CN107057569A - A kind of nano inorganic silicate zinc-rich composite anticorrosion coating and preparation method thereof - Google Patents
A kind of nano inorganic silicate zinc-rich composite anticorrosion coating and preparation method thereof Download PDFInfo
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- CN107057569A CN107057569A CN201710027613.8A CN201710027613A CN107057569A CN 107057569 A CN107057569 A CN 107057569A CN 201710027613 A CN201710027613 A CN 201710027613A CN 107057569 A CN107057569 A CN 107057569A
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- parts
- pyrrole throat
- hyperbranched poly
- polyetheramine
- poly pyrrole
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- 238000000576 coating method Methods 0.000 title claims abstract description 28
- 239000011248 coating agent Substances 0.000 title claims abstract description 27
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910052909 inorganic silicate Inorganic materials 0.000 title claims abstract description 21
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 21
- 239000011701 zinc Substances 0.000 title claims abstract description 21
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 90
- 229920000128 polypyrrole Polymers 0.000 claims abstract description 69
- 229920001577 copolymer Polymers 0.000 claims abstract description 62
- -1 polyoxyethylene Polymers 0.000 claims abstract description 50
- 229920000289 Polyquaternium Polymers 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 28
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims abstract description 28
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims abstract description 26
- 239000008367 deionised water Substances 0.000 claims abstract description 25
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 25
- 230000004048 modification Effects 0.000 claims abstract description 23
- 238000012986 modification Methods 0.000 claims abstract description 23
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 14
- MDFFNEOEWAXZRQ-UHFFFAOYSA-N aminyl Chemical compound [NH2] MDFFNEOEWAXZRQ-UHFFFAOYSA-N 0.000 claims abstract description 14
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920001228 polyisocyanate Polymers 0.000 claims abstract description 14
- 239000005056 polyisocyanate Substances 0.000 claims abstract description 14
- 239000004111 Potassium silicate Substances 0.000 claims abstract description 13
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052913 potassium silicate Inorganic materials 0.000 claims abstract description 13
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 13
- 239000011592 zinc chloride Substances 0.000 claims abstract description 13
- 235000005074 zinc chloride Nutrition 0.000 claims abstract description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 78
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 50
- 238000006243 chemical reaction Methods 0.000 claims description 37
- 238000003756 stirring Methods 0.000 claims description 33
- 229920000642 polymer Polymers 0.000 claims description 30
- 238000000967 suction filtration Methods 0.000 claims description 30
- 238000001291 vacuum drying Methods 0.000 claims description 30
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 26
- 229910052757 nitrogen Inorganic materials 0.000 claims description 26
- 206010013786 Dry skin Diseases 0.000 claims description 25
- 238000001556 precipitation Methods 0.000 claims description 25
- 239000007787 solid Substances 0.000 claims description 25
- 238000005406 washing Methods 0.000 claims description 25
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 24
- 229920000570 polyether Polymers 0.000 claims description 21
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 150000008065 acid anhydrides Chemical class 0.000 claims description 15
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 14
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 claims description 14
- UFWIBTONFRDIAS-UHFFFAOYSA-N naphthalene-acid Natural products C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 7
- 239000003822 epoxy resin Substances 0.000 claims description 7
- 150000002460 imidazoles Chemical class 0.000 claims description 7
- 229920000647 polyepoxide Polymers 0.000 claims description 7
- 150000003462 sulfoxides Chemical class 0.000 claims description 7
- 239000003643 water by type Substances 0.000 claims description 7
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 claims description 6
- 229940100630 metacresol Drugs 0.000 claims description 6
- ZJJATABWMGVVRZ-UHFFFAOYSA-N 1,12-dibromododecane Chemical class BrCCCCCCCCCCCCBr ZJJATABWMGVVRZ-UHFFFAOYSA-N 0.000 claims description 5
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 claims description 5
- VORLTHPZWVELIX-UHFFFAOYSA-N 1-methyl-2h-quinoline Chemical compound C1=CC=C2N(C)CC=CC2=C1 VORLTHPZWVELIX-UHFFFAOYSA-N 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 238000005292 vacuum distillation Methods 0.000 claims description 5
- HYZJCKYKOHLVJF-UHFFFAOYSA-N 1H-benzimidazole Chemical compound C1=CC=C2NC=NC2=C1 HYZJCKYKOHLVJF-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 150000001412 amines Chemical group 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 150000001556 benzimidazoles Chemical class 0.000 claims description 2
- 229960001760 dimethyl sulfoxide Drugs 0.000 description 18
- 239000002585 base Substances 0.000 description 12
- 238000005260 corrosion Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000013535 sea water Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920001909 styrene-acrylic polymer Polymers 0.000 description 2
- HSTOKWSFWGCZMH-UHFFFAOYSA-N 3,3'-diaminobenzidine Chemical compound C1=C(N)C(N)=CC=C1C1=CC=C(N)C(N)=C1 HSTOKWSFWGCZMH-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229920000554 ionomer Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 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
- C09D187/00—Coating compositions based on unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
- C09D187/005—Block or graft polymers not provided for in groups C09D101/00 - C09D185/04
-
- 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
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
-
- 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
- C09D171/00—Coating compositions based on polyethers obtained by reactions forming an ether link in the main chain; Coating compositions based on derivatives of such polymers
- C09D171/02—Polyalkylene oxides
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- Paints Or Removers (AREA)
Abstract
The invention discloses a kind of nano inorganic silicate zinc-rich composite anticorrosion coating, it is included：Nanomete talc powder, zinc chloride, potassium silicate, polyoxyethylene polyoxy propyl alcohol amidogen ether, KH 560, polyquaternium modification sulphonation polyetheramine hyperbranched poly pyrrole throat copolymer, polyisocyanates, deionized water and dimethyl sulfoxide (DMSO).The invention also discloses the preparation method of the nano inorganic silicate zinc-rich composite anticorrosion coating.
