CN107033740B - A kind of preparation method of antibacterial anticorrosion waterborne epoxy coatings - Google Patents
A kind of preparation method of antibacterial anticorrosion waterborne epoxy coatings Download PDFInfo
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- CN107033740B CN107033740B CN201710386727.1A CN201710386727A CN107033740B CN 107033740 B CN107033740 B CN 107033740B CN 201710386727 A CN201710386727 A CN 201710386727A CN 107033740 B CN107033740 B CN 107033740B
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 45
- 229920006334 epoxy coating Polymers 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 230000032050 esterification Effects 0.000 claims abstract description 27
- 238000005886 esterification reaction Methods 0.000 claims abstract description 27
- 239000004593 Epoxy Substances 0.000 claims abstract description 22
- 230000009435 amidation Effects 0.000 claims abstract description 11
- 238000007112 amidation reaction Methods 0.000 claims abstract description 11
- 239000004166 Lanolin Substances 0.000 claims abstract description 10
- 229940039717 lanolin Drugs 0.000 claims abstract description 10
- 235000019388 lanolin Nutrition 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 23
- 229920000647 polyepoxide Polymers 0.000 claims description 21
- 239000003822 epoxy resin Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 15
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 14
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 14
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 14
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000005642 Oleic acid Substances 0.000 claims description 14
- -1 amino ester Chemical class 0.000 claims description 14
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 14
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 11
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 10
- 150000001408 amides Chemical class 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 10
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- 239000000084 colloidal system Substances 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 8
- 238000004945 emulsification Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 claims description 6
- 230000003197 catalytic effect Effects 0.000 claims description 6
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 5
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 5
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 5
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- NWGKJDSIEKMTRX-MDZDMXLPSA-N Sorbitan oleate Chemical compound CCCCCCCC\C=C\CCCCCCCC(=O)OCC(O)C1OCC(O)C1O NWGKJDSIEKMTRX-MDZDMXLPSA-N 0.000 claims description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 claims description 5
- GRHBQAYDJPGGLF-UHFFFAOYSA-N isothiocyanic acid Chemical compound N=C=S GRHBQAYDJPGGLF-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 229920002866 paraformaldehyde Polymers 0.000 claims description 5
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 5
- 229940068041 phytic acid Drugs 0.000 claims description 5
- 235000002949 phytic acid Nutrition 0.000 claims description 5
- 239000000467 phytic acid Substances 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 239000004677 Nylon Substances 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 4
- 150000004702 methyl esters Chemical class 0.000 claims description 4
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 4
- 229920001778 nylon Polymers 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 4
- WBHHMMIMDMUBKC-XLNAKTSKSA-N ricinelaidic acid Chemical compound CCCCCC[C@@H](O)C\C=C\CCCCCCCC(O)=O WBHHMMIMDMUBKC-XLNAKTSKSA-N 0.000 claims description 4
- 229960003656 ricinoleic acid Drugs 0.000 claims description 4
- FEUQNCSVHBHROZ-UHFFFAOYSA-N ricinoleic acid Natural products CCCCCCC(O[Si](C)(C)C)CC=CCCCCCCCC(=O)OC FEUQNCSVHBHROZ-UHFFFAOYSA-N 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- 229910015900 BF3 Inorganic materials 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims 1
- 238000000576 coating method Methods 0.000 abstract description 24
- 239000011248 coating agent Substances 0.000 abstract description 23
- 239000000758 substrate Substances 0.000 abstract description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000002421 anti-septic effect Effects 0.000 abstract description 3
- 238000004176 ammonification Methods 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 239000004408 titanium dioxide Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 23
- 239000003973 paint Substances 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 230000003115 biocidal effect Effects 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- 238000011056 performance test Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000003026 anti-oxygenic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000011256 inorganic filler Substances 0.000 description 2
- 229910003475 inorganic filler Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 241000228197 Aspergillus flavus Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241001515917 Chaetomium globosum Species 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 235000012216 bentonite Nutrition 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical group OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000003137 locomotive effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 239000002504 physiological saline solution Substances 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000002604 ultrasonography Methods 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
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
-
- 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
-
- 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
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Plant Pathology (AREA)
- Paints Or Removers (AREA)
- Epoxy Resins (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention discloses a kind of preparation methods of antibacterial anticorrosion waterborne epoxy coatings, colloidal sol is passed through esterification by the present invention, ammonification, amidation processing, effectively improve the dispersibility of colloidal sol in the epoxy, improve the compatibility of titanium dioxide Yu each raw material, effectively reduce reunion, enhance the uniform and stable property of coating, surface strength and bacteriostasis property, colloidal sol esterification is improved to the lubricity and dispersibility of coating, the lanolin etc. that coating of the invention is added can effectively improve the antiseptic property of film, viscosity of the coating of the invention is high, it is strong with the caking property of substrate, antibacterial intensity is high.
