CN111690309A - Normal-temperature curing water-based epoxy resin coating and preparation method thereof - Google Patents
Normal-temperature curing water-based epoxy resin coating and preparation method thereof Download PDFInfo
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- CN111690309A CN111690309A CN202010687237.7A CN202010687237A CN111690309A CN 111690309 A CN111690309 A CN 111690309A CN 202010687237 A CN202010687237 A CN 202010687237A CN 111690309 A CN111690309 A CN 111690309A
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- 238000000576 coating method Methods 0.000 title claims abstract description 69
- 239000011248 coating agent Substances 0.000 title claims abstract description 64
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 42
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 40
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 31
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 18
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 15
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 15
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims abstract description 14
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 13
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 13
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000839 emulsion Substances 0.000 claims abstract description 13
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 71
- 238000006243 chemical reaction Methods 0.000 claims description 57
- 239000002585 base Substances 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 claims description 16
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 16
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 claims description 16
- YCOZIPAWZNQLMR-UHFFFAOYSA-N pentadecane Chemical compound CCCCCCCCCCCCCCC YCOZIPAWZNQLMR-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000011812 mixed powder Substances 0.000 claims description 14
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 14
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- IVSZLXZYQVIEFR-UHFFFAOYSA-N m-xylene Chemical group CC1=CC=CC(C)=C1 IVSZLXZYQVIEFR-UHFFFAOYSA-N 0.000 claims description 12
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 10
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- GEZGAZKEOUKLBR-UHFFFAOYSA-N 1-phenylpyrrole Chemical compound C1=CC=CN1C1=CC=CC=C1 GEZGAZKEOUKLBR-UHFFFAOYSA-N 0.000 claims description 8
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 8
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 8
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 8
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 229910003445 palladium oxide Inorganic materials 0.000 claims description 8
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 8
- JQPTYAILLJKUCY-UHFFFAOYSA-N palladium(ii) oxide Chemical compound [O-2].[Pd+2] JQPTYAILLJKUCY-UHFFFAOYSA-N 0.000 claims description 8
- 239000011787 zinc oxide Substances 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 6
- 239000000460 chlorine Substances 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 5
- 235000011152 sodium sulphate Nutrition 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- -1 polydimethylsiloxane Polymers 0.000 claims description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052593 corundum Inorganic materials 0.000 claims description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 2
- 239000003973 paint Substances 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 11
- 239000006260 foam Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 239000005028 tinplate Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/08—Preparation of nitro compounds by substitution of hydrogen atoms by nitro groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C263/00—Preparation of derivatives of isocyanic acid
- C07C263/04—Preparation of derivatives of isocyanic acid from or via carbamates or carbamoyl halides
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C263/00—Preparation of derivatives of isocyanic acid
- C07C263/16—Preparation of derivatives of isocyanic acid by reactions not involving the formation of isocyanate groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C269/00—Preparation of derivatives of carbamic acid, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/553—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having one nitrogen atom as the only ring hetero atom
- C07F9/572—Five-membered rings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/4007—Curing agents not provided for by the groups C08G59/42 - C08G59/66
- C08G59/4014—Nitrogen containing compounds
- C08G59/4028—Isocyanates; Thioisocyanates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5033—Amines aromatic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Inorganic Chemistry (AREA)
- Epoxy Resins (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a normal temperature curing water-based epoxy resin coating and a preparation method thereof, wherein the coating comprises a coating base liquid and a modified curing agent, and the coating base liquid and the modified curing agent are mixed according to the volume ratio of 2: 1, mixing, wherein the coating base liquid is prepared from the following raw materials in parts by weight: 100-120 parts of water-based epoxy resin emulsion, 0.5-2 parts of zinc stearate, 0.5-2 parts of heat-resistant auxiliary agent, 0.01-0.05 part of defoaming agent, 5-15 parts of talcum powder, 5-15 parts of kaolin powder and 4-6 parts of emulsifier; after the modified curing agent and the coating base liquid are mixed and coated, the coating molecules become high molecules with a three-dimensional network structure, so that the water resistance of the coating is improved, and the heat-resistant auxiliary agent is prepared.
Description
Technical Field
The invention belongs to the technical field of coating production, and particularly relates to a normal-temperature curing water-based epoxy resin coating and a preparation method thereof.
Background
As one of the three general thermosetting resins, epoxy resin is widely applied to the fields of mechano-electronics, aerospace, transportation, construction and the like due to its excellent technological properties, mechanical properties and physical properties, and epoxy resin usually uses a large amount of organic solvent during application, which increases the cost on one hand, and on the other hand, because the volatilization of organic solvent causes environmental pollution and harm to human health, the application of solvent epoxy resin is more and more limited, and even is forbidden by developed countries.