Description
Technical field
The invention belongs to technical field of coatings, more particularly it relates to which a kind of nano inorganic silicate zinc-rich is compound
Anticorrosive paint and preparation method thereof.
Background technology
Earth surface is largely covered by seawater, and ship is chronically in marine environment, corrodes extremely serious, corrosion is not
But the intensity of ship steel structure can be reduced, shortens ship's life, can also increase ship resistance, the speed of a ship or plane is reduced, ship is influenceed
Energy and navigation safety.Because corrosion causes structural failure and destruction, the loss of property even life is of common occurrence, it may be said that ship is rotten
Erosion is to influence one of the maximum factor in its life-span.
The anti-corrosion of current ship it is general in hull and hull bottom daub to obstruct contact of the seawater with ship, traditional ship
Coating is not fine and close enough due to being limited by own material property and technique, and water proof anti-seepage permeability is bad, poor adhesive force, sea water resistance
Property, the problems such as protecting against shock is bad.It is not satisfactory to the corrosion protection of parent metal effect, and have quite a few coating because
The harmful toxic matters such as leaded or chromate, the danger that there is pollution environment during preparation and use, this can hold with social economy
The requirement of continuous development strategy is incompatible.
At present, the marine ship coating of China's production, because the limitation of product formula, has weatherability, water resistance
Difference, easily catch fire and anti-corrosion, the shortcomings of mould proof, acid-proof alkaline is poor.
Hence it is highly desirable to by the improvement of formula, obtain weatherability and water resistance is strong, fire resistance is good and with anti-
The new coating of rotten, mould proof and acidproof alkali ability.
The content of the invention
In order to solve the above problems, one aspect of the present invention provides a kind of nano inorganic silicate zinc-rich composite anti-corrosive and applied
Material, in parts by weight, its preparing raw material include following components：
5-15 parts of nanomete talc powder
5-10 parts of zinc chloride
1-3 parts of potassium silicate
5-10 parts of polyoxyethylene polyoxy propyl alcohol amidogen ether
5-9 parts of KH-560
Polyquaternium modification sulphonation polyetheramine -5-10 parts of hyperbranched poly pyrrole throat copolymer
1-3 parts of polyisocyanates
15-25 parts of deionized water
1-5 parts of dimethyl sulfoxide (DMSO).
Preferably, described nano inorganic silicate zinc-rich composite anticorrosion coating, in parts by weight, its preparing raw material is included
Following components：
6-8 parts of nanomete talc powder
6-8 parts of zinc chloride
1-2 parts of potassium silicate
7-9 parts of polyoxyethylene polyoxy propyl alcohol amidogen ether
6-8 parts of KH-560
Polyquaternium modification sulphonation polyetheramine -6-9 parts of hyperbranched poly pyrrole throat copolymer
1-2 parts of polyisocyanates
17-20 parts of deionized water
2-3 parts of dimethyl sulfoxide (DMSO).
It is highly preferred that described nano inorganic silicate zinc-rich composite anticorrosion coating, in parts by weight, its preparing raw material bag
Containing following components：
7 parts of nanomete talc powder
7 parts of zinc chloride
2 parts of potassium silicate
8 parts of polyoxyethylene polyoxy propyl alcohol amidogen ether
7 parts of KH-560
Polyquaternium modification sulphonation polyetheramine -8 parts of hyperbranched poly pyrrole throat copolymer
2 parts of polyisocyanates
19 parts of deionized water
2 parts of dimethyl sulfoxide (DMSO).
In one embodiment, the preparation of the polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer
Method is：
（1）Prepare polyquaternium
In the three-necked bottle that 1000ml is dried, add 1,12- dibromo-dodecanes 0.1mol, Isosorbide-5-Nitrae-lupetazin 0.092mol with
And solvent dimethyl sulfoxide (DMSO) 80ml, at 50 DEG C after reaction 5 hours, add N- methylimidazole 0.0025mol and N- methyl
Quinoline 0.0025mol, at 50 DEG C after reaction 5 hours, vacuum distillation removes solvent and obtains polyquaternium；
（2）Prepare amino-terminated polyetheramine
In the three-necked bottle that 1000mL is dried, 95 grams epoxy resin E51,0.26mol benzylamine and 700 grams of diformazans are sequentially added
Base sulfoxide, leads to nitrogen protection and magnetic agitation；It is stirred at room temperature after 1h, heat up 95 DEG C of reaction 6h, after reaction terminates, is down to room temperature,
And pour into rapidly in 2000mL deionized waters, obtain a large amount of solid precipitations；With after the deionized water cyclic washing product, suction filtration is simultaneously
Collected polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain amino-terminated polyetheramine；
（3）Prepare hyperbranched poly pyrrole throat
In the three-necked bottle that 100mL is dried, 0.01 mole of the acid anhydride of 1,3,5- tri- (4- naphthoxys -1,8- diacid) benzene three is sequentially added
With 25ml metacresols, stir under nitrogen protection, after three acid anhydrides are completely dissolved, the 3 of 0.006 mole of addition, 3 '-benzidine