Description
Technical field
The invention belongs to paint fields, and in particular to a kind of preparation method of antibacterial anticorrosion waterborne epoxy coatings.
Background technique
Epoxy resin is for maximum with liquid resin portion in anticorrosive coating, but the current coating industrially used
Major part is solvent based coating, and for conventional solution-type coating mostly using aromatic hydrocarbons, esters, alcohols, ketone etc. as solvent, these solvents are equal
With different degrees of toxicity, and volatile matter is directly discharged into air, and environmental pollution is heavier.With the increasing of people's environmental consciousness
By force, the novel anticorrosion coating such as powdery paints, solventless coatings and water paint etc. without organic solvent or low VOC is green
Coating is developed in succession.Powdery paints is because condition of cure is more harsh, to limit its development；Solventless epoxy coating exists
Solvent free paint field is that comparison is successful, only in recent years in the safe and reliable of the hypotoxicity of reactive diluent and curing agent
Property etc. is challenged, improving among；And waterborne epoxy coatings is other than the plurality of advantages for adhering to solvent based coating,
To improving performance, reducing pollution, expansion application etc. development, oneself covers locomotive, aviation, food, building etc. in field,
Therefore waterborne epoxy coatings is to develop a very rapid field in recent years；
For epoxy resin cured product because brittleness is big, impact resistance, resistance to acid and alkali, flexibility and temperature tolerance are poor, limit epoxy
The application of cold coating, therefore be always one of the emphasis studied anti-corrosive paint of epoxy resin to the modification of epoxy resin, and
In order to improve its mechanical property, it is often added the inorganic fillers such as various bentonites, graphene wherein, but these inorganic fillers
It is poor with the compatibility of epoxy resin, it be easy to cause the storage stability of coating poor, and agglomeration easy to form, reduces coating
Quality, and the adhesive force grade of traditional aqueous epoxide resin paint and substrate is 2 grades, although can satisfy actual production life
In requirement to film, but for some needs often poor substrates of wiping, profile pattern, it is desired nonetheless to stronger
Just peel strength be able to satisfy to the protection of the persistence of substrate, meanwhile, in order to improving to environment is adaptability, antibacterial antiseptic property
It is also an important indicator for judging finished product coating comprehensive performance, this point is often neglected by people in traditional aqueous epoxide resin paint
Depending on, therefore, it is an object of the invention to provide a kind of more high adhesion force, finished product good dispersion, do not agglomerate, biocidal property is strong, storage
The good aqueous epoxide resin paint of stability.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of antibacterial anticorrosion water-base epoxies to apply
The preparation method of material.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of antibacterial anticorrosion waterborne epoxy coatings, comprising the following steps:
(1) lanolin for taking 3-4 parts by weight is added in the isopropanol of 57-60 times of its weight, is kept the temperature at 80-85 DEG C
Stirring 4-10 minutes；
(2) ethyl orthosilicate for taking 10-17 parts by weight is added in the deionized water of 30-40 times of its weight, stirs 1-2
Hour, it mixes, is stirred to react 40-50 minutes with the aqueous isopropanol of above-mentioned lanolin, the palm acid-mixed with 10-13 parts by weight
