CN115537100A - Epoxy zinc-rich primer containing conductive polyaniline coated hollow glass beads and preparation method thereof - Google Patents
Epoxy zinc-rich primer containing conductive polyaniline coated hollow glass beads and preparation method thereof Download PDFInfo
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- CN115537100A CN115537100A CN202211397586.0A CN202211397586A CN115537100A CN 115537100 A CN115537100 A CN 115537100A CN 202211397586 A CN202211397586 A CN 202211397586A CN 115537100 A CN115537100 A CN 115537100A
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 82
- 239000004593 Epoxy Substances 0.000 title claims abstract description 71
- 239000011521 glass Substances 0.000 title claims abstract description 70
- 239000011701 zinc Substances 0.000 title claims abstract description 49
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 49
- 239000011324 bead Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 46
- 239000003822 epoxy resin Substances 0.000 claims abstract description 32
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 32
- 239000002904 solvent Substances 0.000 claims abstract description 18
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 239000004005 microsphere Substances 0.000 claims description 23
- 238000002791 soaking Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 7
- 239000004952 Polyamide Substances 0.000 claims description 6
- 229920002647 polyamide Polymers 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000004359 castor oil Chemical class 0.000 claims description 5
- 235000019438 castor oil Nutrition 0.000 claims description 5
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Chemical class CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 5
- 239000008096 xylene Substances 0.000 claims description 5
- 239000000440 bentonite Substances 0.000 claims description 4
- 229910000278 bentonite Inorganic materials 0.000 claims description 4
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical class O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 229920005989 resin Polymers 0.000 abstract description 9
- 239000011347 resin Substances 0.000 abstract description 9
- 239000011159 matrix material Substances 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 description 15
- 239000000243 solution Substances 0.000 description 15
- 230000007797 corrosion Effects 0.000 description 14
- 239000003973 paint Substances 0.000 description 11
- 239000002994 raw material Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 229910021389 graphene Inorganic materials 0.000 description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 7
- 239000002184 metal Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 4
- BYMMIQCVDHHYGG-UHFFFAOYSA-N Cl.OP(O)(O)=O Chemical compound Cl.OP(O)(O)=O BYMMIQCVDHHYGG-UHFFFAOYSA-N 0.000 description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- -1 polyethylene Polymers 0.000 description 3
- 230000037452 priming Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- CUVLMZNMSPJDON-UHFFFAOYSA-N 1-(1-butoxypropan-2-yloxy)propan-2-ol Chemical compound CCCCOCC(C)OCC(C)O CUVLMZNMSPJDON-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 2
- 238000004210 cathodic protection Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000005028 tinplate Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- 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
- C09D5/10—Anti-corrosive paints containing metal dust
- C09D5/106—Anti-corrosive paints containing metal dust containing Zn
-
- 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
- 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
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
-
- 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
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0893—Zinc
Abstract
The invention belongs to the field of special coatings, and particularly relates to an epoxy zinc-rich primer containing conductive polyaniline-coated hollow glass beads and a preparation method thereof. The epoxy zinc-rich primer provided by the invention comprises a component A and a component B; the component A comprises the following components in parts by weight: 10-20 parts of epoxy resin, 3-10 parts of conductive polyaniline-coated hollow glass beads, 40-60 parts of zinc powder, 1-2 parts of dispersing agent, 0.5-1 part of flatting agent, 0.5-1 part of anti-settling agent and 10-20 parts of solvent; the component B is an epoxy curing agent, and the mass ratio of the epoxy curing agent to the epoxy resin is 1: (1.5-2.5). The epoxy zinc-rich primer provided by the invention has high utilization rate of zinc powder, the bonding strength between the hollow glass beads in the primer and the resin matrix is high, and the hollow glass beads are not easy to float upwards.
Description
Technical Field
The invention belongs to the field of special coatings, and particularly relates to an epoxy zinc-rich primer containing conductive polyaniline-coated hollow glass beads and a preparation method thereof.
Background
The metal base material is seen everywhere in various industries, the loss caused by metal corrosion is as high as hundreds of millions of yuan each year, and the epoxy zinc-rich primer has excellent protection effect on the metal base material, especially has outstanding anti-corrosion performance.