After a paint film generated after the traditional water-based epoxy resin paint is coated is soaked in water for a long time, the surface of the paint film foams and even the paint film falls off, so that the paint loses the protection effect, part of the paint film can be used under a high-temperature condition, and the paint film is baked at a high temperature for a long time, so that the surface of the paint film cracks and foams, and the performance of the paint is greatly reduced.
Disclosure of Invention
The invention aims to provide a normal-temperature curing water-based epoxy resin coating and a preparation method thereof.
The technical problems to be solved by the invention are as follows:
after a paint film generated after the traditional water-based epoxy resin paint is coated is soaked in water for a long time, the surface of the paint film foams and even the paint film falls off, so that the paint loses the protection effect, part of the paint film can be used under a high-temperature condition, and the paint film is baked at a high temperature for a long time, so that the surface of the paint film cracks and foams, and the performance of the paint is greatly reduced.
The purpose of the invention can be realized by the following technical scheme:
a normal temperature curing water-based epoxy resin coating comprises a coating base liquid and a modified curing agent;
the coating base liquid is prepared from the following raw materials in parts by weight: 100-120 parts of water-based epoxy resin emulsion, 0.5-2 parts of zinc stearate, 0.5-2 parts of heat-resistant auxiliary agent, 0.01-0.05 part of defoaming agent, 5-15 parts of talcum powder, 5-15 parts of kaolin powder and 4-6 parts of emulsifier;
the coating base liquid is prepared by the following steps:
step S1: adding zinc stearate, talcum powder and kaolin powder into a crusher, crushing, sieving by a 300-mesh sieve with 500 meshes, and mixing to obtain mixed powder;
step S2: adding dimethylacetamide and a heat-resistant auxiliary agent into a reaction kettle, stirring at the temperature of 30-50 ℃ until the dimethylacetamide and the heat-resistant auxiliary agent are uniformly mixed, adding an aqueous epoxy resin emulsion, and stirring at the temperature of 60-80 ℃ for 20-30min to prepare a premixed solution;
step S3: and (4) adding the premixed liquid prepared in the step S2 and the mixed powder prepared in the step S1 into a stirring kettle, stirring for 20-30min under the condition that the rotating speed is 1200-1500r/min, adding the emulsifier and the defoaming agent, and continuously stirring for 1-1.5h to prepare the coating base liquid.
Further, the defoaming agent is one or two of polydimethylsiloxane and ethylene glycol siloxane which are mixed in any proportion, and the emulsifier is one or two of sodium dodecyl sulfate and sodium dodecyl benzene sulfonate which are mixed in any proportion.
Further, the modified curing agent is prepared by the following steps:
step A1: adding p-xylene into a reaction kettle, stirring and adding a first mixed acid under the condition that the rotation speed is 300-500r/min, reacting for 30-40min at the temperature of 40-50 ℃, adding a second mixed acid, and reacting for 1-1.5h at the temperature of 60-70 ℃ to obtain an intermediate F1;
the reaction process is as follows:
step A2: adding the intermediate F1 and ethanol obtained in the step A1 into a reaction kettle, stirring until the intermediate F1 is completely dissolved, adding palladium chloride, reacting for 3-4h under the conditions that the pressure is 7-8MPa and the temperature is 175-185 ℃, adding n-pentadecane and zinc oxide, introducing nitrogen for protection, and reacting under the conditions that the pressure is 0.8-1.5MPa and the temperature is 250-300 ℃ to obtain an intermediate F2;
the reaction process is as follows:
step A3: adding the intermediate F2 prepared in the step A2 and ferric chloride into a reaction kettle, introducing chlorine to fill the reaction kettle, reacting for 30-40min to prepare an intermediate F3, adding the intermediate F3 and hydrocyanic acid into a fluidized bed reactor, and passing through NiO-Al at the temperature of 550-600 DEG C2O3Catalyst, reacting to obtain intermediate F4;
the reaction process is as follows:
step A4: and B, adding the intermediate F4 prepared in the step A3 and m-xylene into a reaction kettle, stirring until the intermediate F4 is completely mixed, adding cobalt oxide and palladium oxide, and reacting for 4-5h under the conditions that the pressure is 15-20MPa and the temperature is 120-150 ℃ to prepare the modified curing agent.