It closes, is sent in reaction kettle, insulation reaction 1-2 hours of 110-120 DEG C, discharging cooling obtained esterification sol dispersion；
(3) gamma-aminopropyl-triethoxy-silane for taking 0.7-1 parts by weight is mixed with above-mentioned esterification sol dispersion, is increased
Temperature is 60-65 DEG C, 30-40 minutes ultrasonic, and precipitating is washed in filtering, and air drying obtains amino ester colloidal sol；
(4) the hexadecyldimethyl benzyl ammonium tertiary amine of 1-2 parts by weight, the tetrahydrofuran mixing of 16-20 parts by weight are taken, stirring is equal
It is even, obtain catalytic mixing solution；
(5) above-mentioned amino ester colloidal sol is taken, mixes, stirs evenly with 10-14 parts by weight, 30-35% formalin,
Above-mentioned catalytic mixing solution is added, insulated and stirred 36-50 minutes at 70-75 DEG C, obtains amide oligomers colloidal sol；
(6) polyethylene glycol of 2-4 parts by weight, the epoxy resin E44 mixing of 35-40 parts by weight are taken, stirs evenly, is sent to
In reaction kettle, adjusting temperature of reaction kettle is 56-70 DEG C, insulated and stirred 10-20 minutes, is passed through nitrogen, the three of 1-2 parts by weight are added
It is fluorinated borate ether, is stirred to react 3-4 hours, is discharged, reducing temperature is 35-40 DEG C, and the oleic acid of 3-4 parts by weight is added, and heat preservation is stirred
It mixes 1-2 hours, obtains oleic acid modified epoxy prepolymer；
(7) above-mentioned amide oligomers colloidal sol, oleic acid modified epoxy prepolymer are mixed, is added to mixture weight 4-
In 6 times of deionized water, insulated and stirred 4-6 hours at 70-75 DEG C, amidation oligomer epoxy sol is obtained；
(8) above-mentioned amidation oligomer epoxy sol is taken, antibacterial esterification solution, 100-120 weight with 3-5 parts by weight
Measure the methyl diphenylene diisocyanate mixing of epoxy resin E44,2-3 parts by weight of part, the insulated and stirred 110- at 60-70 DEG C
130 minutes, be added the deionized water of mixture weight 65-80%, the ricinoleic acid of 0.6-1%, 0.4-0.7% sorbester p17, stirring
Uniformly, using colloid mill grinding, homogenizer emulsification to get the antibacterial anticorrosion waterborne epoxy coatings.
In the step (8), the milling time of colloid mill is 30-40 minutes, and the pressure of homogenizer emulsification is 40-
60MPa, emulsification times are 20-30 minutes.
The application method of the antibacterial anticorrosion waterborne epoxy coatings are as follows:
Before use, antibacterial anticorrosion waterborne epoxy coatings is mixed with the curing agent of its weight 20-25%, stir evenly,
It can be coated.
The curing agent is methylhexahydrophthalic anhydride.
The preparation method of the antibacterial esterification solution the following steps are included:
Take the isothiocyanic acid of the phosphorus oxychloride of 10-13 parts by weight, the phytic acid of 7-9 parts by weight, 4-6 parts by weight mixed
It closes, is added in the deionized water of 15-20 times of mixture weight, stirs evenly, the pentaerythrite of 30-40 parts by weight is added, send
Enter into reaction kettle, insulation reaction 1-2 hours at 90-100 DEG C, the nylon acid methyl esters of 80-100 parts by weight is added, is passed through nitrogen
Gas, reduction temperature are room temperature, and the paraformaldehyde of 2-3 parts by weight is added, stirs evenly, and the triethylamine of 0.5-1 parts by weight, drop is added dropwise
It is 90-95 DEG C that temperature of reaction kettle is adjusted after adding, and is stirred to react 100-110 minutes, discharges, is cooled to room temperature to get described
Antibacterial esterification solution.