The anticorrosion effect of the epoxy zinc-rich primer mainly depends on zinc powder playing a role in cathodic protection, but as the zinc powder has high density, after the zinc powder is added into epoxy resin, the zinc powder can be slowly deposited at the bottom after a period of time, so that the zinc powder is unevenly dispersed in the resin, and after the epoxy zinc-rich primer is coated, formed into a film and cured, nearly half of the zinc powder cannot play a role in cathodic protection, so that the great waste of the zinc powder is caused. In addition, the traditional epoxy zinc-rich primer still has microcracks after being used for a period of time, so that chloride ions in air or seawater enter a paint film through the microcracks and further damage an oxide film on the surface of a metal base material after reaching the metal base material, thereby accelerating the corrosion of the metal base material; the addition of the hollow glass beads can prevent the micro-crack of a paint film from expanding, but the hollow glass beads serving as low-density inorganic light materials are difficult to disperse uniformly in a resin matrix, have low bonding strength with the resin matrix material, and are easy to float after being stored for a period of time.
Disclosure of Invention
In view of the above, the present invention aims to provide an epoxy zinc-rich primer containing conductive polyaniline-coated hollow glass microspheres and a preparation method thereof, wherein the epoxy zinc-rich primer has a high zinc powder utilization rate, the bonding strength between the hollow glass microspheres in the primer and a resin matrix is high, and the hollow glass microspheres are not easy to float.
The invention provides an epoxy zinc-rich primer containing conductive polyaniline-coated hollow glass beads, which comprises a component A and a component B;
the component A comprises the following components in parts by weight: 10 to 20 parts of epoxy resin, 3 to 10 parts of conductive polyaniline-coated hollow glass beads, 40 to 60 parts of zinc powder, 1 to 2 parts of dispersant, 0.5 to 1 part of flatting agent, 0.5 to 1 part of anti-settling agent and 10 to 20 parts of solvent;
the component B is an epoxy curing agent, and the mass ratio of the epoxy curing agent to the epoxy resin is 1: (1.5-2.5).
Preferably, the epoxy resin is one or more of epoxy resin E-44, epoxy resin E-51 and epoxy resin E-21.
Preferably, the conductive polyaniline in the conductive polyaniline-coated hollow glass microsphere is one or more of protonic acid doped conductive polyaniline, light-induced doped conductive polyaniline and electrochemical doped conductive polyaniline.
Preferably, the density of the hollow glass beads in the conductive polyaniline-coated hollow glass beads is 0.15-0.7 g/cm 3 The particle size is 10 to 100 μm.
Preferably, the particle size of the zinc powder is 400-800 meshes.
Preferably, the solvent is one or more of acetone, toluene, xylene and dibutyl ester.
Preferably, the dispersant is available under the trade designation BYK-161, BYK-162, BYK-163, and BYK-164.
Preferably, the flatting agent is one or more of BYK-346, BYK-341, BYK-337 and BYK-354.
Preferably, the anti-settling agent is one or more of organic bentonite, castor oil derivative and polyamide wax.
The invention provides a preparation method of the epoxy zinc-rich primer in the technical scheme, which comprises the following steps:
mixing epoxy resin, conductive polyaniline-coated hollow glass microspheres, zinc powder, a dispersing agent, a leveling agent, an anti-settling agent and a solvent to obtain a component A; taking an epoxy curing agent as a component B;
when in use, the component A and the component B are mixed according to the proportion.
Preferably, the conductive polyaniline-coated hollow glass bead is prepared by the following steps:
and soaking the hollow glass beads in a conductive polyaniline solution, taking out and drying to obtain the conductive polyaniline-coated hollow glass beads.
Preferably, the concentration of the conductive polyaniline solution is 8-20 wt%; the soaking temperature is 20-40 ℃; the soaking time is 30-60 min.
