CN116814103A - High-alkalinity magnesium cement-based steel anticorrosion coating - Google Patents
High-alkalinity magnesium cement-based steel anticorrosion coating Download PDFInfo
- Publication number
- CN116814103A CN116814103A CN202310167148.3A CN202310167148A CN116814103A CN 116814103 A CN116814103 A CN 116814103A CN 202310167148 A CN202310167148 A CN 202310167148A CN 116814103 A CN116814103 A CN 116814103A
- Authority
- CN
- China
- Prior art keywords
- steel
- coating
- magnesium
- magnesium cement
- alkalinity
- 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
Links
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 42
- 238000000576 coating method Methods 0.000 title claims abstract description 42
- 239000010959 steel Substances 0.000 title claims abstract description 42
- 239000011248 coating agent Substances 0.000 title claims abstract description 39
- 239000004568 cement Substances 0.000 title claims abstract description 29
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 26
- 239000011777 magnesium Substances 0.000 title claims abstract description 26
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 13
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 12
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims abstract description 11
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 11
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 11
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 11
- 229910021487 silica fume Inorganic materials 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001868 water Inorganic materials 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000005260 corrosion Methods 0.000 claims description 18
- 230000007797 corrosion Effects 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims 1
- 238000002161 passivation Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract 1
- 239000003973 paint Substances 0.000 description 17
- 238000005498 polishing Methods 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 2
- 239000004137 magnesium phosphate Substances 0.000 description 2
- 229960002261 magnesium phosphate Drugs 0.000 description 2
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 2
- 235000010994 magnesium phosphates Nutrition 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010669 acid-base reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000006255 coating slurry Substances 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
- C09D1/06—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances cement
-
- 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
- C09D5/08—Anti-corrosive 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
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
Landscapes
- 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)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention discloses an overbased magnesium cement-based steel anticorrosive coating which comprises, by weight, 50-70% of magnesium oxide, 10-20% of dipotassium hydrogen phosphate, 10-20% of silica fume, 10-20% of water and 2-8% of magnesium hydroxide, wherein the sum of the weight percentages is 100%. The novel high-alkalinity magnesium cement-based steel anticorrosive coating has the advantages of few required raw materials and simple preparation process, and the high-alkalinity characteristic can enable the surface of the steel to form a passivation film protecting layer, so that a good anticorrosive effect is exerted.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to a novel high-alkalinity magnesium cement-based steel anti-corrosion coating.
Background
The steel product with the surface not protected is easy to corrode, and the service cycle is greatly shortened. The corrosion-resistant coating can effectively reduce the corrosion rate of steel products, so that the corrosion-resistant coating is the most common corrosion-resistant measure at present, wherein the most widely applied corrosion-resistant organic coating is mainly used, but the organic coating has long curing time, can release volatile organic substances (such as solvents and the like) and is easy to age and lose efficacy under the influence of environmental factors such as ultraviolet rays and the like. Compared with organic paint, inorganic coating has no release of organic matter and excellent ageing resistance, and is also widely used.
Conventional Magnesium Phosphate Cements (MPC) are inorganic cements that cure by acid-base reactions of acid phosphates and magnesium oxide at room temperature. MPC has the advantages of quick solidification, good adhesion with steel, less influence from environment, no release of volatile organic compounds, and the like, and has corrosion inhibition. Thus, MPC has been used as a long-lasting corrosion-resistant coating material. Unlike traditional MPC, the present invention prepares one kind of high alkalinity magnesium cement paint with basic dipotassium hydrogen phosphate, magnesia, silica fume and magnesium hydroxide as main material and has high alkalinity characteristic to form passivation film protecting layer on steel interface and thus excellent anticorrosive performance.
Disclosure of Invention
The invention aims to provide a novel high-alkalinity magnesium cement-based steel anticorrosion coating which can form a passivation film on the surface of steel so as to have a good anticorrosion effect on the steel, and is a novel green inorganic anticorrosion coating material.