Advantages of the present invention:
The present invention hydrolyzes in deionized water using ethyl orthosilicate as presoma, and the isopropanol that lanolin is then added is molten
Liquid mixes esterification with palmitinic acid, obtains esterification sol dispersion, which has dispersibility, lubricity well,
Then using gamma-aminopropyl-triethoxy-silane processing esterification colloidal sol, amino ester colloidal sol is obtained, it is then mixed with formalin
It closes, uses hexadecyldimethyl benzyl ammonium tertiary amine for catalyst, obtain amide oligomers colloidal sol, then with epoxy resin, polyethylene glycol
It for raw material, is handled using oleic acid, obtains oil acidification epoxy prepolymer；Then it is mixed with amide oligomers colloidal sol,
By reacting for oleic acid and amino, amidation oligomer epoxy sol is obtained, is then dispersed by sorbester p17, is obtained antibacterial
Anticorrosion waterborne epoxy coatings；
In antibacterial esterification solution of the invention, using isothiocyanic acid, phosphorus oxychloride, phytic acid as raw material, by water
Then obtained esterified material is condensed by Xie Houyu mixed esters of pentaerythritol with paraformaldehyde, then be catalyzed by triethylamine
It is modified, organic phosphorus vulcanization ester solution is obtained, the organic phosphorus vulcanization ester solution not only biocidal property with higher also has well
Antioxygenic property can be improved finished polycarbonate material biocidal property, antioxygenic property, improve the comprehensive performance of finished product coating；
The present invention handles colloidal sol by esterification, ammonification, amidation, effectively improves point of colloidal sol in the epoxy
Dissipate property, improve the compatibility of titanium dioxide Yu each raw material, effectively reduce reunion, enhance coating uniform and stable property,
Colloidal sol esterification is improved the lubricity and dispersibility of coating, the sheep that coating of the invention is added by surface strength and bacteriostasis property
Hair rouge etc. can effectively improve the antiseptic property of film, and viscosity of the coating of the invention is high, strong with the caking property of substrate, antibacterial strong
Degree is high.
Specific embodiment
Embodiment 1
A kind of preparation method of antibacterial anticorrosion waterborne epoxy coatings, comprising the following steps:
(1) lanolin for taking 4 parts by weight is added in the isopropanol of 60 times of its weight, and insulated and stirred 10 is divided at 85 DEG C
Clock；
(2) ethyl orthosilicate for taking 17 parts by weight is added in the deionized water of 40 times of its weight, is stirred 2 hours, and upper
The aqueous isopropanol mixing for stating lanolin, is stirred to react 50 minutes, mixes with the palmitinic acid of 13 parts by weight, be sent to reaction kettle
In, insulation reaction 2 hours of 120 DEG C, discharging cooling obtained esterification sol dispersion；
(3) gamma-aminopropyl-triethoxy-silane for taking 1 parts by weight is mixed with above-mentioned esterification sol dispersion, increases temperature
It is 65 DEG C, precipitating is washed in 30-40 minutes ultrasonic, filtering, and air drying obtains amino ester colloidal sol；
(4) the hexadecyldimethyl benzyl ammonium tertiary amine of 2 parts by weight, the tetrahydrofuran mixing of 20 parts by weight are taken, stirs evenly, must urge
Change mixed solution；
(5) take above-mentioned amino ester colloidal sol, with 14 parts by weight, 35% formalin mix, stir evenly, in addition
Catalytic mixing solution is stated, insulated and stirred 50 minutes at 75 DEG C obtain amide oligomers colloidal sol；
(6) polyethylene glycol of 4 parts by weight, the epoxy resin E44 mixing of 40 parts by weight are taken, stirs evenly, is sent to reaction
In kettle, adjusting temperature of reaction kettle is 70 DEG C, insulated and stirred 20 minutes, is passed through nitrogen, the boron trifluoride ether of 2 parts by weight is added,
It is stirred to react 4 hours, discharges, reducing temperature is 40 DEG C, and the oleic acid of 4 parts by weight is added, insulated and stirred 2 hours, it is modified to obtain oleic acid
Epoxy prepolymer；
(7) above-mentioned amide oligomers colloidal sol, oleic acid modified epoxy prepolymer are mixed, is added to mixture weight 6
In deionized water again, insulated and stirred 6 hours at 75 DEG C obtain amidation oligomer epoxy sol；
(8) above-mentioned amidation oligomer epoxy sol is taken, with the antibacterial esterification solution of 3 parts by weight, 120 parts by weight
The methyl diphenylene diisocyanate mixing of epoxy resin E44,3 parts by weight, insulated and stirred 130 minutes at 70 DEG C are added mixed
Deionized water, 1% ricinoleic acid, 0.7% sorbester p17 for closing material weight 80%, stir evenly, using colloid mill grinding,
Matter machine emulsifies to get the antibacterial anticorrosion waterborne epoxy coatings.