The reaction process is as follows:
further, the dosage volume ratio of the p-xylene, the first mixed acid and the second mixed acid in the step A1 is 2: 1: 1, the dosage ratio of the intermediate F1, the palladium chloride, the n-pentadecane and the zinc oxide in the step A2 is 10 mL:3 g: 5mL of: 2g, wherein the mass ratio of the intermediate F2 to the ferric chloride in the step A3 is 5: 1, intermediate F3, hydrocyanic acid, NiO-Al2O3The catalyst dosage ratio is 10 mL:3g, wherein the dosage ratio of the intermediate F4, the cobalt oxide and the palladium oxide in the step A4 is 10 mL:3 g: 3g of the total weight.
Further, the first mixed acid in the step a1 is prepared by mixing nitric acid, sulfuric acid and deionized water in a volume ratio of 2.7: 6.3: 1, mixing the second mixed acid with nitric acid, sulfuric acid and deionized water in a volume ratio of 6: 3: 1 and mixing.
Further, the heat-resistant auxiliary agent is prepared by the following steps:
step B1: adding 1-phenylpyrrole into a reaction kettle, stirring the mixture at the temperature of 60-70 ℃ until the 1-phenylpyrrole is completely molten, adding concentrated sulfuric acid, reacting the mixture for 10-12h at the temperature of 140-170 ℃, adding sodium sulfate, and reacting the mixture for 20-30min at the rotation speed of 200-300r/min to obtain an intermediate E1;
the reaction process is as follows:
step B2: adding the intermediate E1 and a sodium hydroxide solution into a reaction kettle, stirring for 20-30min under the condition that the rotating speed is 300-500r/min, adding a hydrochloric acid solution, and continuously stirring for 10-15min to obtain an intermediate E2;
the reaction process is as follows:
step B3: mixing a potassium dichromate aqueous solution with concentrated sulfuric acid to prepare a mixed solution, adding the intermediate E2 prepared in the step B2 and ethanol into a reaction kettle, stirring for 10-15min under the condition that the rotation speed is 100-200r/min until the intermediate E2 is completely dissolved, slowly adding the mixed solution under the condition that the temperature is 30-35 ℃, and reacting for 1.5-2h under the condition that the temperature is 40-50 ℃ to prepare an intermediate E3;
the reaction process is as follows:
step B4: and B3, adding the intermediate E3 and dichloromethane into a reaction kettle, stirring until the intermediate E3 is completely dissolved, adding aluminum chloride powder, stirring for 10-15min at the rotation speed of 300-130 ℃ and 500r/min, slowly dropwise adding phosphorus oxychloride at the temperature of 55-60 ℃, and reacting for 8-10h at the temperature of 110-130 ℃ after dropwise adding to obtain the heat-resistant auxiliary agent.
The reaction process is as follows:
further, the amount ratio of the 1-phenylpyrrole, the concentrated sulfuric acid and the sodium sulfate in the step B1 is 1: 1.2: 1.2, the dosage ratio of the intermediate E1, the sodium hydroxide solution and the hydrochloric acid solution in the step B2 is 10 g: 5mL of: 8mL, 30-35% of sodium hydroxide solution by mass, 60-65% of hydrochloric acid solution by mass, and the volume ratio of the potassium dichromate aqueous solution to the concentrated sulfuric acid in the step B3 is 1: 1.7, the mass fraction of the potassium dichromate aqueous solution is 45-50%, and the dosage ratio of the intermediate E2 to the mixed solution is 1 g: 40mL, the using amount ratio of the intermediate E3, the aluminum chloride powder and the phosphorus oxychloride in the step B4 is 6g to 1.2g to 1mL, and the mass fractions of the concentrated sulfuric acid in the step B1 and the step B3 are 98%.