In order to achieve the above purpose, the invention adopts the following technical scheme:
an anticorrosive coating for high-alkalinity magnesium cement-based steel comprises the following raw materials in percentage by weight: 50-70% of magnesium oxide, 10-20% of dipotassium hydrogen phosphate, 10-20% of silica fume, 10-20% of water and 2-8% of magnesium hydroxide, wherein the sum of the weight percentages is 100%.
The application method of the high-alkalinity magnesium cement-based steel anti-corrosion coating comprises the steps of uniformly mixing magnesium oxide, dipotassium hydrogen phosphate, silica fume, water and magnesium hydroxide until the slurry is in a colloidal and viscous state, coating the surface of the pretreated steel, and curing the steel at room temperature for 48 hours after the surface is coagulated.
Further, the thickness of the coating is 0.5 mm-2.0 mm.
Further, the pretreatment of the steel is to clean the surface of the steel by adopting polishing or sand blasting and other processes, and the steel has certain roughness so as to strengthen the adhesion between the coating and the steel and enable the surface of the steel to form a passivation film under alkaline conditions.
Compared with the prior art, the invention has the following beneficial effects:
(1) Compared with organic paint, the magnesium cement-based paint has the advantages of no organic volatile matter, incombustibility, difficult aging and the like;
(2) Compared with inorganic silicate and zinc-rich coating, the magnesium cement-based coating has very good self-adhesive property, can be quickly solidified, and has better hardness after hardening.
(3) The magnesium cement-based coating not only maintains the advantages of the traditional Magnesium Phosphate Cement (MPC) -based coating in the aspects of compressive strength, cohesiveness, water resistance, compactness and the like, but also can form a passivation film protective layer on a steel interface due to the high alkalinity of the material, so that the protective effect of the coating on the steel is further enhanced.
Drawings
FIG. 1 shows the tafel curves of the coatings of examples and comparative examples obtained by immersing 14 d in 3.5% NaCl solution.
Detailed Description
In order to make the contents of the present invention more easily understood, the technical scheme of the present invention will be further described with reference to the specific embodiments, but the present invention is not limited thereto.
Example 1
The raw materials are uniformly mixed according to the proportion of 58.7 percent of magnesium oxide, 12 percent of dipotassium hydrogen phosphate, 17.3 percent of silica fume, 10 percent of water and 2 percent of magnesium hydroxide, so as to obtain the high-alkalinity magnesium cement-based anticorrosive paint. The obtained anticorrosive paint slurry is uniformly painted on the surface of steel after oil removal, rust removal, cleaning, drying and polishing treatment, the thickness of the coating is 500 mu m, and then the steel is placed at room temperature for curing for 48 hours, so that a sample coated with the overbased magnesium cement-based anticorrosive paint is obtained.
Example 2
The high alkaline magnesium cement-based anticorrosive paint is prepared by uniformly mixing 56.7% of magnesium oxide, 12% of dipotassium hydrogen phosphate, 17.3% of silica fume, 10% of water and 4% of magnesium hydroxide. The obtained anticorrosive paint slurry is uniformly painted on the surface of steel after oil removal, rust removal, cleaning, drying and polishing treatment, the thickness of the coating is 500 mu m, and then the steel is placed at room temperature for curing for 48 hours, so that a sample coated with the overbased magnesium cement-based anticorrosive paint is obtained.
Example 3
The high alkaline magnesium cement-based anticorrosive paint is prepared by uniformly mixing 54.7% of magnesium oxide, 12% of dipotassium hydrogen phosphate, 17.3% of silica fume, 10% of water and 6% of magnesium hydroxide. The obtained anticorrosive paint slurry is uniformly painted on the surface of steel after oil removal, rust removal, cleaning, drying and polishing treatment, the thickness of the coating is 500 mu m, and then the steel is placed at room temperature for curing for 48 hours, so that a sample coated with the overbased magnesium cement-based anticorrosive paint is obtained.