In the step (8), the milling time of colloid mill is 40 minutes, and the pressure of homogenizer emulsification is 60MPa, emulsifies
Time is 30 minutes.
The application method of the antibacterial anticorrosion waterborne epoxy coatings are as follows:
Before use, antibacterial anticorrosion waterborne epoxy coatings is mixed with the curing agent of its weight 25%, stir evenly, i.e.,
It can be coated.
The curing agent is methylhexahydrophthalic anhydride.
The preparation method of the antibacterial esterification solution the following steps are included:
The isothiocyanic acid mixing for taking the phosphorus oxychloride of 10 parts by weight, the phytic acid of 7 parts by weight, 4 parts by weight, is added
It into 15 times of mixture weight of deionized waters, stirs evenly, the pentaerythrite of 30 parts by weight is added, is sent in reaction kettle,
The nylon acid methyl esters of 80 parts by weight is added in insulation reaction 1 hour at 90 DEG C, is passed through nitrogen, and reduction temperature is room temperature, is added 2
The paraformaldehyde of parts by weight, stirs evenly, and the triethylamine of 0.5 parts by weight is added dropwise, and it is 90 that temperature of reaction kettle is adjusted after being added dropwise
DEG C, it is stirred to react 100 minutes, discharges, be cooled to room temperature to get the antibacterial esterification solution.
Embodiment 2
A kind of preparation method of antibacterial anticorrosion waterborne epoxy coatings, comprising the following steps:
(1) lanolin for taking 3 parts by weight is added in the isopropanol of 57 times of its weight, and insulated and stirred 4 is divided at 80 DEG C
Clock；
(2) ethyl orthosilicate for taking 10 parts by weight is added in the deionized water of 30 times of its weight, is stirred 1 hour, and upper
The aqueous isopropanol mixing for stating lanolin, is stirred to react 40 minutes, mixes with the palmitinic acid of 10 parts by weight, be sent to reaction kettle
In, insulation reaction 1 hour of 110 DEG C, discharging cooling obtained esterification sol dispersion；
(3) gamma-aminopropyl-triethoxy-silane for taking 0.7 parts by weight is mixed with above-mentioned esterification sol dispersion, increases temperature
Degree is 60 DEG C, ultrasound 30 minutes, and precipitating is washed in filtering, and air drying obtains amino ester colloidal sol；
(4) the hexadecyldimethyl benzyl ammonium tertiary amine of 1 parts by weight, the tetrahydrofuran mixing of 16 parts by weight are taken, stirs evenly, must urge
Change mixed solution；
(5) above-mentioned amino ester colloidal sol is taken, mixes, stirs evenly, in addition with 10 parts by weight, 30-% formalin
Catalytic mixing solution is stated, insulated and stirred 36 minutes at 70 DEG C obtain amide oligomers colloidal sol；
(6) polyethylene glycol of 2 parts by weight, the epoxy resin E44 mixing of 35 parts by weight are taken, stirs evenly, is sent to reaction
In kettle, adjusting temperature of reaction kettle is 56 DEG C, insulated and stirred 10 minutes, is passed through nitrogen, the boron trifluoride ether of 1 parts by weight is added,
It is stirred to react 3 hours, discharges, reducing temperature is 35 DEG C, and the oleic acid of 3 parts by weight is added, insulated and stirred 1 hour, it is modified to obtain oleic acid
Epoxy prepolymer；
(7) above-mentioned amide oligomers colloidal sol, oleic acid modified epoxy prepolymer are mixed, is added to mixture weight 4
In deionized water again, insulated and stirred 4 hours at 70 DEG C obtain amidation oligomer epoxy sol；
(8) above-mentioned amidation oligomer epoxy sol is taken, with the antibacterial esterification solution of 5 parts by weight, 100 parts by weight
The methyl diphenylene diisocyanate mixing of epoxy resin E44,2 parts by weight, insulated and stirred 110 minutes at 60 DEG C are added mixed
Deionized water, 0.6% ricinoleic acid, 0.4% sorbester p17 for closing material weight 65%, stir evenly, ground using colloid mill,
Homogenizer emulsifies to get the antibacterial anticorrosion waterborne epoxy coatings.