The invention has the beneficial effects that: the invention prepares a modified curing agent in the process of preparing a normal temperature curing water-based epoxy resin coating, the molecule of the modified curing agent contains nitrogen atoms, the nitrogen atoms contain active hydrogen, when the coating is used, the volume ratio of the modified curing agent to the coating base liquid is 2: 1, after coating, active hydrogen on molecules of a modified curing agent opens epoxy groups on molecules of the waterborne epoxy resin to enable the waterborne epoxy resin to be crosslinked and cured, the molecules of the modified curing agent contain isocyanate groups, the isocyanate groups can react with hydroxyl groups in the waterborne epoxy resin and are further cured with water, carbon dioxide can be generated in the reaction process to form a water-insoluble vesicular condensation body, so that the molecules of a coating film become macromolecules with a three-dimensional net structure, and further the water resistance of the coating film is improved, meanwhile, the invention also prepares a heat-resistant auxiliary agent in the process of preparing the coating, the heat-resistant auxiliary agent can complex metal chloride when being mixed with zinc stearate, so as to improve the heat resistance and the weather resistance of the coating, the molecules of the heat-resistant auxiliary agent contain benzene rings and imide heterocycles, the crosslinking density of the molecules is higher, and when the heat-resistant auxiliary agent is crosslinked with the waterborne, the proportion of rotatable monomers on the epoxy resin molecules is reduced, the rigidity of the epoxy resin molecular chain is increased, and the heat resistance of the coating is further improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A normal temperature curing water-based epoxy resin coating comprises a coating base liquid and a modified curing agent;
the coating base liquid is prepared from the following raw materials in parts by weight: 100 parts of water-based epoxy resin emulsion, 0.5 part of zinc stearate, 0.5 part of heat-resistant auxiliary agent, 0.01 part of defoaming agent, 5 parts of talcum powder, 5 parts of kaolin powder and 4 parts of emulsifier;
the coating base liquid is prepared by the following steps:
step S1: adding zinc stearate, talcum powder and kaolin powder into a grinder, grinding, sieving by a 300-mesh sieve, and mixing to obtain mixed powder;
step S2: adding dimethylacetamide and a heat-resistant auxiliary agent into a reaction kettle, stirring at the temperature of 30 ℃ until the dimethylacetamide and the heat-resistant auxiliary agent are uniformly mixed, adding an aqueous epoxy resin emulsion, and stirring at the temperature of 60 ℃ for 20min to prepare a premixed solution;
step S3: and (4) adding the premixed liquid prepared in the step S2 and the mixed powder prepared in the step S1 into a stirring kettle, stirring for 20min under the condition that the rotating speed is 1200r/min, adding the emulsifier and the defoaming agent, and continuously stirring for 1h to prepare the coating base liquid.
The modified curing agent is prepared by the following steps:
step A1: adding p-xylene into a reaction kettle, stirring and adding a first mixed acid under the condition that the rotating speed is 300r/min, reacting for 30min at the temperature of 40 ℃, adding a second mixed acid, and reacting for 1h at the temperature of 60 ℃ to obtain an intermediate F1;
step A2: adding the intermediate F1 prepared in the step A1 and ethanol into a reaction kettle, stirring until the intermediate F1 is completely dissolved, adding palladium chloride, reacting for 3 hours under the conditions of pressure of 7MPa and temperature of 175 ℃, adding n-pentadecane and zinc oxide, introducing nitrogen for protection, and reacting under the conditions of pressure of 0.8MPa and temperature of 250 ℃ to prepare an intermediate F2;
step A3: adding the intermediate F2 prepared in the step A2 and ferric chloride into a reaction kettle, introducing chlorine to fill the reaction kettle, reacting for 30min to prepare an intermediate F3, adding the intermediate F3 and hydrocyanic acid into a fluidized bed reactor, and passing through NiO-Al at the temperature of 550 DEG C2O3Catalyst, reacting to obtain intermediate F4;
step A4: and B, adding the intermediate F4 prepared in the step A3 and m-xylene into a reaction kettle, stirring until the intermediate F4 is completely mixed, adding cobalt oxide and palladium oxide, and reacting for 4 hours under the conditions that the pressure is 15MPa and the temperature is 120 ℃ to prepare the modified curing agent.
The heat-resistant auxiliary agent is prepared by the following steps:
step B1: adding 1-phenylpyrrole into a reaction kettle, stirring at the temperature of 60 ℃ until the 1-phenylpyrrole is completely molten, adding concentrated sulfuric acid, reacting at the temperature of 140 ℃ for 10 hours, adding sodium sulfate, and reacting at the rotation speed of 200r/min for 20 minutes to obtain an intermediate E1;
step B2: adding the intermediate E1 and a sodium hydroxide solution into a reaction kettle, stirring for 20min under the condition that the rotating speed is 300r/min, adding a hydrochloric acid solution, and continuously stirring for 10min to obtain an intermediate E2;
step B3: mixing a potassium dichromate aqueous solution with concentrated sulfuric acid to prepare a mixed solution, adding the intermediate E2 prepared in the step B2 and ethanol into a reaction kettle, stirring for 10min under the condition that the rotating speed is 100r/min until the intermediate E2 is completely dissolved, slowly adding the mixed solution under the condition that the temperature is 30 ℃, and reacting for 1.5h under the condition that the temperature is 40 ℃ to prepare an intermediate E3;
step B4: and B3, adding the intermediate E3 and dichloromethane prepared in the step B3 into a reaction kettle, stirring until the intermediate E3 is completely dissolved, adding aluminum chloride powder, stirring for 10min at the rotation speed of 300r/min, slowly dropwise adding phosphorus oxychloride at the temperature of 55 ℃, and reacting for 8h at the temperature of 110 ℃ after dropwise adding to obtain the heat-resistant auxiliary agent.