Example 4
The magnesium oxide 52.7%, the dipotassium hydrogen phosphate 12%, the silica fume 17.3%, the water 11% and the magnesium hydroxide 8% are uniformly mixed to obtain the high-alkalinity magnesium cement-based anticorrosive paint. The obtained anticorrosive paint slurry is uniformly painted on the surface of steel after oil removal, rust removal, cleaning, drying and polishing treatment, the thickness of the coating is 500 mu m, and then the steel is placed at room temperature for curing for 48 hours, so that a sample coated with the overbased magnesium cement-based anticorrosive paint is obtained.
Comparative example
The magnesium cement-based anticorrosive paint is prepared by uniformly mixing 59.8% of magnesium oxide, 12% of dipotassium hydrogen phosphate, 17.3% of silica fume and 10.9% of water. And uniformly brushing the obtained anti-corrosion coating slurry on the surface of the steel subjected to degreasing, rust removal, cleaning, drying and polishing, wherein the thickness of the coating is 500 mu m, and then placing the steel at room temperature for curing for 48 hours to obtain a sample coated with the magnesium cement anti-corrosion coating.
Table 1 shows the pH of the coatings obtained in examples 1-4 and comparative examples under the same test conditions, and Table 1 demonstrates that replacing part of the magnesium oxide with magnesium hydroxide increases the alkalinity of the coating.
TABLE 1 coating pH test results
The samples subjected to the corrosion protection treatment in examples 1-4 and comparative examples are subjected to performance test according to the applicable convention of the electrochemical measurement method for corrosion and corrosion test of GB/T40299-2021 steel and alloy. FIG. 1 shows the tafel curves of the coatings of examples 1-4 and comparative examples obtained after preservative treatment by immersing the samples in a 3.5% NaCl solution in 14 d. As can be seen from fig. 1, the higher the alkalinity of the coating, the better the corrosion protection of the coating, since the higher the alkalinity the faster the rate of formation of the passivation film and the more complete the film.
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (3)
1. An overbased magnesium cement-based steel corrosion resistant coating, characterized by: the high-alkalinity magnesium cement-based steel anticorrosive coating comprises the following raw materials in percentage by weight: 50-70% of magnesium oxide, 10-20% of dipotassium hydrogen phosphate, 10-20% of silica fume, 10-20% of water and 2-8% of magnesium hydroxide, wherein the sum of the weight percentages is 100%.
2. The overbased magnesium cement-based steel corrosion protection coating of claim 1, wherein: uniformly mixing magnesium oxide, dipotassium hydrogen phosphate, silica fume, water and magnesium hydroxide, coating the mixture on the surface of the pretreated steel, and curing the steel for 48 hours at room temperature after the steel is coagulated.