In the step (8), the milling time of colloid mill is 30 minutes, and the pressure of homogenizer emulsification is 40MPa, emulsifies
Time is 20 minutes.
The application method of the antibacterial anticorrosion waterborne epoxy coatings are as follows:
Before use, antibacterial anticorrosion waterborne epoxy coatings is mixed with the curing agent of its weight 20%, stir evenly, i.e.,
It can be coated.
The curing agent is methylhexahydrophthalic anhydride.
The preparation method of the antibacterial esterification solution the following steps are included:
The isothiocyanic acid mixing for taking the phosphorus oxychloride of 13 parts by weight, the phytic acid of 9 parts by weight, 6 parts by weight, is added
It into 20 times of mixture weight of deionized waters, stirs evenly, the pentaerythrite of 40 parts by weight is added, is sent in reaction kettle,
The nylon acid methyl esters of 100 parts by weight is added in insulation reaction 2 hours at 100 DEG C, is passed through nitrogen, and reduction temperature is room temperature, is added
The paraformaldehyde of 3 parts by weight, stirs evenly, and the triethylamine of 1 parts by weight is added dropwise, and it is 95 that temperature of reaction kettle is adjusted after being added dropwise
DEG C, it is stirred to react 110 minutes, discharges, be cooled to room temperature to get the antibacterial esterification solution.
Performance test:
The performance test of 1-2 coating of the embodiment of the present invention:
Coating is without agglomeration without deposition, the flat and smooth no particle of coating；Adhesive force: 1 grade；
Film corrosion resistance: distilled water/d impregnates edge blistering: 14-17；3% sodium chloride solution/d impregnates edge blistering:
10-16；10% sodium hydroxide solution/d impregnates edge blistering: 10-15；10% hydrochloric acid solution/d impregnates edge blistering: 3-5；Gasoline/
D impregnates edge blistering: 6-8；
Pencil hardness: 4H；
Tensile strength/PMa:100-105；
The performance test of traditional aqueous epoxide resin paint: adhesive force: 2 grades；
Film corrosion resistance: distilled water/d impregnates edge blistering: 3-5；3% sodium chloride solution/d impregnates edge blistering: 5-
7；10% sodium hydroxide solution/d impregnates edge blistering: 4-6；10% hydrochloric acid solution/d impregnates edge blistering: 1-2；Gasoline/d impregnates
Edge blistering: 2-3；
Pencil hardness: 2H；
Tensile strength/PMa:70-80.
Bactericidal properties test:
Chaetomium globosum bacterium, Aspergillus flavus are spread evenly across respectively be coated with the embodiment of the present invention 1 antibacterial anticorrosion it is aqueous
Epoxy coating, the antibacterial anticorrosion waterborne epoxy coatings of the embodiment of the present invention 2, traditional aqueous epoxide resin paint glass slide
On, bacterium solution is gently stained with swab stick after 0,10,30,60 hour and is placed in physiological saline, is vibrated, is taken 0.5ml in culture dish, add
Enter culture medium, is cultivated 48 hours in incubator；
As can be seen that antibacterial anticorrosion waterborne epoxy coatings of the invention has compared to traditional aqueous epoxide resin paint
Better adhesive force, peel strength is high, water-fast, sour, alkali, salt, gasoline strong, pencil hardness height, tensile strength height, biocidal property
By force, comprehensive performance is superior.