Amine, is stirred at room temperature after 60min, is heated to 80 DEG C, reacts 4h, then at 185 DEG C, reacts 10h；After reaction terminates, it is down to
Room temperature, and pour into rapidly in 2000mL methanol, obtain a large amount of solid precipitations；With after the methanol cyclic washing product, suction filtration is simultaneously received
Collect polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours produce the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
（4）Prepare polyetheramine-hyperbranched poly pyrrole throat copolymer
In the three-necked bottle that 100mL is dried, 1 gram of the amino-terminated polyetheramine, 0.6 gram of naphthalene anhydride end-blocking is sequentially added
The metacresol of hyperbranched poly pyrrole throat, 10mL dimethyl sulfoxide (DMSO) and 10mL, stirs after 60min, is heated under nitrogen protection
80 DEG C, 4h is reacted, then at 185 DEG C, reacts 10h；After reaction terminates, room temperature is down to, and is poured into rapidly in 2000mL methanol, is obtained
To a large amount of solids precipitation；With after the methanol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 50 DEG C of dryings
24 hours, produce polyetheramine-hyperbranched poly pyrrole throat copolymer；
（5）Prepare sulfonated polyether amine-hyperbranched poly pyrrole throat copolymer
In the three-necked bottle that 100mL is dried, 1 gram of the polyetheramine-hyperbranched poly pyrrole throat copolymer and 10mL is sequentially added
Mass fraction 98% the concentrated sulfuric acid, under nitrogen protection, at 40 DEG C stir 180min after, pour into frozen water, washed repeatedly with frozen water
Wash after the product, suction filtration and collected polymer, in vacuum drying oven, 60 DEG C of dryings produce sulfonated polyether amine-hyperbranched for 24 hours
Poly- pyrrole throat copolymer；
（6）Prepare polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer
In 100ml three-necked bottles, step is added（1）0.2 gram of obtained polyquaternium, step（5）Obtained sulfonated polyether amine-
0.5 gram of hyperbranched poly pyrrole throat copolymer, 0.2 gram of hexamethylene diamine, 0.05 gram of sodium hydroxide, deionized water 2mL and N, N- dimethyl
Formamide 50ml, after stirring at room temperature；After being reacted 10 hours at 60 DEG C, room temperature is down to, and pour into 2000mL first rapidly
In alcohol, a large amount of solid precipitations are obtained；With after the methanol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 60
DEG C dry 24 hours, obtain polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer.
It is preferably carried out in one kind in mode, described nano inorganic silicate zinc-rich composite anticorrosion coating, with parts by weight
Meter, its preparing raw material also includes following components：
1-3 parts of 5- amino-2-mercapto phenyl formic benzimidazoles
4- (imidazoles -1- bases) 1-3 parts of aniline；
Preferably, described nano inorganic silicate zinc-rich composite anticorrosion coating, in parts by weight, its preparing raw material also include with
Lower component：
2 parts of 5- amino-2-mercapto phenyl formics benzimidazole
4- (imidazoles -1- bases) 2 parts of aniline.
Another aspect of the present invention provides a kind of preparation method of nano inorganic silicate zinc-rich composite anticorrosion coating, bag
Include：Described material component is added and is sufficiently mixed in mixer after 1-100 minutes, discharging is obtained.
In one embodiment, the well-mixed time is 18 minutes.
In one embodiment, the stir speed (S.S.) of the mixer is 10 ~ 1000 revs/min；Preferably, the mixer
Stir speed (S.S.) be 300 revs/min.
Compared with prior art, beneficial effects of the present invention are：
1st, the addition of single substance is passed through（That is the addition of polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer）Both
Excellent weatherability, higher intensity, good fire resistance and excellent anti-microbial property can be provided, and can be risen again
Prevent system excessively crisp to plasticization, processing step can also be greatly reduced, so that there is provided the advantageous effects of the present invention.
2nd, the addition of 5- amino-2-mercapto phenyl formics benzimidazole and 4- (imidazoles -1- bases) aniline can improve the rigidity of system
And by improving the crosslink density of system with sulfonic ionomer, further, strengthen the intensity and water resistance of coating, from
And there is provided the advantageous effects of the present invention.
Embodiment
Raw material:
Nanomete talc powder（50 nanometers of average grain diameter）Purchased from poly- thousand Chemical Co., Ltd. in Shanghai.Polyisocyanates is that Hensel steps MDI,
Model 5005/44V20.Polyoxyethylene polyoxy propyl alcohol amidogen ether (BAPE nitrogen-containing polyethers defoamer) is purchased from Shanghai De Mao, model
K12.3,3 '-diaminobenzidine is purchased from CTI, and directly uses, without being further purified.Styrene-acrylic emulsion is purchased from Henkel, board
Number be 1863.Epoxy silane coupling agent KH-560 is purchased from Chemical Reagent Co., Ltd., Sinopharm Group.1,3,5- tri- (4- naphthoxys-
1,8- diacid) benzene three acid anhydride prepared according to method disclosed in patent CN101270111B.Other raw materials, which are purchased from Aladdin reagent, to be had
Limit company.
