost, flameproof effect be good, applied range.
Specific embodiment
Self-crosslinking fire-resistant coating for steel structure of the present invention and preparation method thereof is done with reference to specific embodiment
Further illustrate, but protection scope of the present invention is not limited to this.
Embodiment 1
Weigh water-borne Self-Crosslinked Acrylic emulsion 28g and be put in agitator and start stirring, then weigh APP successively
17g, tripolycyanamide 13g, monopentaerythritol 8g, expanded graphite (80 mesh expand more than 200 times) 4g, titanium dioxide 3g, high-alumina refractory
Mud 7g, ceramic fibre 8g, diethylene glycol monobutyl ether 0.1g, methylcellulose 0.2g, deionized water 12g are added in agitator, and
Dispersion stirring 30min at a high speed is carried out, adjusting viscosity followed by carries out sand milling into sand mill, packs, and obtains final product the slim of the present invention
Fire-resistant coating for steel structure.
Embodiment 2
Weigh water-borne Self-Crosslinked Acrylic emulsion 24g and be put in agitator and start stirring, then weigh APP successively
19g, tripolycyanamide 14g, Bis(pentaerythritol) 10g, expanded graphite (80 mesh expand more than 200 times) 6g, titanium dioxide 3g, high-alumina refractory
Mud 4g, ceramic fibre 10g, diethylene glycol monobutyl ether 0.2g, hydroxyethyl cellulose 0.1g, deionized water 10g are added in agitator,
And dispersion stirring 30min at a high speed is carried out, adjusting viscosity followed by carries out sand milling into sand mill, packs, and obtains final product the thin of the present invention
Formed steel construction fireproof coating.
Embodiment 3
Weigh water-borne Self-Crosslinked Acrylic emulsion 22g and be put in agitator and start stirring, then weigh APP successively
20g, tripolycyanamide 15g, tripentaerythritol 13g, expanded graphite (80 mesh expand more than 200 times) 3g, titanium dioxide 5g, high-alumina refractory
Mud 2g, ceramic fibre 6g, diethylene glycol monobutyl ether 0.3g, hydroxypropyl methyl cellulose 0.1g, deionized water 14g add agitator
It is interior, and dispersion stirring 30min at a high speed is carried out, adjusting viscosity followed by carries out sand milling into sand mill, packs, and obtains final product the present invention's
Thin section steel structure fire-resisting paint.
Embodiment 4
Weigh water-borne Self-Crosslinked Acrylic emulsion 12g and be put in agitator and start stirring, then weigh APP successively
22g, tripolycyanamide 20g, tripentaerythritol 18g, expanded graphite (80 mesh expand more than 200 times) 5g, titanium dioxide 1g, high-alumina refractory
Mud 3g, ceramic fibre 5g, diethylene glycol monobutyl ether 0.1g, hydroxypropyl methyl cellulose 0.3g, deionized water 14g add agitator
It is interior, and dispersion stirring 30min at a high speed is carried out, adjusting viscosity followed by carries out sand milling into sand mill, packs, and obtains final product the present invention's
Thin section steel structure fire-resisting paint.
Embodiment 5
Weigh water-borne Self-Crosslinked Acrylic emulsion 13g and be put in agitator and start stirring, then weigh APP successively
28g, tripolycyanamide 16g, Bis(pentaerythritol) 9g, expanded graphite (80 mesh expand more than 200 times) 2g, titanium dioxide 4g, high-alumina refractory
Mud 5g, ceramic fibre 5g, diethylene glycol monobutyl ether 0.2g, hydroxyethyl cellulose 0.5g, deionized water 18g are added in agitator,
And dispersion stirring 30min at a high speed is carried out, adjusting viscosity followed by carries out sand milling into sand mill, packs, and obtains final product the thin of the present invention
Formed steel construction fireproof coating.
II type APP of the degree of polymerization of above-mentioned APP more than 1000.According to GB14907-2002《Steel construction is prevented
Fiery coating general technical specifications》The fire-resistant coating for steel structure prepared to more than carries out performance detection, as a result such as following table.