Compared with the prior art, the invention provides the epoxy zinc-rich primer containing the conductive polyaniline coated hollow glass beads and the preparation method thereof. The epoxy zinc-rich primer provided by the invention comprises a component A and a component B; the component A comprises the following components in parts by weight: 10 to 20 parts of epoxy resin, 3 to 10 parts of conductive polyaniline-coated hollow glass beads, 40 to 60 parts of zinc powder, 1 to 2 parts of dispersant, 0.5 to 1 part of flatting agent, 0.5 to 1 part of anti-settling agent and 10 to 20 parts of solvent; the component B is an epoxy curing agent, and the mass ratio of the epoxy curing agent to the epoxy resin is 1: (1.5-2.5). According to the invention, a certain amount of conductive polyaniline is added into the epoxy zinc-rich primer to coat the hollow glass beads, so that a conductive bridge can be formed between the upper-layer zinc powder and the bottom zinc powder, the zinc powder deposited at the bottom is activated, the cathode protection effect of the zinc powder in the epoxy zinc-rich primer is fully exerted, and the utilization rate of the zinc powder is greatly improved; meanwhile, compared with the traditional hollow glass beads, the conductive polyaniline coated hollow glass beads can be better dispersed in the resin matrix, the bonding strength of the hollow glass beads and the resin matrix can be obviously enhanced, and the floating problem caused by the small density of the hollow glass beads can be effectively avoided.
Detailed Description
The technical solutions in the embodiments of the present invention are 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 of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The invention provides an epoxy zinc-rich primer containing conductive polyaniline-coated hollow glass beads, which comprises a component A and a component B;
the component A comprises the following components in parts by weight: 10-20 parts of epoxy resin, 3-10 parts of conductive polyaniline-coated hollow glass beads, 40-60 parts of zinc powder, 1-2 parts of dispersing agent, 0.5-1 part of flatting agent, 0.5-1 part of anti-settling agent and 10-20 parts of solvent;
the component B is an epoxy curing agent, and the mass ratio of the epoxy curing agent to the epoxy resin is 1: (1.5-2.5).
In the component A, the epoxy resin is preferably one or more of epoxy resin E-44, epoxy resin E-51 and epoxy resin E-21; the epoxy equivalent of the epoxy resin is preferably 180 to 250, and specifically 180, 185, 190, 195, 200, 210, 215, 220, 225, 230, 235, 240, 245 or 250.
In the epoxy zinc-rich primer provided by the invention, in the component A, the content of the epoxy resin in the component A can be 10 parts by weight, 11 parts by weight, 12 parts by weight, 13 parts by weight, 14 parts by weight, 15 parts by weight, 16 parts by weight, 17 parts by weight, 18 parts by weight, 19 parts by weight or 20 parts by weight.
In the component A, the epoxy zinc-rich primer provided by the inventionThe conductive polyaniline in the hollow glass microsphere coated by the conductive polyaniline is preferably one or more of protonic acid doped conductive polyaniline, photoinduced doped conductive polyaniline and electrochemical doped conductive polyaniline, and more preferably hydrochloric acid phosphoric acid doped conductive polyaniline; the molecular weight of the hydrochloric acid phosphoric acid doped conductive polyaniline is preferably 726; the density of the hydrochloric acid phosphoric acid doped conductive polyaniline is preferably 0.7-0.9 g/cm 3 More preferably 0.804g/cm 3 。
In the epoxy zinc-rich primer provided by the invention, in the component A, the density of the hollow glass beads in the conductive polyaniline-coated hollow glass beads is preferably 0.15-0.7 g/cm 3 Specifically, it may be 0.15g/cm 3 、0.2g/cm 3 、0.25g/cm 3 、0.3g/cm 3 、0.35g/cm 3 、0.38g/cm 3 、0.4g/cm 3 、0.45g/cm 3 、0.5g/cm 3 、0.55g/cm 3 、0.6g/cm 3 、0.65g/cm 3 Or 0.7g/cm 3 (ii) a The particle size of the hollow glass microspheres in the conductive polyaniline-coated hollow glass microspheres is preferably 10-100 μm, and specifically may be 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 65 μm, 70 μm, 80 μm, 90 μm or 100 μm.
In the epoxy zinc-rich primer provided by the invention, in the component A, the conductive polyaniline-coated hollow glass microspheres are preferably prepared by soaking the hollow glass microspheres in a conductive polyaniline solution, taking out and drying; wherein the solvent in the conductive polyaniline solution is preferably N, N-dimethylformamide and/or N-methylpyrrolidone; the concentration of the conductive polyaniline solution is preferably 8-20 wt%, and specifically can be 8wt%, 9wt%, 10wt%, 11wt%, 12wt%, 13wt%, 14wt%, 15wt%, 16wt%, 17wt%, 18wt%, 19wt% or 20wt%; the soaking temperature is preferably 20-40 ℃, and specifically can be 20 ℃, 25 ℃ (room temperature), 30 ℃, 35 ℃ or 40 ℃; the soaking time is preferably 30-60 min, and specifically can be 30min, 35min, 40min, 45min, 50min, 55min or 60min; the drying temperature is preferably 60-80 ℃, and specifically can be 60 ℃, 65 ℃, 70 ℃, 75 ℃ or 80 ℃; the drying time is preferably 1 to 3 hours, and specifically can be 1 hour, 1.5 hours, 2 hours, 2.5 hours or 3 hours.