Embodiment 1
By 7 grams of nanomete talc powder, 7 grams of zinc chloride, 2 grams of potassium silicate, 8 grams of polyoxyethylene polyoxy propyl alcohol amidogen ether, 7 grams of KH-560,
Polyquaternium modification sulphonation polyetheramine -8 grams of hyperbranched poly pyrrole throat copolymer, 2 grams of polyisocyanates, 19 grams of deionized water with
And be sufficiently mixed in 2 grams of addition mixers of dimethyl sulfoxide (DMSO) after 18 minutes, discharging is obtained, and stir speed (S.S.) is 300 revs/min；
The preparation method of the polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer is：
（1）Prepare polyquaternium
In the three-necked bottle that 1000ml is dried, add 1,12- dibromo-dodecanes 0.1mol, Isosorbide-5-Nitrae-lupetazin 0.092mol with
And solvent dimethyl sulfoxide (DMSO) 80ml, at 50 DEG C after reaction 5 hours, add N- methylimidazole 0.0025mol and N- methyl
Quinoline 0.0025mol, at 50 DEG C after reaction 5 hours, vacuum distillation removes solvent and obtains polyquaternium；
（2）Prepare amino-terminated polyetheramine
In the three-necked bottle that 1000mL is dried, 95 grams epoxy resin E51,0.26mol benzylamine and 700 grams of diformazans are sequentially added
Base sulfoxide, leads to nitrogen protection and magnetic agitation；It is stirred at room temperature after 1h, heat up 95 DEG C of reaction 6h, after reaction terminates, is down to room temperature,
And pour into rapidly in 2000mL deionized waters, obtain a large amount of solid precipitations；With after the deionized water cyclic washing product, suction filtration is simultaneously
Collected polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain amino-terminated polyetheramine；
（3）Prepare hyperbranched poly pyrrole throat
In the three-necked bottle that 100mL is dried, 0.01 mole of the acid anhydride of 1,3,5- tri- (4- naphthoxys -1,8- diacid) benzene three is sequentially added
With 25ml metacresols, stir under nitrogen protection, after three acid anhydrides are completely dissolved, the 3 of 0.006 mole of addition, 3 '-benzidine
Amine, is stirred at room temperature after 60min, is heated to 80 DEG C, reacts 4h, then at 185 DEG C, reacts 10h；After reaction terminates, it is down to
Room temperature, and pour into rapidly in 2000mL methanol, obtain a large amount of solid precipitations；With after the methanol cyclic washing product, suction filtration is simultaneously received
Collect polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours produce the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
（4）Prepare polyetheramine-hyperbranched poly pyrrole throat copolymer
In the three-necked bottle that 100mL is dried, 1 gram of the amino-terminated polyetheramine, 0.6 gram of naphthalene anhydride end-blocking is sequentially added
The metacresol of hyperbranched poly pyrrole throat, 10mL dimethyl sulfoxide (DMSO) and 10mL, stirs after 60min, is heated under nitrogen protection
80 DEG C, 4h is reacted, then at 185 DEG C, reacts 10h；After reaction terminates, room temperature is down to, and is poured into rapidly in 2000mL methanol, is obtained
To a large amount of solids precipitation；With after the methanol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 50 DEG C of dryings
24 hours, produce polyetheramine-hyperbranched poly pyrrole throat copolymer；
（5）Prepare sulfonated polyether amine-hyperbranched poly pyrrole throat copolymer
In the three-necked bottle that 100mL is dried, 1 gram of the polyetheramine-hyperbranched poly pyrrole throat copolymer and 10mL is sequentially added
Mass fraction 98% the concentrated sulfuric acid, under nitrogen protection, at 40 DEG C stir 180min after, pour into frozen water, washed repeatedly with frozen water
Wash after the product, suction filtration and collected polymer, in vacuum drying oven, 60 DEG C of dryings produce sulfonated polyether amine-hyperbranched for 24 hours
Poly- pyrrole throat copolymer；
（6）Prepare polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer
In 100ml three-necked bottles, step is added（1）0.2 gram of obtained polyquaternium, step（5）Obtained sulfonated polyether amine-
0.5 gram of hyperbranched poly pyrrole throat copolymer, 0.2 gram of hexamethylene diamine, 0.05 gram of sodium hydroxide, deionized water 2mL and N, N- dimethyl
Formamide 50ml, after stirring at room temperature；After being reacted 10 hours at 60 DEG C, room temperature is down to, and pour into 2000mL first rapidly
In alcohol, a large amount of solid precipitations are obtained；With after the methanol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 60
DEG C dry 24 hours, obtain polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer.