When in use, the coating base liquid and the modified curing agent are mixed according to the volume ratio of 2: 1 and mixing.
Example 2
A normal temperature curing water-based epoxy resin coating comprises a coating base liquid and a modified curing agent;
the coating base liquid is prepared from the following raw materials in parts by weight: 110 parts of water-based epoxy resin emulsion, 1 part of zinc stearate, 1 part of heat-resistant auxiliary agent, 0.03 part of defoaming agent, 10 parts of talcum powder, 10 parts of kaolin powder and 5 parts of emulsifier;
the coating base liquid is prepared by the following steps:
step S1: adding zinc stearate, talcum powder and kaolin powder into a grinder, grinding, sieving by a 400-mesh sieve, and mixing to obtain mixed powder;
step S2: adding dimethylacetamide and a heat-resistant auxiliary agent into a reaction kettle, stirring at 40 ℃ until the dimethylacetamide and the heat-resistant auxiliary agent are uniformly mixed, adding an aqueous epoxy resin emulsion, and stirring at 70 ℃ for 25min to prepare a premixed solution;
step S3: and (4) adding the premixed liquid prepared in the step S2 and the mixed powder prepared in the step S1 into a stirring kettle, stirring for 25min under the condition that the rotating speed is 1300r/min, adding the emulsifier and the defoaming agent, and continuously stirring for 1.3h to prepare the coating base liquid.
The modified curing agent is prepared by the following steps:
step A1: adding p-xylene into a reaction kettle, stirring and adding a first mixed acid under the condition that the rotating speed is 400r/min, reacting for 35min at the temperature of 45 ℃, adding a second mixed acid, and reacting for 1.3h at the temperature of 65 ℃ to obtain an intermediate F1;
step A2: adding the intermediate F1 prepared in the step A1 and ethanol into a reaction kettle, stirring until the intermediate F1 is completely dissolved, adding palladium chloride, reacting for 3.5 hours under the conditions that the pressure is 7.5MPa and the temperature is 180 ℃, adding n-pentadecane and zinc oxide, introducing nitrogen for protection, and reacting under the conditions that the pressure is 1.2MPa and the temperature is 280 ℃ to prepare an intermediate F2;
step A3: adding the intermediate F2 prepared in the step A2 and ferric chloride into a reaction kettle, introducing chlorine to fill the reaction kettle, reacting for 35min to prepare an intermediate F3, adding the intermediate F3 and hydrocyanic acid into a fluidized bed reactor, and passing through NiO-Al at the temperature of 580 DEG C2O3Catalyst, reacting to obtain intermediate F4;
step A4: and B, adding the intermediate F4 prepared in the step A3 and m-xylene into a reaction kettle, stirring until the intermediate F4 is completely mixed, adding cobalt oxide and palladium oxide, and reacting for 4.5 hours under the conditions that the pressure is 18MPa and the temperature is 130 ℃ to prepare the modified curing agent.
When in use, the coating base liquid and the modified curing agent are mixed according to the volume ratio of 2: 1 and mixing.
Example 3
A normal temperature curing water-based epoxy resin coating comprises a coating base liquid and a modified curing agent;
the coating base liquid is prepared from the following raw materials in parts by weight: 120 parts of water-based epoxy resin emulsion, 2 parts of zinc stearate, 2 parts of heat-resistant auxiliary agent, 0.05 part of defoaming agent, 15 parts of talcum powder, 15 parts of kaolin powder and 6 parts of emulsifier;
the coating base liquid is prepared by the following steps:
step S1: adding zinc stearate, talcum powder and kaolin powder into a grinder, grinding, sieving by a 500-mesh sieve, and mixing to obtain mixed powder;
step S2: adding dimethylacetamide and a heat-resistant auxiliary agent into a reaction kettle, stirring at the temperature of 50 ℃ until the dimethylacetamide and the heat-resistant auxiliary agent are uniformly mixed, adding an aqueous epoxy resin emulsion, and stirring at the temperature of 80 ℃ for 30min to prepare a premixed solution;
step S3: and (4) adding the premixed liquid prepared in the step S2 and the mixed powder prepared in the step S1 into a stirring kettle, stirring for 30min at the rotation speed of 1500r/min, adding an emulsifier and a defoaming agent, and continuously stirring for 1.5h to prepare the coating base liquid.