Claims (4)
1. a kind of preparation method of antibacterial anticorrosion waterborne epoxy coatings, which comprises the following steps:
(1) lanolin for taking 3-4 parts by weight is added in the isopropanol of 57-60 times of its weight, the insulated and stirred at 80-85 DEG C
4-10 minutes；
(2) ethyl orthosilicate for taking 10-17 parts by weight is added in the deionized water of 30-40 times of its weight, is stirred 1-2 hours,
It is mixed with the aqueous isopropanol of above-mentioned lanolin, is stirred to react 40-50 minutes, is mixed with the palmitinic acid of 10-13 parts by weight, be sent into
Into reaction kettle, insulation reaction 1-2 hours of 110-120 DEG C, discharging cooling obtained esterification sol dispersion；
(3) gamma-aminopropyl-triethoxy-silane for taking 0.7-1 parts by weight is mixed with above-mentioned esterification sol dispersion, increases temperature
It is 60-65 DEG C, precipitating is washed in 30-40 minutes ultrasonic, filtering, and air drying obtains amino ester colloidal sol；
(4) the hexadecyldimethyl benzyl ammonium tertiary amine of 1-2 parts by weight, the tetrahydrofuran mixing of 16-20 parts by weight are taken, stirs evenly, obtains
Catalytic mixing solution；
(5) above-mentioned amino ester colloidal sol is taken, mixes, stirs evenly with 10-14 parts by weight, 30-35% formalin, is added
Above-mentioned catalytic mixing solution obtains amide oligomers colloidal sol insulated and stirred 36-50 minutes at 70-75 DEG C；
(6) polyethylene glycol of 2-4 parts by weight, the epoxy resin E44 mixing of 35-40 parts by weight are taken, stirs evenly, is sent to reaction
In kettle, adjusting temperature of reaction kettle is 56-70 DEG C, insulated and stirred 10-20 minutes, is passed through nitrogen, the borontrifluoride of 1-2 parts by weight is added
Borate ether is stirred to react 3-4 hours, discharging, and reducing temperature is 35-40 DEG C, and the oleic acid of 3-4 parts by weight, insulated and stirred 1-2 is added
Hour, obtain oleic acid modified epoxy prepolymer；
(7) above-mentioned amide oligomers colloidal sol, oleic acid modified epoxy prepolymer are mixed, is added to 4-6 times of mixture weight
Deionized water in, insulated and stirred 4-6 hours at 70-75 DEG C, obtain amidation oligomer epoxy sol；
(8) above-mentioned amidation oligomer epoxy sol is taken, with the antibacterial esterification solution of 3-5 parts by weight, 100-120 parts by weight
Epoxy resin E44,2-3 parts by weight methyl diphenylene diisocyanate mixing, the insulated and stirred 110-130 at 60-70 DEG C
Minute, be added the deionized water of mixture weight 65-80%, the ricinoleic acid of 0.6-1%, 0.4-0.7% sorbester p17, stirring is equal
It is even, using colloid mill grinding, homogenizer emulsification to get the antibacterial anticorrosion waterborne epoxy coatings；
The preparation method of the antibacterial esterification solution the following steps are included:
The isothiocyanic acid mixing of the phosphorus oxychloride of 10-13 parts by weight, the phytic acid of 7-9 parts by weight, 4-6 parts by weight is taken,
It is added in the deionized water of 15-20 times of mixture weight, stirs evenly, the pentaerythrite of 30-40 parts by weight is added, is sent to
In reaction kettle, insulation reaction 1-2 hours at 90-100 DEG C, the nylon acid methyl esters of 80-100 parts by weight is added, is passed through nitrogen, drop
Low temperature is room temperature, and the paraformaldehyde of 2-3 parts by weight is added, stirs evenly, and the triethylamine of 0.5-1 parts by weight is added dropwise, drips
It is 90-95 DEG C that temperature of reaction kettle is adjusted after finishing, and is stirred to react 100-110 minutes, discharges, is cooled to room temperature to get described antibacterial
It is esterified solution.
2. a kind of preparation method of antibacterial anticorrosion waterborne epoxy coatings according to claim 1, which is characterized in that described
The step of (8) in, the milling time of colloid mill is 30-40 minute, and the pressure that homogenizer emulsifies is 40-60MPa, emulsification times are
20-30 minutes.
3. a kind of preparation method of antibacterial anticorrosion waterborne epoxy coatings according to claim 1, which is characterized in that described
The application method of antibacterial anticorrosion waterborne epoxy coatings are as follows:
Before use, antibacterial anticorrosion waterborne epoxy coatings is mixed with the curing agent of its weight 20-25%, stir evenly
It is coated.
4. a kind of preparation method of antibacterial anticorrosion waterborne epoxy coatings according to claim 3, which is characterized in that described
Curing agent be methylhexahydrophthalic anhydride.
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