Embodiment 2
By 7 grams of nanomete talc powder, 7 grams of zinc chloride, 2 grams of potassium silicate, 8 grams of polyoxyethylene polyoxy propyl alcohol amidogen ether, 7 grams of KH-560,
Polyquaternium modified polyether amine -8 grams of hyperbranched poly pyrrole throat copolymer, 2 grams of polyisocyanates, 19 grams of deionized water and two
It is sufficiently mixed in 2 grams of addition mixers of methyl sulfoxide after 18 minutes, discharging is obtained, stir speed (S.S.) is 300 revs/min；
The preparation method of the polyquaternium modified polyether amine-hyperbranched poly pyrrole throat copolymer is：
（1）Prepare polyquaternium
In the three-necked bottle that 1000ml is dried, add 1,12- dibromo-dodecanes 0.1mol, Isosorbide-5-Nitrae-lupetazin 0.092mol with
And solvent dimethyl sulfoxide (DMSO) 80ml, at 50 DEG C after reaction 5 hours, add N- methylimidazole 0.0025mol and N- methyl
Quinoline 0.0025mol, at 50 DEG C after reaction 5 hours, vacuum distillation removes solvent and obtains polyquaternium；
（2）Prepare amino-terminated polyetheramine
In the three-necked bottle that 1000mL is dried, 95 grams epoxy resin E51,0.26mol benzylamine and 700 grams of diformazans are sequentially added
Base sulfoxide, leads to nitrogen protection and magnetic agitation；It is stirred at room temperature after 1h, heat up 95 DEG C of reaction 6h, after reaction terminates, is down to room temperature,
And pour into rapidly in 2000mL deionized waters, obtain a large amount of solid precipitations；With after the deionized water cyclic washing product, suction filtration is simultaneously
Collected polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain amino-terminated polyetheramine；
（3）Prepare hyperbranched poly pyrrole throat
In the three-necked bottle that 100mL is dried, 0.01 mole of the acid anhydride of 1,3,5- tri- (4- naphthoxys -1,8- diacid) benzene three is sequentially added
With 25ml metacresols, stir under nitrogen protection, after three acid anhydrides are completely dissolved, the 3 of 0.006 mole of addition, 3 '-benzidine
Amine, is stirred at room temperature after 60min, is heated to 80 DEG C, reacts 4h, then at 185 DEG C, reacts 10h；After reaction terminates, it is down to
Room temperature, and pour into rapidly in 2000mL methanol, obtain a large amount of solid precipitations；With after the methanol cyclic washing product, suction filtration is simultaneously received
Collect polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours produce the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
（4）Prepare polyetheramine-hyperbranched poly pyrrole throat copolymer
In the three-necked bottle that 100mL is dried, 1 gram of the amino-terminated polyetheramine, 0.6 gram of naphthalene anhydride end-blocking is sequentially added
The metacresol of hyperbranched poly pyrrole throat, 10mL dimethyl sulfoxide (DMSO) and 10mL, stirs after 60min, is heated under nitrogen protection
80 DEG C, 4h is reacted, then at 185 DEG C, reacts 10h；After reaction terminates, room temperature is down to, and is poured into rapidly in 2000mL methanol, is obtained
To a large amount of solids precipitation；With after the methanol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 50 DEG C of dryings
24 hours, produce polyetheramine-hyperbranched poly pyrrole throat copolymer；
（5）Prepare polyquaternium modified polyether amine-hyperbranched poly pyrrole throat copolymer
In 100ml three-necked bottles, step is added（1）0.2 gram of obtained polyquaternium, step（4）Obtained polyetheramine-over-expense
Change poly- 0.5 gram of pyrrole throat copolymer, 0.2 gram of hexamethylene diamine, 0.05 gram of sodium hydroxide, deionized water 2mL and N, N- dimethyl formyl
Amine 50ml, after stirring at room temperature；After being reacted 10 hours at 60 DEG C, room temperature is down to, and is poured into rapidly in 2000mL methanol,
Obtain a large amount of solid precipitations；With after the methanol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 60 DEG C are done
Dry 24 hours, obtain polyquaternium modified polyether amine-hyperbranched poly pyrrole throat copolymer.
Embodiment 3
By 7 grams of nanomete talc powder, 7 grams of zinc chloride, 2 grams of potassium silicate, 8 grams of polyoxyethylene polyoxy propyl alcohol amidogen ether, 7 grams of KH-560,
Sulfonated polyether amine -8 grams of hyperbranched poly pyrrole throat copolymer, 2 grams of polyisocyanates, 19 grams of deionized water and dimethyl sulfoxide (DMSO)
It is sufficiently mixed in 2 grams of addition mixers after 18 minutes, discharging is obtained, stir speed (S.S.) is 300 revs/min；
The preparation method of the sulfonated polyether amine-hyperbranched poly pyrrole throat copolymer is：
（1）Prepare amino-terminated polyetheramine
In the three-necked bottle that 1000mL is dried, 95 grams epoxy resin E51,0.26mol benzylamine and 700 grams of diformazans are sequentially added
Base sulfoxide, leads to nitrogen protection and magnetic agitation；It is stirred at room temperature after 1h, heat up 95 DEG C of reaction 6h, after reaction terminates, is down to room temperature,
And pour into rapidly in 2000mL deionized waters, obtain a large amount of solid precipitations；With after the deionized water cyclic washing product, suction filtration is simultaneously
Collected polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain amino-terminated polyetheramine；
（2）Prepare hyperbranched poly pyrrole throat
In the three-necked bottle that 100mL is dried, 0.01 mole of the acid anhydride of 1,3,5- tri- (4- naphthoxys -1,8- diacid) benzene three is sequentially added
With 25ml metacresols, stir under nitrogen protection, after three acid anhydrides are completely dissolved, the 3 of 0.006 mole of addition, 3 '-benzidine
Amine, is stirred at room temperature after 60min, is heated to 80 DEG C, reacts 4h, then at 185 DEG C, reacts 10h；After reaction terminates, it is down to
Room temperature, and pour into rapidly in 2000mL methanol, obtain a large amount of solid precipitations；With after the methanol cyclic washing product, suction filtration is simultaneously received
Collect polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours produce the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
（3）Prepare polyetheramine-hyperbranched poly pyrrole throat copolymer
In the three-necked bottle that 100mL is dried, 1 gram of the amino-terminated polyetheramine, 0.6 gram of naphthalene anhydride end-blocking is sequentially added
The metacresol of hyperbranched poly pyrrole throat, 10mL dimethyl sulfoxide (DMSO) and 10mL, stirs after 60min, is heated under nitrogen protection
80 DEG C, 4h is reacted, then at 185 DEG C, reacts 10h；After reaction terminates, room temperature is down to, and is poured into rapidly in 2000mL methanol, is obtained
To a large amount of solids precipitation；With after the methanol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 50 DEG C of dryings
24 hours, produce polyetheramine-hyperbranched poly pyrrole throat copolymer；
（4）Prepare sulfonated polyether amine-hyperbranched poly pyrrole throat copolymer
In the three-necked bottle that 100mL is dried, 1 gram of the polyetheramine-hyperbranched poly pyrrole throat copolymer and 10mL is sequentially added
Mass fraction 98% the concentrated sulfuric acid, under nitrogen protection, at 40 DEG C stir 180min after, pour into frozen water, washed repeatedly with frozen water
Wash after the product, suction filtration and collected polymer, in vacuum drying oven, 60 DEG C of dryings produce sulfonated polyether amine-hyperbranched for 24 hours
Poly- pyrrole throat copolymer.