The modified curing agent is prepared by the following steps:
step A1: adding p-xylene into a reaction kettle, stirring and adding a first mixed acid under the condition that the rotating speed is 500r/min, reacting for 40min at the temperature of 50 ℃, adding a second mixed acid, and reacting for 1.5h at the temperature of 70 ℃ to obtain an intermediate F1;
step A2: adding the intermediate F1 prepared in the step A1 and ethanol into a reaction kettle, stirring until the intermediate F1 is completely dissolved, adding palladium chloride, reacting for 4 hours under the conditions of pressure of 8MPa and temperature of 185 ℃, adding n-pentadecane and zinc oxide, introducing nitrogen for protection, and reacting under the conditions of pressure of 1.5MPa and temperature of 300 ℃ to prepare an intermediate F2;
step A3: adding the intermediate F2 prepared in the step A2 and ferric chloride into a reaction kettle, introducing chlorine to fill the reaction kettle, reacting for 40min to prepare an intermediate F3, adding the intermediate F3 and hydrocyanic acid into a fluidized bed reactor, and passing through NiO-Al at the temperature of 600 DEG C2O3Catalyst, reacting to obtain intermediate F4;
step A4: and B, adding the intermediate F4 prepared in the step A3 and m-xylene into a reaction kettle, stirring until the intermediate F4 is completely mixed, adding cobalt oxide and palladium oxide, and reacting for 5 hours under the conditions that the pressure is 20MPa and the temperature is 150 ℃ to prepare the modified curing agent.
When in use, the coating base liquid and the modified curing agent are mixed according to the volume ratio of 2: 1 and mixing.
Comparative example 1
Compared with the example 1, the heat-resistant assistant is not added in the comparative example, and the coating is prepared by the following specific steps:
step S1: adding zinc stearate, talcum powder and kaolin powder into a grinder, grinding, sieving by a 300-mesh sieve, and mixing to obtain mixed powder;
step S2: adding dimethylacetamide and aqueous epoxy resin emulsion into a stirring kettle, and stirring for 20min at the temperature of 60 ℃ to prepare a premixed solution;
step S3: and (4) adding the premixed liquid prepared in the step S2 and the mixed powder prepared in the step S1 into a stirring kettle, stirring for 20min under the condition that the rotating speed is 1200r/min, adding the emulsifier and the defoaming agent, and continuously stirring for 1h to prepare the coating base liquid.
When in use, the coating base liquid and the modified curing agent are mixed according to the volume ratio of 2: 1 and mixing.
Comparative example 2
Compared with example 1, the modified curing agent is replaced by diethylenetriamine during the use process of the comparative example.
Comparative example 3
The comparative example is a water-based epoxy resin coating which is common in the market.
The results of the performance test on the coatings prepared in examples 1 to 3 and comparative examples 1 to 3 are shown in table 1 below;
water resistance: the coatings prepared in examples 1 to 3 and comparative examples 1 to 3 were respectively applied to a tin plate having a specification of 50mm × 120mm × 0.3, the tin plate was immersed in distilled water for 60, 90, and 120 days, respectively, and the state of the surface paint film was observed.
Heat resistance: the coatings prepared in examples 1 to 3 and comparative examples 1 to 3 were applied to a tin plate having a size of 50mm × 120mm × 0.3, respectively, and the tin plate was left at temperatures of 400, 500, 600, 700, 800, and 900 ℃ for 100 and 200 hours, and the state of the topcoat film was observed.
TABLE 1
From the above table 1, it can be seen that the coatings prepared in examples 1-3 and comparative example 1 do not have the phenomenon of foaming or peeling off after being soaked in distilled water for 60 days, 90 days and 120 days, respectively, and the coatings prepared in examples 1-3 and comparative example 2 do not have the phenomenon of cracking and foaming after being baked for 100-200h at the temperature of 400-900 ℃.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (8)
1. A normal temperature curing water-based epoxy resin coating is characterized in that: comprises a coating base liquid and a modified curing agent;
the coating base liquid is prepared from the following raw materials in parts by weight: 100-120 parts of water-based epoxy resin emulsion, 0.5-2 parts of zinc stearate, 0.5-2 parts of heat-resistant auxiliary agent, 0.01-0.05 part of defoaming agent, 5-15 parts of talcum powder, 5-15 parts of kaolin powder and 4-6 parts of emulsifier;
the coating base liquid is prepared by the following steps:
step S1: adding zinc stearate, talcum powder and kaolin powder into a crusher, crushing, sieving by a 300-mesh sieve with 500 meshes, and mixing to obtain mixed powder;
step S2: adding dimethylacetamide and a heat-resistant auxiliary agent into a reaction kettle, stirring at the temperature of 30-50 ℃ until the dimethylacetamide and the heat-resistant auxiliary agent are uniformly mixed, adding an aqueous epoxy resin emulsion, and stirring at the temperature of 60-80 ℃ for 20-30min to prepare a premixed solution;
step S3: and (4) adding the premixed liquid prepared in the step S2 and the mixed powder prepared in the step S1 into a stirring kettle, stirring for 20-30min under the condition that the rotating speed is 1200-1500r/min, adding the emulsifier and the defoaming agent, and continuously stirring for 1-1.5h to prepare the coating base liquid.
