CN106939138B - A kind of preparation method of antistripping oligomer waterborne epoxy coatings - Google Patents
A kind of preparation method of antistripping oligomer waterborne epoxy coatings Download PDFInfo
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- CN106939138B CN106939138B CN201710265650.2A CN201710265650A CN106939138B CN 106939138 B CN106939138 B CN 106939138B CN 201710265650 A CN201710265650 A CN 201710265650A CN 106939138 B CN106939138 B CN 106939138B
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- 229920006334 epoxy coating Polymers 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000003822 epoxy resin Substances 0.000 claims abstract description 28
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 28
- 239000006185 dispersion Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims description 26
- 239000004593 Epoxy Substances 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 16
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 16
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 16
- 239000005642 Oleic acid Substances 0.000 claims description 16
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 16
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 16
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 16
- 150000001408 amides Chemical class 0.000 claims description 15
- -1 amino ester Chemical class 0.000 claims description 15
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 14
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- 230000009435 amidation Effects 0.000 claims description 11
- 238000007112 amidation reaction Methods 0.000 claims description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 230000032050 esterification Effects 0.000 claims description 10
- 238000005886 esterification reaction Methods 0.000 claims description 10
- 239000004166 Lanolin Substances 0.000 claims description 9
- 238000004945 emulsification Methods 0.000 claims description 9
- 229940039717 lanolin Drugs 0.000 claims description 9
- 235000019388 lanolin Nutrition 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 230000003197 catalytic effect Effects 0.000 claims description 8
- 239000000084 colloidal system Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 229960004756 ethanol Drugs 0.000 claims description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 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
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 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 4
- 238000007605 air drying Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 4
- 238000000034 method Methods 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
- 229910052757 nitrogen Inorganic materials 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
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical group OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- 239000003973 paint Substances 0.000 abstract description 12
- 239000000853 adhesive Substances 0.000 abstract description 8
- 230000001070 adhesive effect Effects 0.000 abstract description 8
- 239000000758 substrate Substances 0.000 abstract description 7
- 238000005054 agglomeration Methods 0.000 abstract description 6
- 230000002776 aggregation Effects 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000008021 deposition Effects 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract description 3
- 239000007864 aqueous solution Substances 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 19
- 238000000576 coating method Methods 0.000 description 17
- 239000011248 coating agent Substances 0.000 description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 description 8
- 235000019441 ethanol Nutrition 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 5
- 238000004132 cross linking Methods 0.000 description 5
- 229910015900 BF3 Inorganic materials 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 239000011256 inorganic filler Substances 0.000 description 3
- 229910003475 inorganic filler Inorganic materials 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010422 painting Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BLALBRWEAJQIIL-UHFFFAOYSA-N [Cl].CC(O)=O Chemical compound [Cl].CC(O)=O BLALBRWEAJQIIL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 235000012216 bentonite Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000009500 colour coating Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- VEUUMBGHMNQHGO-UHFFFAOYSA-N ethyl chloroacetate Chemical compound CCOC(=O)CCl VEUUMBGHMNQHGO-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000003137 locomotive effect Effects 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
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002633 protecting effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000008279 sol Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 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
- 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
- C08G59/14—Polycondensates modified by chemical after-treatment
- C08G59/1433—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
- C08G59/1438—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
- C08G59/1455—Monocarboxylic acids, anhydrides, halides, or low-molecular-weight esters thereof
- C08G59/1461—Unsaturated monoacids
- C08G59/1472—Fatty acids
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
-
- 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
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Paints Or Removers (AREA)
- Epoxy Resins (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of preparation methods of antistripping oligomer waterborne epoxy coatings, antistripping oligomer waterborne epoxy coatings of the invention has better adhesive force compared to traditional aqueous epoxide resin paint, peel strength is high, water-fast, sour, alkali, salt, gasoline strong, pencil hardness height, tensile strength are high, each raw material good dispersion in aqueous solution, without agglomeration without deposition, no particle good coated in substrate surface planarization.