Embodiment 4
By 7 grams of nanomete talc powder, 7 grams of zinc chloride, 2 grams of potassium silicate, 8 grams of polyoxyethylene polyoxy propyl alcohol amidogen ether, 7 grams of KH-560,
4 grams of polyetheramine, 4 grams of hyperbranched poly pyrrole throat copolymer, 2 grams of polyisocyanates, 19 grams of deionized water and dimethyl sulfoxide (DMSO) 2
It is sufficiently mixed in gram addition mixer after 18 minutes, discharging is obtained, stir speed (S.S.) is 300 revs/min；
The preparation method of the polyetheramine is：
In the three-necked bottle that 1000mL is dried, 95 grams epoxy resin E51,0.26mol benzylamine and 700 grams of diformazans are sequentially added
Base sulfoxide, leads to nitrogen protection and magnetic agitation；It is stirred at room temperature after 1h, heat up 95 DEG C of reaction 6h, after reaction terminates, is down to room temperature,
And pour into rapidly in 2000mL deionized waters, obtain a large amount of solid precipitations；With after the deionized water cyclic washing product, suction filtration is simultaneously
Collected polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain amino-terminated polyetheramine；
The preparation method of the hyperbranched poly pyrrole throat is：
In the three-necked bottle that 100mL is dried, 0.01 mole of the acid anhydride of 1,3,5- tri- (4- naphthoxys -1,8- diacid) benzene three is sequentially added
With 25ml metacresols, stir under nitrogen protection, after three acid anhydrides are completely dissolved, the 3 of 0.006 mole of addition, 3 '-benzidine
Amine, is stirred at room temperature after 60min, is heated to 80 DEG C, reacts 4h, then at 185 DEG C, reacts 10h；After reaction terminates, it is down to
Room temperature, and pour into rapidly in 2000mL methanol, obtain a large amount of solid precipitations；With after the methanol cyclic washing product, suction filtration is simultaneously received
Collect polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours produce the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride.
Embodiment 5
By 7 grams of nanomete talc powder, 7 grams of zinc chloride, 2 grams of potassium silicate, 8 grams of polyoxyethylene polyoxy propyl alcohol amidogen ether, 7 grams of KH-560,
15 grams of styrene-acrylic emulsion, 2 grams of polyisocyanates, in 2 grams of addition mixers of 19 grams of deionized water and dimethyl sulfoxide (DMSO) fully
After mixing 18 minutes, discharging is obtained, and stir speed (S.S.) is 300 revs/min.
Embodiment 6
By 7 grams of nanomete talc powder, 7 grams of zinc chloride, 2 grams of potassium silicate, 8 grams of polyoxyethylene polyoxy propyl alcohol amidogen ether, 7 grams of KH-560,
Polyquaternium modification sulphonation polyetheramine -8 grams of hyperbranched poly pyrrole throat copolymer, 2 grams of polyisocyanates, 19 grams of deionized water, two
Filled in 2 grams of methyl sulfoxide, 2 grams of 5- amino-2-mercapto phenyl formics benzimidazole and 4- (imidazoles -1- bases) 2 grams of addition mixers of aniline
After dividing mixing 18 minutes, discharging is obtained, and stir speed (S.S.) is 300 revs/min；
The preparation method of the polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer is：
（1）Prepare polyquaternium
In the three-necked bottle that 1000ml is dried, add 1,12- dibromo-dodecanes 0.1mol, Isosorbide-5-Nitrae-lupetazin 0.092mol with
And solvent dimethyl sulfoxide (DMSO) 80ml, at 50 DEG C after reaction 5 hours, add N- methylimidazole 0.0025mol and N- methyl
Quinoline 0.0025mol, at 50 DEG C after reaction 5 hours, vacuum distillation removes solvent and obtains polyquaternium；
（2）Prepare amino-terminated polyetheramine
In the three-necked bottle that 1000mL is dried, 95 grams epoxy resin E51,0.26mol benzylamine and 700 grams of diformazans are sequentially added
Base sulfoxide, leads to nitrogen protection and magnetic agitation；It is stirred at room temperature after 1h, heat up 95 DEG C of reaction 6h, after reaction terminates, is down to room temperature,
And pour into rapidly in 2000mL deionized waters, obtain a large amount of solid precipitations；With after the deionized water cyclic washing product, suction filtration is simultaneously
Collected polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain amino-terminated polyetheramine；
（3）Prepare hyperbranched poly pyrrole throat
In the three-necked bottle that 100mL is dried, 0.01 mole of the acid anhydride of 1,3,5- tri- (4- naphthoxys -1,8- diacid) benzene three is sequentially added
With 25ml metacresols, stir under nitrogen protection, after three acid anhydrides are completely dissolved, the 3 of 0.006 mole of addition, 3 '-benzidine
Amine, is stirred at room temperature after 60min, is heated to 80 DEG C, reacts 4h, then at 185 DEG C, reacts 10h；After reaction terminates, it is down to
Room temperature, and pour into rapidly in 2000mL methanol, obtain a large amount of solid precipitations；With after the methanol cyclic washing product, suction filtration is simultaneously received
Collect polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours produce the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