2. The normal-temperature curing water-based epoxy resin coating as claimed in claim 1, wherein: the defoaming agent is one or two of polydimethylsiloxane and ethylene glycol siloxane which are mixed according to any proportion, and the emulsifier is one or two of sodium dodecyl sulfate and sodium dodecyl benzene sulfonate which are mixed according to any proportion.
3. The normal-temperature curing water-based epoxy resin coating as claimed in claim 1, wherein: the modified curing agent is prepared by the following steps:
step A1: adding p-xylene into a reaction kettle, stirring and adding a first mixed acid under the condition that the rotation speed is 300-500r/min, reacting for 30-40min at the temperature of 40-50 ℃, adding a second mixed acid, and reacting for 1-1.5h at the temperature of 60-70 ℃ to obtain an intermediate F1;
step A2: adding the intermediate F1 and ethanol obtained in the step A1 into a reaction kettle, stirring until the intermediate F1 is completely dissolved, adding palladium chloride, reacting for 3-4h under the conditions that the pressure is 7-8MPa and the temperature is 175-185 ℃, adding n-pentadecane and zinc oxide, introducing nitrogen for protection, and reacting under the conditions that the pressure is 0.8-1.5MPa and the temperature is 250-300 ℃ to obtain an intermediate F2;
step A3: adding the intermediate F2 prepared in the step A2 and ferric chloride into a reaction kettle, introducing chlorine to fill the reaction kettle, reacting for 30-40min to prepare an intermediate F3, adding the intermediate F3 and hydrocyanic acid into a fluidized bed reactor, and passing through NiO-Al at the temperature of 550-600 DEG C2O3Catalyst, reacting to obtain intermediate F4;
step A4: and B, adding the intermediate F4 prepared in the step A3 and m-xylene into a reaction kettle, stirring until the intermediate F4 is completely mixed, adding cobalt oxide and palladium oxide, and reacting for 4-5h under the conditions that the pressure is 15-20MPa and the temperature is 120-150 ℃ to prepare the modified curing agent.
4. The normal-temperature curing water-based epoxy resin coating as claimed in claim 3, wherein: the volume ratio of the p-xylene to the first mixed acid to the second mixed acid in the step A1 is 2: 1: 1, intermediate F1 described in step a2, palladium chloride,The dosage ratio of the n-pentadecane to the zinc oxide is 10 mL:3 g: 5mL of: 2g, wherein the mass ratio of the intermediate F2 to the ferric chloride in the step A3 is 5: 1, intermediate F3, hydrocyanic acid, NiO-Al2O3The catalyst dosage ratio is 10 mL:3g, wherein the dosage ratio of the intermediate F4, the cobalt oxide and the palladium oxide in the step A4 is 10 mL:3 g: 3g of the total weight.
5. The normal-temperature curing water-based epoxy resin coating as claimed in claim 3, wherein: the first mixed acid in the step A1 is prepared by mixing nitric acid, sulfuric acid and deionized water in a volume ratio of 2.7: 6.3: 1, mixing the second mixed acid with nitric acid, sulfuric acid and deionized water in a volume ratio of 6: 3: 1 and mixing.
6. The normal-temperature curing water-based epoxy resin coating as claimed in claim 1, wherein:
step B1: adding 1-phenylpyrrole into a reaction kettle, stirring the mixture at the temperature of 60-70 ℃ until the 1-phenylpyrrole is completely molten, adding concentrated sulfuric acid, reacting the mixture for 10-12h at the temperature of 140-170 ℃, adding sodium sulfate, and reacting the mixture for 20-30min at the rotation speed of 200-300r/min to obtain an intermediate E1;
step B2: adding the intermediate E1 and a sodium hydroxide solution into a reaction kettle, stirring for 20-30min under the condition that the rotating speed is 300-500r/min, adding a hydrochloric acid solution, and continuously stirring for 10-15min to obtain an intermediate E2;
step B3: mixing a potassium dichromate aqueous solution with concentrated sulfuric acid to prepare a mixed solution, adding the intermediate E2 prepared in the step B2 and ethanol into a reaction kettle, stirring for 10-15min under the condition that the rotation speed is 100-200r/min until the intermediate E2 is completely dissolved, slowly adding the mixed solution under the condition that the temperature is 30-35 ℃, and reacting for 1.5-2h under the condition that the temperature is 40-50 ℃ to prepare an intermediate E3;
step B4: and B3, adding the intermediate E3 and dichloromethane into a reaction kettle, stirring until the intermediate E3 is completely dissolved, adding aluminum chloride powder, stirring for 10-15min at the rotation speed of 300-130 ℃ and 500r/min, slowly dropwise adding phosphorus oxychloride at the temperature of 55-60 ℃, and reacting for 8-10h at the temperature of 110-130 ℃ after dropwise adding to obtain the heat-resistant auxiliary agent.