Above-described embodiment explanation：The present invention adopts water-borne Self-Crosslinked Acrylic emulsion as film forming matter, and adopts poly- phosphorus
Sour ammonium, tripolycyanamide, tetramethylolmethane, expanded graphite (80 mesh expand more than 200 times) are improved as into C catalyst and foaming agent
The fire prevention of fireproof coating, foam performance, mix high-alumina refractory mud and ceramic fibre, significantly improve the fire resistance of fireproof paint coating
Energy and effect of prestressed, the coating of product are undergoing quickly to be burnt when hydrocarbon fire heats up, to steel construction during generation fire
There is good protective effect.
Claims (6)
1. a kind of self-crosslinking fire-resistant coating for steel structure, it is characterised in that calculate in parts by mass, the fireproof coating includes 12-28
The water-borne Self-Crosslinked Acrylic emulsion of part, the pigment of 1-5 parts, the fire proofing additive of 39-62 parts, the fire resistant infilling of 7-17 parts, 0.1-
The deionized water of 0.5 part of thickening agent, the coalescents of 0.1-0.4 parts and 10-18 parts；The thickening agent is cellulose；
Calculate in parts by mass, the fire proofing additive includes the APP of 17-28 parts, the tripolycyanamide of 13-20 parts, 8-18 parts
The expanded graphite of more than 200 times of the expansion of 80 mesh of tetramethylolmethane and 1-6 parts；Titanium dioxide of the pigment for 1-5 parts；It is described
The ceramic fibre of high-alumina refractory mud and 5-10 part of the fire resistant infilling for 2-7 parts；
The APP is II type APP of the degree of polymerization more than 1000；
The coalescents adopt diethylene glycol monobutyl ether.
2. a kind of self-crosslinking fire-resistant coating for steel structure according to claim 1, it is characterised in that the waterborne self-crosslinkable third
The solids content of olefin(e) acid emulsion is 45%-50%, carries out self-crosslinking solidification at normal temperatures during moisture evaporation.
3. a kind of self-crosslinking fire-resistant coating for steel structure according to claim 1, it is characterised in that in the high-alumina refractory mud
Al2O3Content 55%-85%, fineness are -400 mesh of 200 mesh.
4. a kind of self-crosslinking fire-resistant coating for steel structure according to claim 1, it is characterised in that the tetramethylolmethane is single
Any one in tetramethylolmethane, Bis(pentaerythritol) or tripentaerythritol.
5. a kind of self-crosslinking fire-resistant coating for steel structure according to claim 1, it is characterised in that the cellulose adopts first
Any one in base cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose.
6. a kind of preparation method of self-crosslinking fire-resistant coating for steel structure according to claim 1, it is characterised in that the side
Method is specially：Each component is weighed by proportioning raw materials, dispersion machine is started and is added water-borne Self-Crosslinked Acrylic emulsion, deionization successively
Water, APP, tripolycyanamide, tetramethylolmethane, expanded graphite, titanium dioxide and high-alumina refractory mud, then carry out high speed dispersion
15min, adds ceramic fibre, coalescents and cellulose thickener and continues dispersion 10min at a high speed, adjust viscosity and followed by enter
Row grinding, obtains fireproof coating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510119086.4A CN104725957B (en) | 2015-03-18 | 2015-03-18 | A kind of self-crosslinking fire-resistant coating for steel structure and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510119086.4A CN104725957B (en) | 2015-03-18 | 2015-03-18 | A kind of self-crosslinking fire-resistant coating for steel structure and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104725957A CN104725957A (en) | 2015-06-24 |
| CN104725957B true CN104725957B (en) | 2017-03-29 |
Family
ID=53450403
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510119086.4A Active CN104725957B (en) | 2015-03-18 | 2015-03-18 | A kind of self-crosslinking fire-resistant coating for steel structure and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104725957B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105038466A (en) * | 2015-06-30 | 2015-11-11 | 沈阳工业大学辽阳校区 | Steel structure aqueous fireproof coating and preparation method thereof |
| CN106590396B (en) * | 2016-11-29 | 2018-10-30 | 河北晨阳工贸集团有限公司 | Environment protection type wall covering decorative fireproof coating and preparation method thereof |
| CN106752500A (en) * | 2016-11-30 | 2017-05-31 | 佛山市高明区诚睿基科技有限公司 | A kind of preparation method with fire resistant coating stainless steel material |