（4）Prepare polyetheramine-hyperbranched poly pyrrole throat copolymer
In the three-necked bottle that 100mL is dried, 1 gram of the amino-terminated polyetheramine, 0.6 gram of naphthalene anhydride end-blocking is sequentially added
The metacresol of hyperbranched poly pyrrole throat, 10mL dimethyl sulfoxide (DMSO) and 10mL, stirs after 60min, is heated under nitrogen protection
80 DEG C, 4h is reacted, then at 185 DEG C, reacts 10h；After reaction terminates, room temperature is down to, and is poured into rapidly in 2000mL methanol, is obtained
To a large amount of solids precipitation；With after the methanol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 50 DEG C of dryings
24 hours, produce polyetheramine-hyperbranched poly pyrrole throat copolymer；
（5）Prepare sulfonated polyether amine-hyperbranched poly pyrrole throat copolymer
In the three-necked bottle that 100mL is dried, 1 gram of the polyetheramine-hyperbranched poly pyrrole throat copolymer and 10mL is sequentially added
Mass fraction 98% the concentrated sulfuric acid, under nitrogen protection, at 40 DEG C stir 180min after, pour into frozen water, washed repeatedly with frozen water
Wash after the product, suction filtration and collected polymer, in vacuum drying oven, 60 DEG C of dryings produce sulfonated polyether amine-hyperbranched for 24 hours
Poly- pyrrole throat copolymer；
（6）Prepare polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer
In 100ml three-necked bottles, step is added（1）0.2 gram of obtained polyquaternium, step（5）Obtained sulfonated polyether amine-
0.5 gram of hyperbranched poly pyrrole throat copolymer, 0.2 gram of hexamethylene diamine, 0.05 gram of sodium hydroxide, deionized water 2mL and N, N- dimethyl
Formamide 50ml, after stirring at room temperature；After being reacted 10 hours at 60 DEG C, room temperature is down to, and pour into 2000mL first rapidly
In alcohol, a large amount of solid precipitations are obtained；With after the methanol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 60
DEG C dry 24 hours, obtain polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer.
Method of testing
Coating obtained by embodiment 1-6 is coated on ship, and test performance, test result is shown in Table 1.
Table 1
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Surface drying time/h | 1.3 | 2.3 | 1.2 | 10.2 | 4.5 | 1.0 |
| Adhesive force | 1 grade | 1 grade | 1 grade | 4 grades | 2 grades | 0 grade |
| Impact resistance/cm | 96 | 55 | 97 | 8 | 33 | 99 |
| Salt fog resistance（Draw × h) | 1768 | 1233 | 1857 | 13 | 567 | 1903 |
| Resistance to salt water（3.5%NaCl, day） | 188 | 104 | 195 | 5 | 87 | 201 |
| Outward appearance | It is smooth | It is smooth | It is smooth | Out-of-flatness | It is smooth | It is smooth |
| Antifriction performance/number of times | 1823 | 1098 | 1902 | 24 | 771 | 2190 |
| Fire endurance/h | 6.0 | 4.9 | 6.7 | 0.5 | 1.9 | 7.5 |
| Antibiotic rate/% | 99 | 98 | 0 | 0 | 0 | 99 |
Data above can be seen that and without using polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer, 5- ammonia
The coating of base -2-mercaptobenzimidazole and 4- (imidazoles -1- bases) aniline is compared, and coating of the invention has substantially preferably property
Can, thus provide the advantageous effects of the present invention.
Claims (10)
1. a kind of nano inorganic silicate zinc-rich composite anticorrosion coating, it is characterised in that in parts by weight, its preparing raw material is included
Following components：
5-15 parts of nanomete talc powder
5-10 parts of zinc chloride
1-3 parts of potassium silicate
5-10 parts of polyoxyethylene polyoxy propyl alcohol amidogen ether
5-9 parts of KH-560
Polyquaternium modification sulphonation polyetheramine -5-10 parts of hyperbranched poly pyrrole throat copolymer
1-3 parts of polyisocyanates
15-25 parts of deionized water
1-5 parts of dimethyl sulfoxide (DMSO).
2. nano inorganic silicate zinc-rich composite anticorrosion coating according to claim 1, it is characterised in that with parts by weight
Meter, its preparing raw material includes following components：
6-8 parts of nanomete talc powder
6-8 parts of zinc chloride
1-2 parts of potassium silicate
7-9 parts of polyoxyethylene polyoxy propyl alcohol amidogen ether
6-8 parts of KH-560
Polyquaternium modification sulphonation polyetheramine -6-9 parts of hyperbranched poly pyrrole throat copolymer
1-2 parts of polyisocyanates
17-20 parts of deionized water
2-3 parts of dimethyl sulfoxide (DMSO).
3. nano inorganic silicate zinc-rich composite anticorrosion coating according to claim 1, it is characterised in that with parts by weight
Meter, its preparing raw material includes following components：
7 parts of nanomete talc powder
7 parts of zinc chloride
2 parts of potassium silicate
8 parts of polyoxyethylene polyoxy propyl alcohol amidogen ether
7 parts of KH-560
Polyquaternium modification sulphonation polyetheramine -8 parts of hyperbranched poly pyrrole throat copolymer
2 parts of polyisocyanates
19 parts of deionized water
2 parts of dimethyl sulfoxide (DMSO).