7. The normal-temperature curing water-based epoxy resin coating as claimed in claim 6, wherein: the dosage of the 1-phenylpyrrole, the concentrated sulfuric acid and the sodium sulfate in the step B1 is 1: 1.2: 1.2, the dosage ratio of the intermediate E1, the sodium hydroxide solution and the hydrochloric acid solution in the step B2 is 10 g: 5mL of: 8mL, 30-35% of sodium hydroxide solution by mass, 60-65% of hydrochloric acid solution by mass, and the volume ratio of the potassium dichromate aqueous solution to the concentrated sulfuric acid in the step B3 is 1: 1.7, the mass fraction of the potassium dichromate aqueous solution is 45-50%, and the dosage ratio of the intermediate E2 to the mixed solution is 1 g: 40mL, the using amount ratio of the intermediate E3, the aluminum chloride powder and the phosphorus oxychloride in the step B4 is 6g to 1.2g to 1mL, and the mass fractions of the concentrated sulfuric acid in the step B1 and the step B3 are 98%.
8. The preparation method of the normal-temperature curing water-based epoxy resin coating as claimed in claim 1, wherein the preparation method comprises the following steps: the preparation method specifically comprises the preparation of a coating base liquid and the preparation of a modified curing agent;
the preparation steps of the coating base liquid are as follows:
step S1: adding zinc stearate, talcum powder and kaolin powder into a crusher, crushing, sieving by a 300-mesh sieve with 500 meshes, and mixing to obtain mixed powder;
step S2: adding dimethylacetamide and a heat-resistant auxiliary agent into a reaction kettle, stirring at the temperature of 30-50 ℃ until the dimethylacetamide and the heat-resistant auxiliary agent are uniformly mixed, adding an aqueous epoxy resin emulsion, and stirring at the temperature of 60-80 ℃ for 20-30min to prepare a premixed solution;
step S3: and (4) adding the premixed liquid prepared in the step S2 and the mixed powder prepared in the step S1 into a stirring kettle, stirring for 20-30min under the condition that the rotating speed is 1200-1500r/min, adding the emulsifier and the defoaming agent, and continuously stirring for 1-1.5h to prepare the coating base liquid.
The preparation steps of the modified curing agent are as follows:
step A1: adding p-xylene into a reaction kettle, stirring and adding a first mixed acid under the condition that the rotation speed is 300-500r/min, reacting for 30-40min at the temperature of 40-50 ℃, adding a second mixed acid, and reacting for 1-1.5h at the temperature of 60-70 ℃ to obtain an intermediate F1;
step A2: adding the intermediate F1 and ethanol obtained in the step A1 into a reaction kettle, stirring until the intermediate F1 is completely dissolved, adding palladium chloride, reacting for 3-4h under the conditions that the pressure is 7-8MPa and the temperature is 175-185 ℃, adding n-pentadecane and zinc oxide, introducing nitrogen for protection, and reacting under the conditions that the pressure is 0.8-1.5MPa and the temperature is 250-300 ℃ to obtain an intermediate F2;
step A3: adding the intermediate F2 prepared in the step A2 and ferric chloride into a reaction kettle, introducing chlorine to fill the reaction kettle, reacting for 30-40min to prepare an intermediate F3, adding the intermediate F3 and hydrocyanic acid into a fluidized bed reactor, and passing through NiO-Al at the temperature of 550-600 DEG C2O3Catalyst, reacting to obtain intermediate F4;
step A4: and B, adding the intermediate F4 prepared in the step A3 and m-xylene into a reaction kettle, stirring until the intermediate F4 is completely mixed, adding cobalt oxide and palladium oxide, and reacting for 4-5h under the conditions that the pressure is 15-20MPa and the temperature is 120-150 ℃ to prepare the modified curing agent.
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Application publication date: 20200922 |
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