Description
Technical field
The invention belongs to paint fields, and in particular to a kind of preparation method of antistripping oligomer waterborne epoxy coatings.
Background technique
Epoxy resin have excellent chemical corrosion resistance, to numerous grounds have splendid adhesive force, can with it is a variety of solid
Agent solidification, the compactness of film is good, rigidity is strong, heat-resistant antifriction is all fine, in occupation of critical role in anticorrosive paint, leads to
It crosses and adds different filler and adjustment curing agent kind, the anti-corrosive paint of epoxy resin of different properties can be made, be suitable for not
Same anti-corrosion occasion, reaches good protecting effect.It is applied to manufacture epoxy there are about 40% epoxy resin in the world every year to apply
Material, major applications are in corrosion-resistant field.In China, about 30% ~ 40% epoxy resin is processed to various paintings
Material, has extensive purposes in fields such as ship, civil engineering, household electrical appliance, mechanotronics.
Epoxy resin is for the painting that is maximum, but industrially using at present with liquid resin portion in anticorrosive coating
Material is largely solvent based coating, and conventional solution-type coating is mostly using aromatic hydrocarbons, esters, alcohols, ketone etc. as solvent, these solvents
Different degrees of toxicity is all had, and volatile matter is directly discharged into air, environmental pollution is heavier.With people's environmental consciousness
Enhancing, such as powdery paints, solventless coatings and water paint etc. of the novel anticorrosion coating without organic solvent or low VOC are green
Color coating is developed in succession.Powdery paints is because condition of cure is more harsh, to limit its development；Solventless epoxy coating
That comparison is successful in solvent free paint field, only in recent years the safety of the hypotoxicity of reactive diluent and curing agent can
Among being challenged, improving by property etc.；And plurality of advantages of the waterborne epoxy coatings in addition to adhering to solvent based coating
Outside, to improve performance, reduce pollution, expand application etc. development, field oneself cover locomotive, aviation, food, building
Deng, 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
Peel strength be just able to satisfy to the protection of the persistence of substrate, therefore, it is an object of the invention to provide a kind of more high adhesion force,
Finished product good dispersion, non-caking aqueous epoxide resin paint.
Summary of the invention
It is an object of the invention to further increase the peel strength of traditional aqueous epoxy resins, solve inorganic filler with
Dispersed poor problem between epoxy resin, provides a kind of preparation method of antistripping oligomer waterborne epoxy coatings.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of antistripping oligomer waterborne epoxy coatings, comprising the following steps:
(1) lanolin for taking 2-3 parts by weight is added in the dehydrated alcohol of 57-60 times of its weight, is protected at 80-85 DEG C
Temperature stirring 4-10 minutes；
(2) ethyl orthosilicate for taking 27-32 parts by weight is added in the deionized water of 30-40 times of its weight, stirs 1-2
Hour, it is mixed with the ethanol solution of above-mentioned lanolin, is stirred to react 40-50 minutes, is mixed with the monoxone of 10-13 parts by weight,
It 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 1-3 parts by weight is mixed with above-mentioned esterification sol dispersion, increases temperature
Degree 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 0.3-0.5 parts by weight, the tetrahydrofuran mixing of 30-36 parts by weight, stirring are taken
Uniformly, catalytic mixing solution is obtained；
(5) above-mentioned amino ester colloidal sol is taken, mixes, stirs evenly with 10-12 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 1-2 parts by weight, the epoxy resin E44 mixing of 24-30 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, 0.1-0.2 parts by weight are added
Boron trifluoride ether, be stirred to react 3-4 hours, discharge, reduce temperature be 35-40 DEG C, be added 4-5 parts by weight oleic acid, protect
Temperature stirring 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, epoxy resin E44,3-4 weight with 140-150 parts by weight
The methyl diphenylene diisocyanate mixing for measuring part, increasing temperature is 60-70 DEG C, and insulated and stirred 110-130 minutes, mixing is added
Expect the deionized water of weight 65-80%, the ricinoleic acid of 0.6-1%, 0.4-1% sorbester p17, stir evenly, using colloid mill
Grinding, homogenizer emulsification are to get the antistripping oligomer 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 antistripping oligomer waterborne epoxy coatings are as follows: before use, antistripping oligomer is aqueous
Epoxy coating is mixed with the curing agent of its weight 20-25%, is stirred evenly, and can be coated.