3. The overbased magnesium cement-based steel corrosion protection coating of claim 1, wherein: the thickness of the coating is 0.5 mm-2.0 mm.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202310167148.3A CN116814103A (en) | 2023-02-27 | 2023-02-27 | High-alkalinity magnesium cement-based steel anticorrosion coating |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202310167148.3A CN116814103A (en) | 2023-02-27 | 2023-02-27 | High-alkalinity magnesium cement-based steel anticorrosion coating |
Publications (1)
Publication Number | Publication Date |
---|---|
CN116814103A true CN116814103A (en) | 2023-09-29 |
Family
ID=88141759
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202310167148.3A Pending CN116814103A (en) | 2023-02-27 | 2023-02-27 | High-alkalinity magnesium cement-based steel anticorrosion coating |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN116814103A (en) |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2011071569A1 (en) * | 2009-12-11 | 2011-06-16 | Latitude 18, Inc. | Inorganic phosphate corrosion resistant coatings |
CN105174900A (en) * | 2015-09-17 | 2015-12-23 | 盐城工学院 | Sulfate-corrosion-resistant coating material with concrete structure and preparation method of sulfate-corrosion-resistant coating material |
CN115029023A (en) * | 2022-06-13 | 2022-09-09 | 西南科技大学 | Chemical bonding type fireproof anticorrosive paint for steel structure and preparation method thereof |
-
2023
- 2023-02-27 CN CN202310167148.3A patent/CN116814103A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2011071569A1 (en) * | 2009-12-11 | 2011-06-16 | Latitude 18, Inc. | Inorganic phosphate corrosion resistant coatings |
CN102770583A (en) * | 2009-12-11 | 2012-11-07 | 18纬度有限公司 | Inorganic phosphate corrosion resistant coatings |
CN105174900A (en) * | 2015-09-17 | 2015-12-23 | 盐城工学院 | Sulfate-corrosion-resistant coating material with concrete structure and preparation method of sulfate-corrosion-resistant coating material |
CN115029023A (en) * | 2022-06-13 | 2022-09-09 | 西南科技大学 | Chemical bonding type fireproof anticorrosive paint for steel structure and preparation method thereof |
Non-Patent Citations (2)
Title |
---|
殷思艺等: "碳钢表面磷酸酶防腐涂料的制备及改性研究", 涂料工业, vol. 50, no. 7, 31 July 2020 (2020-07-31), pages 35 - 41 * |
秦真波;夏大海;吴忠;胡文彬;: "磷酸盐无机涂料及其研究进展", 表面技术, no. 12, 20 December 2019 (2019-12-20), pages 46 - 54 * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN102127328B (en) | Aqueous on-rust inorganic zinc-enriched coating and preparation method thereof | |
KR101865092B1 (en) | Anti-corrosion water-soluble paint and varnish composition | |
CN102766388A (en) | Heavy-duty coating for prolonging life of sheet metals and preparation method thereof | |
KR101046264B1 (en) | Ceramic powder coating composion, steel pipe pile coated the same and process for preparing the same | |
CN101671515A (en) | Anticorrosive coating for concrete structure reinforcing bars and preparation method thereof | |
CN107531574B (en) | Chromate free ceramic coating composition | |
CN108300302B (en) | Metal surface silane treating agent and preparation method thereof | |
KR101896011B1 (en) | Anti-corrision varnish composition and forming method for anti-corrision coating layer using the same | |
CN1259553A (en) | Protective coating | |
CN102816486B (en) | Rust-removing-free environment-friendly acrylic acid zinc phosphate organic composite ceramic anticorrosive paint and preparation method thereof | |
CN113149597A (en) | Potassium phosphate magnesium-based steel anticorrosive coating material and preparation method thereof | |
CN112143268B (en) | Preparation of phosphate bonded polytetrafluoroethylene coating and coating | |
CN116814103A (en) | High-alkalinity magnesium cement-based steel anticorrosion coating | |
CN111073358A (en) | Phosphate water-based heavy-duty anticorrosive coating and preparation method and construction method thereof | |
CN116253536B (en) | Alkali-activated geopolymer coating and preparation method and application thereof | |
CN109096802B (en) | Phosphate-based inorganic metal anticorrosive paint and application thereof | |
CN110922797A (en) | Anticorrosive nano coating and preparation method thereof | |
CN110950606B (en) | Concrete with antirust function and application process thereof | |
JPH0873778A (en) | Zinc-rich paint and its production | |
KR101963448B1 (en) | Chromium-free zinc-aluminium composite inorganic coating agent, manufacturing method thereof and coating method using the same | |
JP7284452B2 (en) | Rust preventive manufacturing method, rust preventive method, and repair method for reinforced concrete structure | |
CN1113927A (en) | Aqueous anti-corrosion treating agent and its preparing and using method | |
CN1114665C (en) | Zinc base water soluble anti-corrosion paint for metal surface and its prepn. method | |
CN111940258A (en) | Corrosion-resistant coating on surface of magnesium alloy building template and preparation method thereof | |
JPH0122215B2 (en) |
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 |