In the epoxy zinc-rich primer provided by the invention, in the component a, the content of the conductive polyaniline-coated hollow glass bead in the component a can be 3 parts by weight, 3.5 parts by weight, 4 parts by weight, 4.5 parts by weight, 5 parts by weight, 5.5 parts by weight, 6 parts by weight, 6.5 parts by weight, 7 parts by weight, 7.5 parts by weight, 8 parts by weight, 8.5 parts by weight, 9 parts by weight, 9.5 parts by weight or 10 parts by weight.
In the epoxy zinc-rich primer provided by the invention, in the component A, the zinc powder is preferably spherical zinc powder and/or flaky zinc powder; the particle size of the zinc powder is preferably 400 to 800 meshes, and specifically 400 meshes, 425 meshes, 500 meshes, 600 meshes, 625 meshes, 650 meshes, 700 meshes or 800 meshes.
In the epoxy zinc-rich primer provided by the invention, in the component A, the content of the zinc powder in the component A can be 40 parts by weight, 41 parts by weight, 42 parts by weight, 43 parts by weight, 44 parts by weight, 45 parts by weight, 46 parts by weight, 47 parts by weight, 48 parts by weight, 49 parts by weight, 50 parts by weight, 51 parts by weight, 52 parts by weight, 53 parts by weight, 54 parts by weight, 55 parts by weight, 56 parts by weight, 57 parts by weight, 58 parts by weight, 59 parts by weight or 60 parts by weight.
In the epoxy zinc-rich primer provided by the invention, in the component A, the grade of the dispersant is preferably one or more of BYK-161, BYK-162, BYK-163 and BYK-164.
In the epoxy zinc-rich primer provided by the invention, in the component A, the content of the dispersant in the component A can be specifically 1 part by weight, 1.1 parts by weight, 1.2 parts by weight, 1.3 parts by weight, 1.4 parts by weight, 1.5 parts by weight, 1.6 parts by weight, 1.7 parts by weight, 1.8 parts by weight, 1.9 parts by weight or 2 parts by weight.
In the epoxy zinc-rich primer provided by the invention, in the component A, the grade of the leveling agent is preferably one or more of BYK-346, BYK-341, BYK-337 and BYK-354.
In the epoxy zinc-rich primer provided by the invention, in the component A, the content of the leveling agent in the component A can be specifically 0.5 part by weight, 0.55 part by weight, 0.6 part by weight, 0.65 part by weight, 0.7 part by weight, 0.75 part by weight, 0.8 part by weight, 0.85 part by weight, 0.9 part by weight, 0.95 part by weight or 1 part by weight.
In the epoxy zinc-rich primer provided by the invention, in the component A, the anti-settling agent is preferably one or more of organic bentonite, castor oil derivative and polyamide wax, and the castor oil derivative is preferably hydrogenated castor oil.
In the epoxy zinc-rich primer provided by the invention, in the component A, the content of the anti-settling agent in the component A can be specifically 0.5 part by weight, 0.55 part by weight, 0.6 part by weight, 0.65 part by weight, 0.7 part by weight, 0.75 part by weight, 0.8 part by weight, 0.85 part by weight, 0.9 part by weight, 0.95 part by weight or 1 part by weight.
In the epoxy zinc-rich primer provided by the invention, in the component A, the solvent is preferably one or more of acetone, toluene, xylene and dibutyl ester, and is more preferably a mixture of acetone and xylene; in the mixture, the volume ratio of acetone to xylene is preferably (0.5 to 2): 1, more preferably 1.
In the epoxy zinc-rich primer provided by the invention, in the component A, the content of the solvent in the component A can be 10 parts by weight, 11 parts by weight, 12 parts by weight, 13 parts by weight, 14 parts by weight, 15 parts by weight, 16 parts by weight, 17 parts by weight, 18 parts by weight, 19 parts by weight or 20 parts by weight.
In the epoxy zinc-rich primer provided by the invention, in the component b, the epoxy curing agent is preferably one or more of an aliphatic amine curing agent, an aromatic amine curing agent and an amine modified curing agent, and specifically can be polyamide 651.
In the epoxy zinc-rich primer provided by the invention, the mass ratio of the epoxy resin in the component a to the epoxy curing agent in the component b can be specifically 1.5.
The invention also provides a preparation method of the epoxy zinc-rich primer, which comprises the following steps:
mixing epoxy resin, conductive polyaniline-coated hollow glass microspheres, zinc powder, a dispersing agent, a leveling agent, an anti-settling agent and a solvent to obtain a component A; taking an epoxy curing agent as a component B;
when in use, the component A and the component B are mixed according to the proportion.
In the preparation method provided by the invention, the raw material information and the dosage ratio of each component are introduced in the above text, and are not described again; when the component A is prepared, the specific process of mixing is preferably as follows: the preparation method comprises the steps of uniformly mixing epoxy resin, conductive polyaniline-coated hollow glass beads, zinc powder, a dispersing agent, a leveling agent and an anti-settling agent, and then mixing with a solvent.
In the preparation method provided by the invention, the conductive polyaniline-coated hollow glass bead is preferably prepared according to the following steps:
and soaking the hollow glass beads in a conductive polyaniline solution, taking out and drying to obtain the conductive polyaniline-coated hollow glass beads.
In the preparation step of the conductive polyaniline-coated hollow glass microsphere provided by the invention, the conductive polyaniline solution is prepared by mixing conductive polyaniline and a solvent; the particle size of the conductive polyaniline is preferably less than or equal to 50nm, and more preferably less than or equal to 30nm; the solvent is preferably N, N-dimethylformamide and/or N-methylpyrrolidone; the concentration of the conductive polyaniline solution is preferably 8 to 20wt%, and specifically may be 8wt%, 9wt%, 10wt%, 11wt%, 12wt%, 13wt%, 14wt%, 15wt%, 16wt%, 17wt%, 18wt%, 19wt%, or 20wt%.
In the preparation step of the conductive polyaniline-coated hollow glass bead provided by the invention, the soaking temperature is preferably 20-40 ℃, and specifically can be 20 ℃, 25 ℃ (room temperature), 30 ℃, 35 ℃ or 40 ℃; the soaking time is preferably 30-60 min, and specifically can be 30min, 35min, 40min, 45min, 50min, 55min or 60min; the drying temperature is preferably 60-80 ℃, and specifically can be 60 ℃, 65 ℃, 70 ℃, 75 ℃ or 80 ℃; the drying time is preferably 1 to 3 hours, and specifically can be 1 hour, 1.5 hours, 2 hours, 2.5 hours or 3 hours.
According to the technical scheme provided by the invention, a certain amount of conductive polyaniline coated hollow glass microspheres are added into the epoxy zinc-rich primer, so that a conductive bridge can be formed between the upper-layer zinc powder and the bottom zinc powder, the zinc powder deposited at the bottom is activated, the cathode protection effect of the zinc powder in the epoxy zinc-rich primer is fully exerted, and the utilization rate of the zinc powder is greatly improved; meanwhile, compared with the traditional hollow glass beads, the conductive polyaniline-coated hollow glass beads can be better dispersed in a resin matrix, the bonding strength of the hollow glass beads and the resin matrix can be obviously enhanced, and the floating problem caused by the fact that the hollow glass beads are small in density is effectively avoided.
For the sake of clarity, the following examples are given in detail.
In the following examples provided by the present invention, the conductive polyaniline-coated hollow glass microspheres used were prepared according to the following steps:
firstly, N-dimethylformamide is used to mix conductive polyaniline (hydrochloric acid phosphoric acid doped conductive polyaniline, the particle diameter is less than or equal to 30nm, and the density is 0.804 g/cm) 3 Molecular weight of 726) to obtain a conductive polyaniline solution with a concentration of 10 wt%; then hollow glass microspheres (density 0.38 g/cm) 3 Particle size of 65 μm) is added into the conductive polyaniline solution and evenly stirred, and the mixture is soaked for 30min; and then filtering the hollow glass microspheres, putting the hollow glass microspheres in a drying box, and drying the hollow glass microspheres for two hours at the temperature of 70 ℃ to obtain the conductive polyaniline-coated hollow glass microspheres.
In the following examples provided by the present invention, the primer product was prepared as follows: uniformly stirring the raw materials except the solvent in the component A, and then adding the solvent and uniformly stirring to obtain a component A; when in use, the component A and the component B (epoxy curing agent) are mixed according to a proper proportion.
Example 1
Investigating the dispersion condition of the conductive polyaniline-coated hollow glass microspheres in epoxy resin:
and respectively adding the conductive polyaniline-coated hollow glass beads and the uncoated hollow glass beads into the epoxy resin E-51, wherein the adding amount is 3wt% of the mass of the epoxy resin, uniformly stirring, standing, and observing the floating condition of the epoxy resin. The results are shown in table 1:
TABLE 1 dispersion of hollow glass microspheres in epoxy resin
Example 2
Testing corrosion current and corrosion potential of the paint film:
(1) Preparing the epoxy zinc-rich primer with different addition amounts of the conductive polyaniline coated hollow glass beads, wherein the raw material composition is shown in table 2:
table 2 example 2 raw material information for primers used in performance testing
(2) Coating the priming paint 1-5 on a tinplate base material, and drying to form a paint film with the thickness of 80 mu m; the paint film is subjected to H treatment at 0.5mol/L 2 SO 4 Soaking the solution for 1h, and then testing the corrosion current and the corrosion potential of the solution by using a corrosion speed measuring instrument, wherein the higher the corrosion current is, the higher the corrosion potential is, and the higher the corrosion speed is. The test results are shown in table 3:
TABLE 3 Corrosion Current and Corrosion potential test results
| Corrosion current/(μ A. Cm) -2 ) | Corrosion potential/eV | |
| Primer 1 | 15.54 | -3.55 |
| Primer 2 | 11.79 | 0.072 |
| Primer 3 | 7.83 | 0.324 |
| Primer 4 | 4.56 | 0.433 |
| Primer 5 | 2.78 | 0.539 |
Example 3
Testing the adhesion grade, salt spray resistance, impact strength and crack resistance of the paint film:
(1) Preparing a series of epoxy zinc-rich primers with different component compositions, wherein the raw material compositions of the primers A to C are shown in tables 4 to 6:
table 4 example 3 raw material information for primer a used for performance testing
Table 5 example 3 raw material information of primer B used for performance test
Table 6 example 3 raw material information for primer C used for performance testing
The raw material information of primer D is as follows:
65012 parts of polyamide, 10 parts of dipropylene glycol butyl ether, 3 parts of polyethylene wax (basf AF 30), 10 parts of graphene oxide, 300 parts of zinc powder (spherical, 625 meshes), 3480.2 parts of BYK-1910.5 parts of zinc powder by weight, and preparing a component A; LP15011 aqueous epoxy emulsion is component B; the mass ratio of the two is 4.
The raw material information for primer E is as follows:
8 parts of polyamide curing agent, 7 parts of dipropylene glycol butyl ether, 2 parts of organic bentonite (BP-186C, zhejiang Fenghong new material), 65 parts of polyaniline grafted graphene oxide modified zinc powder, BYK-3480.2 parts and BYK-1910.3 parts by weight, and preparing a component A; 6520 the water-based epoxy emulsion is component B; the mass ratio of the two is 5;
in the primer E, the polyaniline grafted graphene oxide modified zinc powder is prepared by the following steps:
(1) preparing p-phenylenediamine grafted graphene oxide:
adding p-phenylenediamine into graphene oxide aqueous dispersion at the temperature of 60 ℃ until the p-phenylenediamine is completely dissolved, after reacting at constant temperature for 4 hours, filtering by using a polypropylene filter membrane with the average pore size of 0.2 mu m to obtain a precipitate, firstly carrying out centrifugal washing on the precipitate by using deionized water for 4 times, then carrying out centrifugal washing on the precipitate by using absolute ethyl alcohol for 4 times, carrying out vacuum drying for 10 hours at the temperature of 60 ℃ after carrying out suction filtration, and thus obtaining p-phenylenediamine grafted graphene oxide powder; the mass ratio of the p-phenylenediamine to the graphene oxide is 1;
(2) polyaniline grafted graphene oxide:
adding the aqueous dispersion of the p-phenylenediamine grafted graphene oxide powder obtained in the step (1) into a hydrochloric acid solution of aniline, uniformly stirring, dropwise adding an ammonium persulfate solution to obtain a mixed solution, stirring the mixed solution at a speed of 500r/min for 10 hours under an ice bath condition, filtering by using a polypropylene filter membrane with an average pore size of 0.2 mu m to obtain a precipitate, centrifugally washing the precipitate by using deionized water for 3 times, centrifugally washing by using absolute ethyl alcohol for 3 times, filtering, and vacuum-drying at 60 ℃ for 8 hours to obtain polyaniline grafted graphene oxide powder; the mass ratio of p-phenylenediamine grafted graphene oxide powder to aniline to ammonium persulfate in the mixed solution is 4;
(3) polyaniline grafted graphene oxide modified zinc powder:
adding BYK191 into the aqueous dispersion of the polyaniline grafted graphene oxide powder in the step (2) to enable the mass ratio of BYK191 to p-phenylenediamine grafted graphene oxide powder to be 8; the mass ratio of polyaniline grafted graphene oxide powder to zinc powder in the mixed solution is 10.
(2) Coating the priming paint A to the priming paint E on a tinplate base material, and drying to form a paint film with the thickness of 80 mu m; and testing the adhesion force grade, salt spray resistance, impact strength and crack resistance of the paint film. The results are shown in Table 7:
TABLE 7 adhesion rating, salt spray resistance, impact strength, crack resistance test results
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Claims (10)
1. An epoxy zinc-rich primer containing conductive polyaniline-coated hollow glass beads comprises a component A and a component B;
the component A comprises the following components in parts by weight: 10 to 20 parts of epoxy resin, 3 to 10 parts of conductive polyaniline-coated hollow glass beads, 40 to 60 parts of zinc powder, 1 to 2 parts of dispersant, 0.5 to 1 part of flatting agent, 0.5 to 1 part of anti-settling agent and 10 to 20 parts of solvent;
the component B is an epoxy curing agent, and the mass ratio of the epoxy curing agent to the epoxy resin is 1: (1.5-2.5).
2. The epoxy zinc rich primer of claim 1, wherein the epoxy resin is one or more of epoxy E-44, epoxy E-51, and epoxy E-21.
3. The epoxy zinc-rich primer according to claim 1, wherein the conductive polyaniline in the conductive polyaniline-coated hollow glass microspheres is one or more of protonic acid doped conductive polyaniline, light-induced doped conductive polyaniline and electrochemical doped conductive polyaniline.
4. The epoxy zinc-rich primer according to claim 1, wherein the density of the hollow glass beads in the conductive polyaniline-coated hollow glass beads is 0.15-0.7 g/cm 3 The particle size is 10 to 100 μm.
5. The epoxy zinc-rich primer as claimed in claim 1, wherein the zinc powder has a particle size of 400 to 800 mesh.
6. The epoxy zinc rich primer of claim 1, wherein the solvent is one or more of acetone, toluene, xylene, and dibutyl ester.
7. The epoxy zinc rich primer of claim 1, wherein the dispersant is one or more of BYK-161, BYK-162, BYK-163, and BYK-164;
the leveling agent is one or more of BYK-346, BYK-341, BYK-337 and BYK-354;
the anti-settling agent is one or more of organic bentonite, castor oil derivatives and polyamide wax.
8. A method of preparing the epoxy zinc rich primer of any one of claims 1 to 7, comprising the steps of:
mixing epoxy resin, conductive polyaniline-coated hollow glass beads, zinc powder, a dispersing agent, a leveling agent, an anti-settling agent and a solvent to obtain a component A; taking an epoxy curing agent as a component B;
when in use, the component A and the component B are mixed according to the proportion.
9. The preparation method according to claim 8, wherein the conductive polyaniline-coated hollow glass microsphere is prepared by the following steps:
and soaking the hollow glass beads in a conductive polyaniline solution, taking out and drying to obtain the conductive polyaniline-coated hollow glass beads.
10. The method according to claim 9, wherein the concentration of the conductive polyaniline solution is 8 to 20wt%; the soaking temperature is 20-40 ℃; the soaking time is 30-60 min.
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