The curing agent is methylhexahydrophthalic anhydride.
Advantages of the present invention:
The present invention uses ethyl orthosilicate for presoma first, the ethanol solution mixed hydrolysis with lanolin, later and chlorine
Acetic acid mixing obtains esterification sol dispersion, is then led to so that monoxone and ethyl alcohol are esterified in hydrolytic sol liquid
Gamma-aminopropyl-triethoxy-silane processing is crossed, amino ester colloidal sol is obtained, then using amide oligomers colloidal sol, formaldehyde as raw material,
Hexadecyldimethyl benzyl ammonium tertiary amine is catalyst, and tetrahydrofuran is solvent, by dehydrating condensation, obtains amide oligomers colloidal sol；
Then by epoxy resin E44, polyethylene glycol blending, using boron trifluoride ether as catalyst preparation epoxy resin pre-polymerization
Then object is handled using oleic acid, obtains carboxylated epoxy resin；
Amide oligomers colloidal sol, oleic acid modified epoxy prepolymer are mixed into crosslinking later, obtain amidation oligomer ring
Oxygen resin sol finally carries out amidation oligomer epoxy sol and epoxy resin, auxiliary agent etc. to mix dispersion, obtains this
The antistripping oligomer waterborne epoxy coatings of invention；
The present invention is by the hydrolysis of ethyl orthosilicate progress synchronous with the esterification of monoxone, ethyl alcohol, so that is formed is molten
Glue is effectively combined with esterified material, and not only sol surface organises, but also improves the intensity and mechanical property of esterified material, from
And the mechanical property on the surface of finished product film can be improved；
The present invention uses ethyl chloroacetate colloidal sol, formaldehyde for raw material, and hexadecyldimethyl benzyl ammonium tertiary amine is catalyst, tetrahydro furan
It mutters and obtains amide oligomers colloidal sol by addition condensation for solvent, with very high adhesion strength, can effectively improve
Caking property between coating and substrate improves the adhesive force and peel strength of film, protective value of the enhancing film to substrate；
Amide oligomers colloidal sol, oleic acid modified epoxy prepolymer are mixed crosslinking, amide oligomers colloidal sol by the present invention
For alkaline sol, oleic acid modified epoxy prepolymer is acidic prepolymer, and the two could be formed with the crosslinking of effect, generates amide
Change cross-linking products, and cross-linking products can be very good to realize water solubility after amidation, so that each raw material in aqueous solution can
Enough dispersions well, so that finished product uniformity is good, no agglomeration, the flat and smooth no particle of coating.
Specific embodiment
Embodiment 1
A kind of preparation method of antistripping oligomer waterborne epoxy coatings, comprising the following steps:
(1) lanolin for taking 2 parts by weight is added in the dehydrated alcohol of 57 times of its weight, and insulated and stirred 4 is divided at 80 DEG C
Clock；
(2) ethyl orthosilicate for taking 27 parts by weight is added in the deionized water of 30 times of its weight, is stirred 1 hour, and upper
The ethanol solution mixing for stating lanolin, is stirred to react 40 minutes, mixes, be sent in reaction kettle with the monoxone of 10 parts by weight,
Insulation reaction 1 hour of 110 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 60 DEG C, precipitating is washed in ultrasound 30 minutes, filtering, and air drying obtains amino ester colloidal sol；
(4) the hexadecyldimethyl benzyl ammonium tertiary amine of 0.3 parts by weight, the tetrahydrofuran mixing of 30 parts by weight are taken, stirs evenly, obtains
Catalytic mixing solution；
(5) take above-mentioned amino ester colloidal sol, with 10 parts by weight, 30% formalin mix, stir evenly, in addition
Catalytic mixing solution is stated, insulated and stirred 36 minutes at 70 DEG C obtain amide oligomers colloidal sol；
(6) polyethylene glycol of 1 parts by weight, the epoxy resin E44 mixing of 24 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 second of 0.1 parts by weight is added
Ether is stirred to react 3 hours, discharging, and reducing temperature is 35 DEG C, and the oleic acid of 4 parts by weight is added, insulated and stirred 1 hour, obtains oleic acid and changes
Property 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 epoxy resin E44 of 140 parts by weight, 3 parts by weight
Methyl diphenylene diisocyanate mixing, increasing temperature is 60 DEG C, and insulated and stirred 110 minutes, going for mixture weight 65% is added
Ionized water, 0.6% ricinoleic acid, 0.4% sorbester p17, stir evenly, and emulsify using colloid mill grinding, homogenizer, colloid
The milling time of mill is 30 minutes, and the pressure of homogenizer emulsification is 40MPa, emulsification times are 20 minutes to get the antistripping
Oligomer waterborne epoxy coatings.
The application method of the antistripping oligomer waterborne epoxy coatings are as follows: before use, antistripping oligomer is aqueous
Epoxy coating is mixed with the methylhexahydrophthalic anhydride of its weight 25%, is stirred evenly, and can be coated.
The performance test of 1 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 and blisters: 14.3；
3% sodium chloride solution/d impregnates edge and blisters: 21；
10% sodium hydroxide solution/d impregnates edge and blisters: 17.5；
10% hydrochloric acid solution/d impregnates edge and blisters: 5；
Gasoline/d impregnates edge and blisters: 6；
Pencil hardness: 4H；
Tensile strength/PMa:110；
Embodiment 2
A kind of preparation method of antistripping oligomer waterborne epoxy coatings, comprising the following steps:
(1) lanolin for taking 3 parts by weight is added in the dehydrated alcohol of 60 times of its weight, the insulated and stirred 10 at 85 DEG C
Minute；
(2) ethyl orthosilicate for taking 32 parts by weight is added in the deionized water of 40 times of its weight, is stirred 2 hours, and upper
The ethanol solution mixing for stating lanolin, is stirred to react 40 minutes, mixes, be sent in reaction kettle with the monoxone of 13 parts by weight,
Insulation reaction 2 hours of 120 DEG C, discharging cooling obtained esterification sol dispersion；
(3) gamma-aminopropyl-triethoxy-silane for taking 3 parts by weight is mixed with above-mentioned esterification sol dispersion, increases temperature
It is 65 DEG C, precipitating is washed in ultrasound 40 minutes, filtering, and air drying obtains amino ester colloidal sol；
(4) the hexadecyldimethyl benzyl ammonium tertiary amine of 0.5 parts by weight, the tetrahydrofuran mixing of 36 parts by weight are taken, stirs evenly, obtains
Catalytic mixing solution；
(5) take above-mentioned amino ester colloidal sol, with 12 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 2 parts by weight, the epoxy resin E44 mixing of 30 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 second of 0.2 parts by weight is added
Ether is stirred to react 4 hours, discharging, and reducing temperature is 40 DEG C, and the oleic acid of 5 parts by weight is added, insulated and stirred 2 hours, obtains oleic acid and changes
Property 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 epoxy resin E44 of 150 parts by weight, 4 parts by weight
Methyl diphenylene diisocyanate mixing, increasing temperature is 70 DEG C, and insulated and stirred 130 minutes, going for mixture weight 80% is added
Ionized water, 1% ricinoleic acid, 1% sorbester p17, stir evenly, and emulsify using colloid mill grinding, homogenizer, colloid mill
Milling time is 30 minutes, and the pressure of homogenizer emulsification is 60MPa, emulsification times are 30 minutes up to the antistripping oligomer
Waterborne epoxy coatings.
Before use, by the methylhexahydrophthalic anhydride of antistripping oligomer waterborne epoxy coatings and its weight 25%
Mixing, stirs evenly, can be coated.
The performance test of 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 and blisters: 14；
3% sodium chloride solution/d impregnates edge and blisters: 20.5；
10% sodium hydroxide solution/d impregnates edge and blisters: 18；
10% hydrochloric acid solution/d impregnates edge and blisters: 5；
Gasoline/d impregnates edge and blisters: 6.5；
Pencil hardness: 4H；2
Tensile strength/PMa:108.5；
The performance test of traditional aqueous epoxide resin paint:
Adhesive force: 2 grades；
Film corrosion resistance:
Distilled water/d impregnates edge and blisters: 4；
3% sodium chloride solution/d impregnates edge and blisters: 6；
10% sodium hydroxide solution/d impregnates edge and blisters: 5；
10% hydrochloric acid solution/d impregnates edge and blisters: 2；
Gasoline/d impregnates edge and blisters: 2.5；
Pencil hardness: 2H；
Tensile strength/PMa:77.
It can thus be seen that antistripping oligomer waterborne epoxy coatings of the invention is applied compared to traditional aqueous epoxy resins
Material has better adhesive force, and peel strength is high, and water-fast, sour, alkali, salt, gasoline pencil hardness is high by force, and tensile strength is high,
Each raw material good dispersion in aqueous solution, no agglomeration is without deposition, and it is good to be coated in substrate surface planarization, no particle.
Claims (3)
1. a kind of preparation method of antistripping oligomer waterborne epoxy coatings, which comprises the following steps:
(1) lanolin for taking 2-3 parts by weight is added in the dehydrated alcohol of 57-60 times of its weight, is kept the temperature and is stirred at 80-85 DEG C
It mixes 4-10 minutes；
(2) ethyl orthosilicate for taking 27-32 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 ethanol solution of above-mentioned lanolin, is stirred to react 40-50 minutes, mixes, be sent to the monoxone of 10-13 parts by weight
In reaction kettle, insulation reaction 1-2 hours at 110-120 DEG C, discharging cooling obtains esterification sol dispersion；
(3) gamma-aminopropyl-triethoxy-silane for taking 1-3 parts by weight is mixed with above-mentioned esterification sol dispersion, is increased temperature and is
60-65 DEG C, 30-40 minutes ultrasonic, precipitating is washed in filtering, and air drying obtains amino ester colloidal sol；
(4) the hexadecyldimethyl benzyl ammonium tertiary amine of 0.3-0.5 parts by weight, the tetrahydrofuran mixing of 30-36 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 10-12 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 1-2 parts by weight, the epoxy resin E44 mixing of 24-30 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 three of 0.1-0.2 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 4-5 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 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, epoxy resin E44,3-4 parts by weight with 140-150 parts by weight
Methyl diphenylene diisocyanate mixing, increase temperature be 60-70 DEG C, insulated and stirred 110-130 minute, addition mixture weight
Measure the deionized water of 65-80%, the ricinoleic acid of 0.6-1%, 0.4-1% sorbester p17, stir evenly, using colloid mill grinding,
Homogenizer emulsifies to get the antistripping oligomer waterborne epoxy coatings；The milling time of colloid mill is 30-40 minutes, homogeneous
The pressure of machine emulsification is 40-60MPa, emulsification times are 20-30 minutes.
2. a kind of preparation method of antistripping oligomer waterborne epoxy coatings according to claim 1, which is characterized in that institute
State the application method of antistripping oligomer waterborne epoxy coatings are as follows: before use, by antistripping oligomer waterborne epoxy coatings with
The curing agent of its weight 20-25% mixes, and stirs evenly, can be coated.
3. a kind of preparation method of antistripping oligomer waterborne epoxy coatings according to claim 2, which is characterized in that institute
The curing agent stated is methylhexahydrophthalic anhydride.
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