4. nano inorganic silicate zinc-rich composite anticorrosion coating according to claim 1, it is characterised in that the polyquaternary amine
The preparation method of salt modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer is：
（1）Prepare polyquaternium
In the three-necked bottle that 1000ml is dried, add 1,12- dibromo-dodecanes 0.1mol, Isosorbide-5-Nitrae-lupetazin 0.092mol with
And solvent dimethyl sulfoxide (DMSO) 80ml, at 50 DEG C after reaction 5 hours, add N- methylimidazole 0.0025mol and N- methyl
Quinoline 0.0025mol, at 50 DEG C after reaction 5 hours, vacuum distillation removes solvent and obtains polyquaternium；
（2）Prepare amino-terminated polyetheramine
In the three-necked bottle that 1000mL is dried, 95 grams epoxy resin E51,0.26mol benzylamine and 700 grams of diformazans are sequentially added
Base sulfoxide, leads to nitrogen protection and magnetic agitation；It is stirred at room temperature after 1h, heat up 95 DEG C of reaction 6h, after reaction terminates, is down to room temperature,
And pour into rapidly in 2000mL deionized waters, obtain a large amount of solid precipitations；With after the deionized water cyclic washing product, suction filtration is simultaneously
Collected polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain amino-terminated polyetheramine；
（3）Prepare hyperbranched poly pyrrole throat
In the three-necked bottle that 100mL is dried, 0.01 mole of the acid anhydride of 1,3,5- tri- (4- naphthoxys -1,8- diacid) benzene three is sequentially added
With 25ml metacresols, stir under nitrogen protection, after three acid anhydrides are completely dissolved, the 3 of 0.006 mole of addition, 3 '-benzidine
Amine, is stirred at room temperature after 60min, is heated to 80 DEG C, reacts 4h, then at 185 DEG C, reacts 10h；After reaction terminates, it is down to
Room temperature, and pour into rapidly in 2000mL methanol, obtain a large amount of solid precipitations；With after the methanol cyclic washing product, suction filtration is simultaneously received
Collect polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours produce the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
（4）Prepare polyetheramine-hyperbranched poly pyrrole throat copolymer
In the three-necked bottle that 100mL is dried, 1 gram of the amino-terminated polyetheramine, 0.6 gram of naphthalene anhydride end-blocking is sequentially added
The metacresol of hyperbranched poly pyrrole throat, 10mL dimethyl sulfoxide (DMSO) and 10mL, stirs after 60min, is heated under nitrogen protection
80 DEG C, 4h is reacted, then at 185 DEG C, reacts 10h；After reaction terminates, room temperature is down to, and is poured into rapidly in 2000mL methanol, is obtained
To a large amount of solids precipitation；With after the methanol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 50 DEG C of dryings
24 hours, produce polyetheramine-hyperbranched poly pyrrole throat copolymer；
（5）Prepare sulfonated polyether amine-hyperbranched poly pyrrole throat copolymer
In the three-necked bottle that 100mL is dried, 1 gram of the polyetheramine-hyperbranched poly pyrrole throat copolymer and 10mL is sequentially added
Mass fraction 98% the concentrated sulfuric acid, under nitrogen protection, at 40 DEG C stir 180min after, pour into frozen water, washed repeatedly with frozen water
Wash after the product, suction filtration and collected polymer, in vacuum drying oven, 60 DEG C of dryings produce sulfonated polyether amine-hyperbranched for 24 hours
Poly- pyrrole throat copolymer；
（6）Prepare polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer
In 100ml three-necked bottles, step is added（1）0.2 gram of obtained polyquaternium, step（5）Obtained sulfonated polyether amine-
0.5 gram of hyperbranched poly pyrrole throat copolymer, 0.2 gram of hexamethylene diamine, 0.05 gram of sodium hydroxide, deionized water 2mL and N, N- dimethyl
Formamide 50ml, after stirring at room temperature；After being reacted 10 hours at 60 DEG C, room temperature is down to, and pour into 2000mL first rapidly
In alcohol, a large amount of solid precipitations are obtained；With after the methanol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 60
DEG C dry 24 hours, obtain polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer.
5. the nano inorganic silicate zinc-rich composite anticorrosion coating according to claim any one of 1-4, it is characterised in that with
Parts by weight meter, its preparing raw material also includes following components：
1-3 parts of 5- amino-2-mercapto phenyl formic benzimidazoles
4- (imidazoles -1- bases) 1-3 parts of aniline.
6. nano inorganic silicate zinc-rich composite anticorrosion coating according to claim 5, it is characterised in that with parts by weight
Meter, its preparing raw material also includes following components：
2 parts of 5- amino-2-mercapto phenyl formics benzimidazole
4- (imidazoles -1- bases) 2 parts of aniline.
7. a kind of preparation method of nano inorganic silicate zinc-rich composite anticorrosion coating, including：By any one of claim 1-6 institutes
The material component stated is added to be sufficiently mixed after 1-100 minutes in mixer, and discharging is obtained.
8. the preparation method of nano inorganic silicate zinc-rich composite anticorrosion coating according to claim 7, it is characterised in that
The well-mixed time is 18 minutes.
9. the preparation method of nano inorganic silicate zinc-rich composite anticorrosion coating according to claim 7, it is characterised in that
The stir speed (S.S.) of the mixer is 10 ~ 1000 revs/min.
10. the preparation method of nano inorganic silicate zinc-rich composite anticorrosion coating according to claim 9, its feature exists
In the stir speed (S.S.) of the mixer is 300 revs/min.
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| CN108144109A (en) * | 2017-12-28 | 2018-06-12 | 浙江海创医疗器械有限公司 | A kind of aerogel dressing of the interpenetrating networks cross-linked structure containing honey |
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Application publication date: 20170818 |