| CN106833204A (en) * | 2017-02-21 | 2017-06-13 | 程艳青 | A kind of indoor formaldehyde-removing antibiotic environmental protection sealing wax and preparation method thereof |
| CN107936735A (en) * | 2017-11-03 | 2018-04-20 | 国家电网公司 | A kind of ice-covering-proof sections tower |
| CN111607299A (en) * | 2020-06-09 | 2020-09-01 | 常州优纳新材料科技有限公司 | Mesoporous material composite steel structure fireproof coating and preparation method thereof |
| CN116814130A (en) * | 2023-07-21 | 2023-09-29 | 烟台艾弗尔阻燃科技有限公司 | Water-based steel structure fireproof paint |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101205441A (en) * | 2007-12-06 | 2008-06-25 | 同济大学 | Steelwork fire-retardant paint using self-crosslinking silicone-acrylic compound emulsion as substrate and preparation thereof |
| CN102002301A (en) * | 2010-11-10 | 2011-04-06 | 同济大学 | Fire-proof and corrosion-proof dual-function paint for water-based ultrathin expansion steel structure and preparation method thereof |
| CN102173691A (en) * | 2011-02-22 | 2011-09-07 | 山西省交通科学研究院 | Single-component tunnel fire-retardant coating and preparation method thereof |
-
2015
- 2015-03-18 CN CN201510119086.4A patent/CN104725957B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101205441A (en) * | 2007-12-06 | 2008-06-25 | 同济大学 | Steelwork fire-retardant paint using self-crosslinking silicone-acrylic compound emulsion as substrate and preparation thereof |
| CN102002301A (en) * | 2010-11-10 | 2011-04-06 | 同济大学 | Fire-proof and corrosion-proof dual-function paint for water-based ultrathin expansion steel structure and preparation method thereof |
| CN102173691A (en) * | 2011-02-22 | 2011-09-07 | 山西省交通科学研究院 | Single-component tunnel fire-retardant coating and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104725957A (en) | 2015-06-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104725957B (en) | A kind of self-crosslinking fire-resistant coating for steel structure and preparation method thereof | |
| CN102838907B (en) | Waterborne ultra-thin steel structure fire retardant coating and preparation method thereof | |
| WO2014090105A1 (en) | Water-based expandable fireproof coating for steel structure and preparation method therefor | |
| CN103146275B (en) | A kind of Grey heat-insulation flame-retardant external wall paint | |
| CN101914333B (en) | Aqueous nano ultra-thin steel structure fireproof coating and preparation method thereof | |
| CN104448237A (en) | Silicon-nitrogen-phosphate coordinating flame retardant epoxy resin powder coating suitable for steel tube and preparation method of silicon-nitrogen-phosphate coordinating flame retardant epoxy resin powder coating | |
| CN104592697B (en) | Low-density and high-flame-retardant composite porous material and preparation method and application thereof | |
| CN103059675A (en) | Thermal insulating and fire retardant coating of indoor ultrathin steel structure and preparation method of coating | |
| CN106118271A (en) | A kind of Water-borne inflation type refractory coating and preparation technology thereof | |
| CN106497339A (en) | A kind of power equipment environment-friendly fireproof material and preparation method thereof | |
| CN106047067A (en) | Building fireproof material | |
| CN108546438A (en) | A kind of aqueous ultra-thin fire-resistant coating for steel structure and its preparation method and application based on aluminum diethylphosphinate | |
| CN108948911A (en) | A kind of fireproof coating and preparation method thereof for door and window | |
| CN105694566A (en) | Fire-retardant coating for ultrathin steel structure | |
| CN111171657A (en) | Energy-saving environment-friendly fireproof coating and preparation method thereof | |
| CN102277030A (en) | Efficient environment-friendly flame retardant for flame retardance of coating and preparation method thereof | |
| CN107652796A (en) | A kind of thin section steel structure fire-resisting paint and its production method | |
| CN107652740A (en) | A kind of aqueous transparent ancient building fire retarding wood protection coating and preparation method thereof | |
| CN103628350A (en) | Flame-resistant carbon-fiber electrothermal paper and preparation method thereof | |
| CN107337970A (en) | A kind of indoor ultrathin steel structure fireproof coating and preparation method thereof | |
| EP2207672A1 (en) | Flame protection and adhesive layer | |
| CN105061917B (en) | Preparation method of flame-retardant low-smoke polystyrene composite | |
| RU2527997C2 (en) | Composition for thermal barrier coatings | |
| CN104387957A (en) | Antistatic coating and preparation method thereof | |
| CN104478301A (en) | Water-borne ultrathin type fireproof heat insulating material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |