CN116855163A - Flexible pressure-sensitive color-changing anti-corrosion primer, preparation method and application thereof, and intelligent threaded fastener with visible fastening degree - Google Patents
Flexible pressure-sensitive color-changing anti-corrosion primer, preparation method and application thereof, and intelligent threaded fastener with visible fastening degree Download PDFInfo
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- 238000005260 corrosion Methods 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
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- 239000011248 coating agent Substances 0.000 claims abstract description 43
- 239000011347 resin Substances 0.000 claims abstract description 36
- 229920005989 resin Polymers 0.000 claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 30
- 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 19
- 230000007797 corrosion Effects 0.000 claims abstract description 15
- 239000002270 dispersing agent Substances 0.000 claims abstract description 15
- 239000002318 adhesion promoter Substances 0.000 claims abstract description 14
- 238000009736 wetting Methods 0.000 claims abstract description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims description 54
- 239000005056 polyisocyanate Substances 0.000 claims description 26
- 229920001228 polyisocyanate Polymers 0.000 claims description 26
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- 239000002904 solvent Substances 0.000 claims description 23
- 229910021485 fumed silica Inorganic materials 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 12
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 11
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 11
- 229920005862 polyol Polymers 0.000 claims description 10
- 150000003077 polyols Chemical class 0.000 claims description 10
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- 230000000007 visual effect Effects 0.000 claims description 9
- -1 7-diethylamino-3- [4' - (trifluoromethyl) benzoyl ] methylcoumarin Chemical compound 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims description 8
- 239000003381 stabilizer Substances 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims description 5
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 5
- PASDCCFISLVPSO-UHFFFAOYSA-N benzoyl chloride Chemical compound ClC(=O)C1=CC=CC=C1 PASDCCFISLVPSO-UHFFFAOYSA-N 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 5
- 239000003431 cross linking reagent Substances 0.000 claims description 5
- 125000005442 diisocyanate group Chemical group 0.000 claims description 5
- 239000012948 isocyanate Substances 0.000 claims description 5
- 150000002513 isocyanates Chemical class 0.000 claims description 5
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004925 Acrylic resin Substances 0.000 claims description 4
- 229920000178 Acrylic resin Polymers 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- XQBCVRSTVUHIGH-UHFFFAOYSA-L [dodecanoyloxy(dioctyl)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCCCCCC)(CCCCCCCC)OC(=O)CCCCCCCCCCC XQBCVRSTVUHIGH-UHFFFAOYSA-L 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
- 150000002009 diols Chemical class 0.000 claims description 4
- 230000000149 penetrating effect Effects 0.000 claims description 4
- 229920001610 polycaprolactone Polymers 0.000 claims description 4
- 239000004632 polycaprolactone Substances 0.000 claims description 4
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 3
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 3
- 239000002518 antifoaming agent Substances 0.000 claims description 3
- 239000000701 coagulant Substances 0.000 claims description 3
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 3
- 229920000570 polyether Polymers 0.000 claims description 3
- 239000005062 Polybutadiene Substances 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 239000003146 anticoagulant agent Substances 0.000 claims description 2
- 229940127219 anticoagulant drug Drugs 0.000 claims description 2
- 229920002857 polybutadiene Polymers 0.000 claims description 2
- 239000013557 residual solvent Substances 0.000 claims description 2
- 238000005507 spraying Methods 0.000 abstract description 13
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 description 37
- 238000007789 sealing Methods 0.000 description 34
- 230000000052 comparative effect Effects 0.000 description 26
- 238000001723 curing Methods 0.000 description 23
- 238000007599 discharging Methods 0.000 description 20
- 238000004806 packaging method and process Methods 0.000 description 20
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 18
- 238000001914 filtration Methods 0.000 description 15
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 11
- 238000005520 cutting process Methods 0.000 description 10
- 229910000838 Al alloy Inorganic materials 0.000 description 9
- 238000011049 filling Methods 0.000 description 9
- 150000003839 salts Chemical class 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000013530 defoamer Substances 0.000 description 8
- 210000001503 joint Anatomy 0.000 description 8
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- 230000007935 neutral effect Effects 0.000 description 5
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 238000005452 bending Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- AOFIWCXMXPVSAZ-UHFFFAOYSA-N 4-methyl-2,6-bis(methylsulfanyl)benzene-1,3-diamine Chemical compound CSC1=CC(C)=C(N)C(SC)=C1N AOFIWCXMXPVSAZ-UHFFFAOYSA-N 0.000 description 3
- 235000019082 Osmanthus Nutrition 0.000 description 3
- 241000333181 Osmanthus Species 0.000 description 3
- 235000019083 Osmanthus fragrans Nutrition 0.000 description 3
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- 239000002131 composite material Substances 0.000 description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 241000272201 Columbiformes Species 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- 229920002635 polyurethane Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- IBOFVQJTBBUKMU-UHFFFAOYSA-N 4,4'-methylene-bis-(2-chloroaniline) Chemical compound C1=C(Cl)C(N)=CC=C1CC1=CC=C(N)C(Cl)=C1 IBOFVQJTBBUKMU-UHFFFAOYSA-N 0.000 description 1
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 description 1
- 241001112258 Moca Species 0.000 description 1
- 229920002396 Polyurea Polymers 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 235000003704 aspartic acid Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/06—Polyurethanes from polyesters
-
- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/08—Polyurethanes from polyethers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16B—DEVICES FOR FASTENING OR SECURING CONSTRUCTIONAL ELEMENTS OR MACHINE PARTS TOGETHER, e.g. NAILS, BOLTS, CIRCLIPS, CLAMPS, CLIPS OR WEDGES; JOINTS OR JOINTING
- F16B35/00—Screw-bolts; Stay-bolts; Screw-threaded studs; Screws; Set screws
- F16B35/04—Screw-bolts; Stay-bolts; Screw-threaded studs; Screws; Set screws with specially-shaped head or shaft in order to fix the bolt on or in an object
- F16B35/06—Specially-shaped heads
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16B—DEVICES FOR FASTENING OR SECURING CONSTRUCTIONAL ELEMENTS OR MACHINE PARTS TOGETHER, e.g. NAILS, BOLTS, CIRCLIPS, CLAMPS, CLIPS OR WEDGES; JOINTS OR JOINTING
- F16B43/00—Washers or equivalent devices; Other devices for supporting bolt-heads or nuts
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a flexible pressure-sensitive color-changing anti-corrosion primer, a preparation method, application and an intelligent threaded fastener with visible fastening degree. The flexible pressure-sensitive color-changing anti-corrosion primer comprises a component A and a component B; the component A comprises flexible resin, a piezochromic indicator, superfine talcum powder, nano aluminum oxide and a wetting dispersant; the component B comprises a flexible curing agent and an adhesion promoter. The flexible pressure-sensitive color-changing anti-corrosion primer disclosed by the invention is simple in preparation method, has a good coating pot life, can be suitable for traditional air spraying, has good pressure-sensitive color-changing property, anti-corrosion property and environmental suitability, and can well solve the micro corrosion problems of threaded fasteners, rivets, joints and fatigue key parts.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a flexible pressure-sensitive color-changing anti-corrosion primer, a preparation method and application thereof, and an intelligent threaded fastener with visible fastening degree.
Background
With the development of light weight materials, light weight materials such as aluminum alloy, composite materials and the like are more widely applied. At present, the combination of different materials is mostly linked by means of rivets, screws and the like, and the anticorrosion measures of the parts are mostly spraying anticorrosion paint along with the main body. In the practical application process, the coating used for rivets, joints and fatigue key parts can bear larger load in the high-speed use process. Because of the effects of vibration and deformation, the rigid coating is easy to generate microcrack or cracking at the positions, so that the protection effect on the metal matrix is lost, and then crevice corrosion or galvanic corrosion is caused, so that the material butt joint position is damaged. The development of crevice corrosion has concealment and burst, the incubation period of initial corrosion is long, and after the corrosion degree reaches a certain critical degree, the rivet or the joint can be damaged in the high-speed use process, so that serious accidents are caused.
In the 90 s of the 20 th century, the army prescription established the federal standard of TT-P-2760 high solids elastic polyurethane primer, which is specially used for rivets and joints and is matched with high-flexibility skin finish. The standard of the coating not only requires that the coating has good physical and mechanical properties, but also has good anti-corrosion protection effect. Such as: a polyurethane primer for a single-liquid elastic moisture-curing aircraft, which is developed by Desotor corporation and has the brand name Koroflex, has a coating film which can bend with the vibration of the aircraft to prevent cracking of rivets and other high-stress-area coatings, and can continue to protect a substrate even if a top coat layer is damaged. The primer can also be used for composite materials and rubber, and has excellent adhesion to a finish layer. The Shermin-WILLIAMS aviation coating supplier produced a high performance two-component chromium-free elastomeric epoxy primer of grade CM0483790 having high flexibility, good dielectric resistance and good adhesion. The German Bayer material science and technology company develops an aspartic acid polyester urea coating which has good elasticity and excellent weather resistance, is applied to ICE high-speed trains, and is not suitable for areas with large temperature interval spans. At present, few flexible primers specially developed for rivets, joints and key fatigue parts are in domestic use. Therefore, it is necessary to prepare a flexible corrosion-resistant primer for rivets, joints and fatigue critical parts, and it is also necessary to invent a simple and easy-to-industrialize method for preparing intelligent threaded fasteners with visual fastening degree to reduce the inspection cost.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a flexible pressure-sensitive color-changing anti-corrosion primer, a preparation method and application thereof, and an intelligent threaded fastener with visible fastening degree. The flexible pressure-sensitive color-changing anti-corrosion primer can adopt a traditional air spraying mode, the application pot life can reach 6 hours, the surface drying time can reach 40 minutes, and the construction is convenient. The composite material has excellent comprehensive mechanical properties and good tensile fatigue resistance, can be used for rivets, joints, fatigue key parts and the like, and can effectively prevent corrosion. More importantly, the coating has a piezochromic function, the fastening degree of the threaded fastener and the connecting part can be effectively checked through the color change, the maintenance time is shortened, and the loss caused by loosening of the threaded fastener and the like is avoided.
The invention aims at providing a flexible pressure-sensitive color-changing anti-corrosion primer which comprises a component A and a component B; the component A comprises flexible resin, a piezochromic indicator, superfine talcum powder, nano aluminum oxide and a wetting dispersant; the component B comprises a flexible curing agent and an adhesion promoter.
In a preferred embodiment of the present invention,
each component in the component A is calculated by taking flexible resin as 100 parts by weight,
100-180 parts by weight of a piezochromic indicator; preferably 120 to 170 parts by weight; more preferably 140 to 170 parts by weight;
20-80 parts of superfine talcum powder; preferably 30 to 50 parts by weight; more preferably 35 to 45 parts by weight;
30-80 parts by weight of nano aluminum oxide; preferably 30 to 50 parts by weight; more preferably 35 to 40 parts by weight;
2-5 parts by weight of wetting dispersant; preferably 2 to 4 parts by weight; more preferably 3 to 4 parts by weight;
each component in the component B takes a flexible curing agent as 100 parts by weight,
0-10 parts by weight of adhesion promoter; preferably 2 to 10 parts by weight; more preferably 4 to 6 parts by weight;
the dosage ratio of the component A to the component B is (4-12): 1, preferably (4 to 10): 1, more preferably (5 to 10): 1.
in a preferred embodiment of the present invention,
the flexible resin is at least one selected from flexible epoxy modified acrylic resin and flexible polyisocyanate prepolymer resin; preferably, the method comprises the steps of,
the flexible epoxy modified acrylic resin is selected from conventional flexible epoxy modified acrylic resin in the prior art in the field, and one or more of A-8200 resin of Qingdian New material Co., ltd.and TC-101B, F221 resin of green-linked chemical technology Co., ltd are preferred in the invention; and/or the number of the groups of groups,
the flexible polyisocyanate prepolymer resin may be obtained commercially or by any method known in the art, and is preferably prepared by a preparation method comprising the steps of:
step 1: reacting isocyanate, a catalyst and part of solvent A to obtain a material 1;
step 2: adding a stabilizer and a cross-linking agent into the material 1 to react to obtain a material 2;
step 3: adding oligomer polyol into the material 2 to react to obtain a material 3;
step 4: adding a coagulant into the material 3 for reaction, and adding the residual solvent A after the reaction is finished to obtain the flexible polyisocyanate prepolymer resin.
In a preferred embodiment of the present invention,
the isocyanate is one or more selected from isophorone diisocyanate, hexamethylene diisocyanate, 4' -dicyclohexylmethane diisocyanate and terephthalyl diisocyanate, preferably isophorone diisocyanate and/or terephthalyl diisocyanate, and the main component is more than or equal to 99%; and/or the number of the groups of groups,
the catalyst is selected from one or more of triethylamine and dioctyltin dilaurate; and/or the number of the groups of groups,
the stabilizer is selected from conventional stabilizers in the field, preferably one or more of Stabaxol-1 and Stabaxol-P stabilizers; and/or the number of the groups of groups,
the oligomer polyol is selected from one or more of polycaprolactone diol, polyether polyol and polybutadiene polyol; and/or the number of the groups of groups,
the crosslinking agent is selected from one or more of conventional crosslinking agents in the field, preferably selected from Trimethylolpropane (TMP), 3 '-dichloro-4, 4' -diaminodiphenylmethane (MOCA), and dimethyl thiotoluenediamine (DMTDA); and/or the number of the groups of groups,
the anti-coagulant is selected from one or more of benzoyl chloride and phosphoric acid; and/or the number of the groups of groups,
the solvent A is one or more selected from butyl acetate, ethyl acetate and propylene glycol methyl ether acetate, and the water content is less than or equal to 0.2%.
The preparation method of the flexible polyisocyanate prepolymer resin can adopt the following specific steps:
step 1: adding 30-45 parts by weight of isocyanate, 0.01-0.05 part by weight of catalyst and 15-30 parts by weight of solvent A into a reaction kettle, introducing nitrogen for protection, stirring for 10-20 min at 20-30 ℃ to uniformly mix the materials, and heating to 60-65 ℃ to react for 10-20 min to obtain a material 1.
Step 2: adding 0.1-1.0 part by weight of stabilizer into the material 1, heating to 70-80 ℃, slowly adding 1.0-1.5 parts by weight of cross-linking agent under the stirring condition, and reacting for 1-1.5 hours at 85-95 ℃ after the adding is finished to obtain the material 2.
Step 3: slowly adding 40-55 parts by weight of oligomer polyol into the material 2 at 70-80 ℃ under stirring, reacting for 2-2.5 h at 85-95 ℃, and then cooling to 40-50 ℃ to obtain the material 3.
Step 4: slowly adding 0.01-0.05 part by weight of coagulant into the material 3 under the condition of stirring at 40-50 ℃, carrying out heat preservation reaction at 40-50 ℃ for 1-1.5 h after the addition, adding 0-30 parts by weight of solvent A after the reaction is finished, cooling to below 40 ℃, discharging, and sealing and packaging to obtain the flexible polyisocyanate prepolymer resin.
In a preferred embodiment of the present invention,
the superfine talcum powder is selected from conventional talcum powder in the prior art in the field, the fineness is 500-2000 meshes, preferably 1250-2000 meshes, more preferably 1250-1500 meshes, and the superfine talcum powder is preferably one or more of Guangxi osmanthus fragrans talcum powder and Qingdao white pigeon talcum powder in the invention; and/or the number of the groups of groups,
the nanometer aluminum oxide is selected from conventional nanometer aluminum oxide in the prior art in the field, the grain diameter is 5-500 nm, preferably 10-100 nm, more preferably 20-80 nm, and is preferably selected from at least one of alpha-phase nanometer aluminum oxide and gamma-phase nanometer aluminum oxide, more preferably one or more of alpha-phase nanometer aluminum oxide of self-gram new material limited company and alpha-phase nanometer aluminum oxide of constant nano new material limited company; and/or the number of the groups of groups,
the piezochromic indicator is selected from conventional indicators in the prior art, and is preferably one or more of 2-phenylamino-3-methyl-6-dibutylamino fluoran of Shanghai Ruiyan fine chemical Co., ltd, 7-diethylamino-3- [4' - (trifluoromethyl) benzoyl ] methylcoumarin of Sichuan foreigner biotechnology Co., ltd; and/or the number of the groups of groups,
the wetting dispersant is selected from conventional dispersants in the prior art, preferably one or more of AFCONA4015, BYK103 and RD 9125; and/or the number of the groups of groups,
the flexible curing agent is selected from conventional curing agents in the prior art, preferably one or more of polyurea curing agents and polyisocyanate curing agents in the invention, more preferably one or more of GB805A-100 and E402-90T; and/or the number of the groups of groups,
the adhesion promoter is selected from conventional promoters in the prior art, and is preferably one or more of amino modified silicon compounds, more preferably one or more of JSC-1120 of the courtesy model 1121 and the Jewelry model.
The component A can be added with any one of conventional fillers or auxiliary agents in the field, such as fumed silica, flatting agents, defoamers, solvents B and the like, and the dosage of the conventional fillers or auxiliary agents is also conventional, and the components are preferably calculated by taking 100 parts by weight of flexible resin in the invention,
1.5 to 5 parts by weight of fumed silica; preferably 2 to 4 parts by weight;
1-5 parts by weight of a leveling agent; preferably 2 to 4 parts by weight;
1-5 parts of defoaming agent; preferably 2 to 3 parts by weight;
30-80 parts by weight of a solvent B; preferably 40 to 60 parts by weight.
The fumed silica is selected from conventional fumed silica in the prior art, preferably having a specific surface area of 50-300m 2 At least one of hydrophobic fumed silica/g, more preferably one or more of HB-151 from Hubei Hui nanotechnology Co., ltd., SJ-301 from Weifang Sanjia chemical Co., ltd; fumed silica mainly plays a role in preventing sedimentation; and/or the number of the groups of groups,
the leveling agent is selected from conventional leveling agents in the prior art in the field, and is preferably selected from one or more of BYK-378 and Levaslip 466; and/or the number of the groups of groups,
the defoamer is selected from conventional defoamers in the prior art, and is preferably one or more of BYK065 and AFCONA 2020; and/or the number of the groups of groups,
the solvent B is selected from conventional solvents in the prior art, and is preferably one or more of ethyl acetate, butyl acetate and propylene glycol methyl ether acetate, wherein the water content is less than or equal to 0.2%.
The second object of the invention is to provide a preparation method of the flexible pressure-sensitive color-changing anti-corrosive primer, which comprises the following steps:
and mixing the component A and the component B respectively, and then mixing the component A and the component B to obtain the flexible pressure-sensitive color-changing anti-corrosion primer.
The invention adopts the following specific technical scheme:
(1) Stirring flexible resin, superfine talcum powder, nano aluminum oxide, wetting dispersant, optional fumed silica, optional solvent B, optional leveling agent and optional defoaming agent for 0.5-1.5 h in sequence in a container, grinding and dispersing by a sand mill until the fineness is less than or equal to 40 mu m, adding a piezochromic indicator, stirring at a high speed in a closed manner for 0.5-1.5 h, filtering, discharging, and sealing and packaging to obtain a flexible pressure-sensitive color-changing anti-corrosive primer A component;
(2) Sealing and stirring the flexible curing agent and the adhesion promoter for 0.5-1 h in a container, filtering and discharging, and sealing and packaging to obtain a component B of the flexible pressure-sensitive color-changing anti-corrosion primer;
(3) And mixing the component A and the component B to obtain the flexible pressure-sensitive color-changing anti-corrosion primer.
The invention also provides the application of the flexible pressure-sensitive color-changing anticorrosive primer which is one of the purposes of the invention or is prepared by the method of the second purpose of the invention in threaded fasteners, rivets, joints and fatigue key parts.
It is a fourth object of the present invention to provide a visual tightening intelligent threaded fastener which is a screw, or comprises a bolt and a nut and optionally a washer, the screw or bolt being coated on its outer layer with a flexible pressure sensitive color changing anticorrosive primer as one of the objects of the present invention or a flexible pressure sensitive color changing anticorrosive primer prepared by the method of the second object of the present invention.
In a preferred embodiment of the present invention,
the bolt comprises a bolt head and a bolt column, wherein the bolt head is positioned at the upper part of the bolt column, an annular groove is formed in the end face of the bolt head, and the center of the annular groove is positioned on the axis of the bolt column; the annular groove is used for filling the flexible pressure-sensitive color-changing anti-corrosion primer so as to display the fastening degree; preferably, the method comprises the steps of,
the annular groove penetrates into the bolt column part, and the depth of the annular groove penetrating into the bolt column part is preferably 1/8-1/4 of the length of the bolt column; and/or the width of the annular groove is 1-2 mm; and/or the number of the groups of groups,
the annular groove is filled with a coating of the flexible pressure-sensitive color-changing anti-corrosive primer; and/or the number of the groups of groups,
the outer diameter of the annular groove is smaller than the diameter of the bolt column, preferably 0.8-3mm smaller than the diameter of the bolt column; and/or the number of the groups of groups,
the ratio of the inner diameter of the annular groove to the diameter of the bolt column is 0.25-0.5.
In a preferred embodiment of the present invention,
the screw comprises a screw head and a screw rod, wherein the screw head is positioned at the upper part of the screw rod, an annular groove is formed in the end face of the screw head, and the center of the annular groove is positioned on the axis of the screw rod; preferably, the method comprises the steps of,
the depth of the annular groove penetrating into the screw part is preferably 1/8-1/4 of the length of the screw; and/or the width of the annular groove is 1-2 mm; and/or the number of the groups of groups,
the annular groove is filled with a coating of the flexible pressure-sensitive color-changing anti-corrosive primer; and/or the number of the groups of groups,
the outer diameter of the annular groove is smaller than the diameter of the screw rod, preferably 0.8-3mm smaller than the diameter of the screw rod; and/or the number of the groups of groups,
the ratio of the inner diameter of the annular groove to the diameter of the screw rod is 0.25-0.5.
The material of the threaded fastener can be selected from metals common in the field, and aluminum alloy is preferred.
The bolt may be obtained by forming an annular groove by ring cutting a circle on the end face of the bolt head from a bolt comprising a bolt head and a bolt stud as is conventional in the art.
The screw may be obtained by forming an annular groove by ring cutting the end face of the screw head into a circle, which is conventional in the prior art and comprises a screw head and a screw shaft.
In a preferred embodiment of the present invention,
the preparation method of the threaded fastener with visible fastening degree comprises the step of spraying the flexible pressure-sensitive color-changing anti-corrosion primer on the surface of the threaded fastener and then curing.
The invention adopts the following specific technical scheme:
the preparation method of the intelligent threaded fastener with visual fastening degree preferably comprises the following steps:
1) And (3) cutting the end face of the bolt head of the bolt around the central point to form an annular groove, then putting the treated bolt into dimethylbenzene for soaking for 4-6 hours, taking out and airing.
2) Spraying the flexible pressure-sensitive color-changing anti-corrosion primer on the bolts treated in the step 1, filling the annular grooves with the flexible pressure-sensitive color-changing anti-corrosion primer, and curing completely.
The nuts and/or gaskets matched with the bolts are preferably placed into dimethylbenzene to be soaked for 4-6 hours, taken out and dried, and then sprayed with flexible pressure-sensitive color-changing anti-corrosion primer, and the cured product is used.
The nut and the gasket can be any nut and gasket in the prior art, and can be matched with the bolt of the invention in size.
According to the invention, a certain pressure is applied to the flexible pressure-sensitive color-changing anti-corrosion primer in the groove through the fastening screw or the bolt, and when the pressure is enough, the paint changes color, so that the fastening degree of the screw or the bolt is enough.
The beneficial effects of the invention are as follows:
the flexible pressure-sensitive color-changing anti-corrosion primer disclosed by the invention is simple in preparation method, has a good coating pot life, can be suitable for traditional air spraying, has good pressure-sensitive color-changing property, anti-corrosion property and environmental suitability, and can well solve the micro corrosion problems of threaded fasteners, rivets, joints and fatigue key parts. By observing the color change of the threaded fastener with visual fastening degree (if the paint does not change color, the fastening degree is low, if the paint changes color, the paint reaches a certain pressure, and the fastening is basically fastened), whether the threaded fastener meets the fastening requirement can be quickly and conveniently found, so that the loss caused by the fastening problem is reduced, and the cost of manual detection is reduced.
Drawings
FIG. 1 is a schematic top view of a bolt in an intelligent threaded fastener with visual fastening, wherein 1 is a bolt post, 2 is an annular groove, and 3 is a bolt head;
fig. 2 is a schematic front view of a bolt in an intelligent threaded fastener with visual fastening, wherein 1 is a bolt post, 2 is an annular groove, and 3 is a bolt head.
Detailed Description
The present invention will be described in detail with reference to the following specific embodiments and the accompanying drawings, and it is necessary to point out that the following embodiments are merely for further explanation of the present invention and should not be construed as limiting the scope of the present invention, and some insubstantial modifications and adaptations of the invention based on the present disclosure will remain within the scope of the invention.
The starting materials used in the examples were all conventional commercially available.
Example 1
The preparation method of the flexible polyisocyanate prepolymer resin in the present embodiment includes the steps of:
step 1: 30 parts by weight of hexamethylene diisocyanate, 0.01 part by weight of triethylamine and 15 parts by weight of butyl acetate are added into a reaction kettle, nitrogen is introduced for protection, stirring is carried out for 20min at 150r/min at 25 ℃ to ensure that the materials are uniformly mixed, and then the temperature is increased to 60 ℃ to react for 15min to obtain a material 1.
Step 2: to the material 1, 0.12 parts by weight of Stabaxol-1 was added, heated to 78℃and 1.2 parts by weight of TMP was slowly added under 180r/min stirring, and reacted at 85℃for 1.5 hours after the addition was completed, to obtain a material 2.
Step 3: to the material 2, 45 parts by weight of polycaprolactone diol PCL2053 of the company Wohan's Biotechnology Co was slowly added at 78℃under 180r/min stirring, reacted at 85℃for 2.5 hours, and then cooled to 45℃to obtain a material 3.
Step 4: slowly adding 0.02 part by weight of benzoyl chloride into the material 3 under the condition of stirring at 45 ℃ and 150r/min, carrying out heat preservation reaction at 40 ℃ for 1.5 hours after the addition, adding 8 parts by weight of butyl acetate after the reaction is finished, cooling to below 40 ℃, discharging, and sealing and packaging to obtain the flexible polyisocyanate prepolymer resin.
The formula composition and the preparation process of the flexible pressure-sensitive color-changing anti-corrosion primer in the embodiment are as follows:
(1) Sequentially adding 45 parts by weight of butyl acetate solvent, 100 parts by weight of the obtained flexible polyisocyanate prepolymer resin, 35 parts by weight of Guangxi osmanthus 1250-mesh superfine talcum powder, 40 parts by weight of alpha-phase nanometer aluminum oxide (model PAT-05A) of Baoket New Material Co., ltd.), 3.5 parts by weight of fumed silica SJ-301, 2.5 parts by weight of BYK-378 flatting agent, 2.5 parts by weight of BYK065 defoamer and 3.5 parts by weight of AFCONA4015 wetting dispersant into a container, stirring for 1h, grinding and dispersing by a sand mill until the fineness is less than or equal to 40 mu m, adding 150 parts by weight of 2-phenylamino-3-methyl-6-dibutylamino fluoran, sealing and stirring for 0.5h at a high speed, filtering and discharging, and sealing and packaging to obtain a component A; the solid content of the component A is 63 percent, and the fineness is 35 mu m;
(2) Sealing and stirring 100 parts by weight of GB805A-100 flexible curing agent and 5.5 parts by weight of the pretty dry 1121 adhesion promoter for 0.5h in a container, filtering and discharging, and sealing and packaging to obtain a component B;
(3) The A component and the B component prepared by the method are prepared into a coating material according to the weight ratio of A to B=80 to 10, and the thickness of the coating for performance test obtained after coating is 40-60 microns.
The preparation method of the intelligent threaded fastener with visible fastening degree comprises the following steps:
1) And (3) cutting the end face of the bolt head of the outer hexagonal aluminum alloy bolt (the total length is 3cm, the bolt head is 4mm, the bolt diameter is 6mm, the length of the hexagonal butt edge is 8 mm) around the central point in a circle to form an annular groove, the depth of the annular groove is 8mm, the width of the annular groove is 1mm, the inner diameter of the annular groove is 2mm, and then putting the processed bolt and a nut and a gasket matched with the processed bolt into dimethylbenzene for 5h, taking out and airing.
2) Firstly mixing the component A and the component B of the flexible pressure-sensitive color-changing anti-corrosion primer of the embodiment 1 according to the dosage ratio (80:10) to obtain the flexible pressure-sensitive color-changing anti-corrosion primer, then respectively spraying the flexible pressure-sensitive color-changing anti-corrosion primer on the bolts, the nuts and the gaskets treated in the step 1), filling the annular grooves with the coating, and curing to obtain the intelligent threaded fastener with visible fastening degree.
Example 2
The preparation method of the flexible polyisocyanate prepolymer resin in the present embodiment includes the steps of:
step 1: 38 parts by weight of terephthalyl diisocyanate, 0.01 part by weight of dioctyl tin dilaurate and 18 parts by weight of ethyl acetate are added into a reaction kettle, nitrogen is introduced for protection, stirring is carried out for 20min at 150r/min at 25 ℃ to ensure that the materials are uniformly mixed, and then the temperature is raised to 63 ℃ for reaction for 15min to obtain a material 1.
Step 2: to the material 1, 0.12 parts by weight of Stabaxol-1 was added, heated to 78℃and 1.0 part by weight of TMP was slowly added under 180r/min stirring, and reacted at 85℃for 1.5 hours after the addition was completed, to obtain a material 2.
Step 3: to the material 2, 43 parts by weight of polycaprolactone diol PCL2053 of the company Wohol Biotechnology Co., ltd was slowly added at 78℃under stirring at 180r/min, reacted at 85℃for 2.5 hours, and then cooled to 45℃to obtain a material 3.
Step 4: slowly adding 0.01 part by weight of benzoyl chloride into the material 3 under the condition of stirring at 45 ℃ and 150r/min, carrying out heat preservation reaction at 45 ℃ for 1.5 hours after the addition, adding 10 parts by weight of ethyl acetate after the reaction is finished, cooling to below 40 ℃, discharging, and sealing and packaging to obtain the flexible polyisocyanate prepolymer resin.
The formula composition and the preparation process of the flexible pressure-sensitive color-changing anti-corrosion primer in the embodiment are as follows:
(1) Sequentially adding 50 parts by weight of ethyl acetate solvent, 100 parts by weight of the obtained flexible polyisocyanate prepolymer resin, 40 parts by weight of Qingdao white pigeon 1500 mesh superfine talcum powder, 35 parts by weight of alpha-phase nanometer aluminum oxide (model HN-L100260) of Hengna New Material Co., ltd.), 3.8 parts by weight of fumed silica SJ-301, 2.2 parts by weight of Levaslip 466 flatting agent, 2.3 parts by weight of AFCONA2020 defoamer and 3.8 parts by weight of BYK103 wetting dispersant into a container, stirring for 1.2 hours, grinding and dispersing by a sand mill until the fineness is less than or equal to 40 mu m, adding 160 parts by weight of 7-diethylamino-3- [4' - (trifluoromethyl) benzoyl ] methylcoumarin, sealing and stirring at a high speed for 0.8 hours, filtering, discharging, and sealing and packaging to obtain a component A; the solid content of the component A is 65 percent, and the fineness is 35 mu m;
(2) Sealing and stirring 100 parts by weight of E402-90T flexible curing agent and 5.2 parts by weight of jercard JSC-1120 adhesion promoter for 0.5h in a container, filtering and discharging, and sealing and packaging to obtain a component B;
(3) The A component and the B component prepared by the method are prepared into a coating material according to the weight ratio of A to B=80 to 12, and the thickness of the coating for performance test obtained after coating is 40-60 microns.
The preparation method of the intelligent threaded fastener with visible fastening degree comprises the following steps:
1) And (3) cutting the end face of the bolt head of the outer hexagonal aluminum alloy bolt (the total length is 3cm, the bolt head is 4mm, the bolt diameter is 6mm, the length of the hexagonal butt edge is 8 mm) around the central point in a circle to form an annular groove, the depth of the annular groove is 8mm, the width of the annular groove is 1mm, the inner diameter of the annular groove is 2mm, and then putting the processed bolt and a nut and a gasket matched with the processed bolt into dimethylbenzene for 5h, taking out and airing.
2) Firstly mixing the component A and the component B of the flexible pressure-sensitive color-changing anti-corrosion primer of the embodiment 2 according to the dosage ratio (80:12) to obtain the flexible pressure-sensitive color-changing anti-corrosion primer, then respectively spraying the flexible pressure-sensitive color-changing anti-corrosion primer on the bolts, the nuts and the gaskets treated in the step 1), filling the annular grooves with the coating, and curing to obtain the intelligent threaded fastener with visible fastening degree.
Example 3
The preparation method of the flexible polyisocyanate prepolymer resin in the present embodiment includes the steps of:
step 1: 42 parts by weight of isophorone diisocyanate, 0.01 part by weight of dioctyl tin dilaurate, 12 parts by weight of ethyl acetate and 5 parts by weight of propylene glycol methyl ether acetate are added into a reaction kettle, nitrogen is introduced for protection, 150r/min is stirred for 15min at 25 ℃ to uniformly mix the materials, and the temperature is raised to 65 ℃ to react for 20min to obtain a material 1.
Step 2: to the material 1, 0.10 parts by weight of Stabaxol-1 was added, heated to 78℃and 1.2 parts by weight of DMTDA was slowly added under 180r/min stirring, and reacted at 85℃for 1.5 hours after the addition, to obtain a material 2.
Step 3: 48 parts by weight of polyether polyol EP330N of Lanxingdong chemical industry Co., ltd.) is slowly added into the material 2 at 78 ℃ under the stirring condition of 180r/min, reacted for 2.5 hours at 85 ℃, and then cooled to 45 ℃ to obtain the material 3.
Step 4: slowly adding 0.01 part by weight of benzoyl chloride into the material 3 under the condition of stirring at 45 ℃ and 150r/min, carrying out heat preservation reaction at 45 ℃ for 1.5 hours after the addition, adding 12 parts by weight of ethyl acetate after the reaction is finished, cooling to below 40 ℃, discharging, and sealing and packaging to obtain the flexible polyisocyanate prepolymer resin.
The formula composition and the preparation process of the flexible pressure-sensitive color-changing anti-corrosion primer in the embodiment are as follows:
(1) Sequentially adding 20 parts by weight of butyl acetate solvent, 20 parts by weight of propylene glycol methyl ether acetate solvent, 100 parts by weight of the obtained flexible polyisocyanate prepolymer resin, 38 parts by weight of Guangxi osmanthus 1250-mesh superfine talcum powder, 40 parts by weight of alpha-phase nanometer aluminum oxide (model PAT-05A) of Baozhi New materials limited company, 3.2 parts by weight of fumed silica HB-151, 2.6 parts by weight of BYK-378 flatting agent, 2.5 parts by weight of AFCONA2020 defoamer and 3.4 parts by weight of RD9125 wetting dispersant into a container, stirring for 1h, grinding and dispersing by a sand mill until the fineness is less than or equal to 40 mu m, adding 160 parts by weight of 7-diethylamino-3- [4' - (trifluoromethyl) benzoyl ] methylcoumarin, sealing and stirring at a high speed for 0.5h, filtering, discharging, and sealing and packaging to obtain a component A; the solid content of the component A is 63 percent, and the fineness is 35 mu m;
(2) Sealing and stirring 100 parts by weight of GB805A-100 flexible curing agent and 4.5 parts by weight of Jewelch JSC-1120 adhesion promoter for 0.5h in a container, filtering and discharging, and sealing and packaging to obtain a component B;
(3) The A component and the B component prepared by the method are prepared into a coating material according to the weight ratio of A to B=80 to 14, and the thickness of the coating for performance test obtained after coating is 40-60 microns.
The preparation method of the intelligent threaded fastener with visible fastening degree comprises the following steps:
1) And (3) cutting the end face of the bolt head of the outer hexagonal aluminum alloy bolt (the total length is 3cm, the bolt head is 4mm, the bolt diameter is 6mm, the length of the hexagonal butt edge is 8 mm) around the central point in a circle to form an annular groove, the depth of the annular groove is 8mm, the width of the annular groove is 1mm, the inner diameter of the annular groove is 2mm, and then putting the processed bolt and a nut and a gasket matched with the processed bolt into dimethylbenzene for 5h, taking out and airing.
2) Firstly mixing the component A and the component B of the flexible pressure-sensitive color-changing anti-corrosion primer of the embodiment 3 according to the dosage ratio (80:14) to obtain the flexible pressure-sensitive color-changing anti-corrosion primer, then respectively spraying the flexible pressure-sensitive color-changing anti-corrosion primer on the bolts, the nuts and the gaskets treated in the step 1), filling the annular grooves with the coating, and curing to obtain the intelligent threaded fastener with visible fastening degree.
Comparative example 1
The flexible polyisocyanate prepolymer resin in this comparative example was prepared in the same manner as in example 1.
The formulation composition and preparation process of the primer in this comparative example are as follows:
(1) 45 parts by weight of butyl acetate solvent, 100 parts by weight of the obtained flexible polyisocyanate prepolymer resin, 35 parts by weight of Guangxi osmanthus 1250-mesh superfine talcum powder, 40 parts by weight of alpha-phase nanometer aluminum oxide (model PAT-05A) of Baoket New Material Co., ltd.), 3.5 parts by weight of fumed silica SJ-301, 2.5 parts by weight of BYK-378 flatting agent, 2.5 parts by weight of BYK065 defoamer and 3.5 parts by weight of AFCONA4015 wetting dispersant are sequentially added into a container, stirred for 1h, ground and dispersed by a sand mill until the fineness is less than or equal to 40 mu m, 150 parts by weight of titanium dioxide is added, sealed high-speed stirring is carried out for 0.5h, filtered discharging is carried out, and the component A is obtained by sealing and packaging. The solid content of the component A is 63 percent, and the fineness is 35 mu m;
(2) Sealing and stirring 100 parts by weight of GB805A-100 flexible curing agent and 5.5 parts by weight of the pretty dry 1121 adhesion promoter for 0.5h in a container, filtering and discharging, and sealing and packaging to obtain a component B;
(3) The A component and the B component prepared by the method are prepared into a coating material according to the weight ratio of A to B=80 to 10, and the thickness of the coating for performance test obtained after coating is 40-60 microns.
The preparation method of the threaded fastener of the comparative example comprises the following steps:
1) And (3) cutting the end face of the bolt head of the outer hexagonal aluminum alloy bolt (the total length is 3cm, the bolt head is 4mm, the bolt diameter is 6mm, the length of the hexagonal butt edge is 8 mm) around the central point in a circle to form an annular groove, the depth of the annular groove is 8mm, the width of the annular groove is 1mm, the inner diameter of the annular groove is 2mm, and then putting the processed bolt and a nut and a gasket matched with the processed bolt into dimethylbenzene for 5h, taking out and airing.
2) Mixing the component A and the component B according to the dosage ratio (80:10) to obtain a primer, spraying the primer on the bolts, the nuts and the gaskets treated in the step 1), filling the annular grooves with the coating, and curing to obtain the threaded fastener coated with the primer.
Comparative example 2
The flexible polyisocyanate prepolymer resin in this comparative example was prepared in the same manner as in example 3.
The formulation composition and preparation process of the primer in this comparative example are as follows:
(1) Sequentially adding 20 parts by weight of butyl acetate solvent, 20 parts by weight of propylene glycol methyl ether acetate solvent, 100 parts by weight of flexible polyisocyanate prepolymer resin, 38 parts by weight of Guangxi sweet osmanthus 1250-mesh superfine talcum powder, 40 parts by weight of alpha-phase nanometer aluminum oxide (model PAT-05A) of Baoket New Material Co., ltd., 3.2 parts by weight of fumed silica HB-151, 2.6 parts by weight of BYK-378 flatting agent, 2.5 parts by weight of AFCONA2020 defoamer and 3.4 parts by weight of RD9125 wetting dispersant into a container, stirring for 1h, grinding and dispersing by a sand mill until the fineness is less than or equal to 40 mu m, adding 160 parts by weight of 7-diethylamino-3- [4' - (trifluoromethyl) benzoyl ] methylcoumarin, sealing and stirring at a high speed for 0.5h, filtering, discharging, and sealing and packaging to obtain a component A; the solid content of the component A is 63 percent, and the fineness is 35 mu m;
(2) Sealing and stirring 100 parts by weight of GB805A-100 flexible curing agent for 0.5h in a container, filtering and discharging, and sealing and packaging to obtain a component B;
(3) The A component and the B component prepared by the method are prepared into a coating material according to the weight ratio of A to B=80 to 14, and the thickness of the coating for performance test obtained after coating is 40-60 microns.
The preparation method of the threaded fastener of the comparative example comprises the following steps:
1) And (3) cutting the end face of the bolt head of the outer hexagonal aluminum alloy bolt (the total length is 3cm, the bolt head is 4mm, the bolt diameter is 6mm, the length of the hexagonal butt edge is 8 mm) around the central point in a circle to form an annular groove, the depth of the annular groove is 8mm, the width of the annular groove is 1mm, the inner diameter of the annular groove is 2mm, and then putting the processed bolt and a nut and a gasket matched with the processed bolt into dimethylbenzene for 5h, taking out and airing.
2) Mixing the component A and the component B according to the dosage ratio (80:14) to obtain a primer, spraying the primer on the bolts, the nuts and the gaskets treated in the step 1), filling the annular grooves with the coating, and curing to obtain the threaded fastener coated with the primer.
Comparative example 3
The flexible polyisocyanate prepolymer resin in this comparative example was prepared in the same manner as in example 3.
The formula composition and the preparation process of the flexible pressure-sensitive color-changing anti-corrosion primer in the comparative example are as follows:
(1) Sequentially adding 20 parts by weight of butyl acetate solvent, 20 parts by weight of propylene glycol methyl ether acetate solvent, 100 parts by weight of flexible polyisocyanate prepolymer resin, 78 parts by weight of Guangxi sweet osmanthus 1250-mesh superfine talcum powder, 3.2 parts by weight of fumed silica HB-151, 2.6 parts by weight of BYK-378 flatting agent, 2.5 parts by weight of AFCONA2020 defoamer and 3.4 parts by weight of RD9125 wetting dispersant into a container, stirring for 1h, grinding and dispersing by a sand mill until the fineness is less than or equal to 40 mu m, adding 160 parts by weight of 7-diethylamino-3- [4' - (trifluoromethyl) benzoyl ] methylcoumarin, sealing and stirring for 0.5h at a high speed, filtering, discharging, and sealing and packaging to obtain a component A; the solid content of the component A is 63 percent, and the fineness is 35 mu m;
(2) Sealing and stirring 100 parts by weight of GB805A-100 flexible curing agent and 4.5 parts by weight of Jewelch JSC-1120 adhesion promoter for 0.5h in a container, filtering and discharging, and sealing and packaging to obtain a component B;
(3) The A component and the B component prepared by the method are prepared into a coating material according to the weight ratio of A to B=80 to 14, and the thickness of the coating for performance test obtained after coating is 40-60 microns.
The preparation method of the threaded fastener of the comparative example comprises the following steps:
1) And (3) cutting the end face of the bolt head of the outer hexagonal aluminum alloy bolt (the total length is 3cm, the bolt head is 4mm, the bolt diameter is 6mm, the length of the hexagonal butt edge is 8 mm) around the central point in a circle to form an annular groove, the depth of the annular groove is 8mm, the width of the annular groove is 1mm, the inner diameter of the annular groove is 2mm, and then putting the processed bolt and a nut and a gasket matched with the processed bolt into dimethylbenzene for 5h, taking out and airing.
2) Mixing the component A and the component B according to the dosage ratio (80:14) to obtain a primer, spraying the primer on the bolts, the nuts and the gaskets treated in the step 1), filling the annular grooves with the coating, and curing to obtain the threaded fastener coated with the primer.
Comparative example 4
The flexible polyisocyanate prepolymer resin in this comparative example was prepared in the same manner as in example 3.
The formula composition and the preparation process of the flexible pressure-sensitive color-changing anti-corrosion primer in the comparative example are as follows:
(1) Sequentially adding 20 parts by weight of butyl acetate solvent, 20 parts by weight of propylene glycol methyl ether acetate solvent, 100 parts by weight of the obtained flexible polyisocyanate prepolymer resin, 78 parts by weight of alpha-phase nano aluminum oxide (model PAT-05A) of Baote New Material Co., ltd.), 3.2 parts by weight of fumed silica HB-151, 2.6 parts by K-378 flatting agent, 2.5 parts by weight of AFCONA2020 defoamer and 3.4 parts by weight of RD9125 wetting dispersant, stirring for 1h, grinding and dispersing by a sand mill until the fineness is less than or equal to 40 mu m, adding 160 parts by weight of 7-diethylamino-3- [4' - (trifluoromethyl) benzoyl ] methylcoumarin, sealing and stirring for 0.5h at a high speed, filtering and discharging, and sealing and packaging to obtain a component A; the solid content of the component A is 63 percent, and the fineness is 35 mu m;
(2) Sealing and stirring 100 parts by weight of GB805A-100 flexible curing agent and 4.5 parts by weight of Jewelch JSC-1120 adhesion promoter for 0.5h in a container, filtering and discharging, and sealing and packaging to obtain a component B;
(3) The A component and the B component prepared by the method are prepared into a coating material according to the weight ratio of A to B=80 to 14, and the thickness of the coating for performance test obtained after coating is 40-60 microns.
The preparation method of the threaded fastener of the comparative example comprises the following steps:
1) And (3) cutting the end face of the bolt head of the outer hexagonal aluminum alloy bolt (the total length is 3cm, the bolt head is 4mm, the bolt diameter is 6mm, the length of the hexagonal butt edge is 8 mm) around the central point in a circle to form an annular groove, the depth of the annular groove is 8mm, the width of the annular groove is 1mm, the inner diameter of the annular groove is 2mm, and then putting the processed bolt and a nut and a gasket matched with the processed bolt into dimethylbenzene for 5h, taking out and airing.
2) Mixing the component A and the component B according to the dosage ratio (80:14) to obtain a primer, spraying the primer on the bolts, the nuts and the gaskets treated in the step 1), filling the annular grooves with the coating, and curing to obtain the threaded fastener coated with the primer.
TABLE 1 Main Performance index of the flexible pressure sensitive color-changing anticorrosive primer prepared in examples 1 to 3 and comparative examples 1 to 4
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As can be seen from the above table, the coatings of examples 1 to 3 all have good tensile strength and elongation at break, good tearing strength and good bending resistance, and have excellent neutral salt spray resistance, good acid salt spray resistance, excellent humidity resistance and other environmental suitability, and especially, the neutral salt spray test of the painting X method shows that the flexible pressure-sensitive color-changing anti-corrosion primer has good anti-corrosion performance, the appearance of a paint film is smooth, no bubbles or particles exist, the intelligent threaded fastener can realize fastening color change, and the fastening degree of a bolt can be indicated to a certain extent. Examples 1 to 3 were not significantly different from comparative example 1 in terms of tensile strength, elongation at break, bending resistance, acid salt spray resistance, neutral salt spray resistance, etc., but the fastening bolt of comparative example 1 did not give an indication; examples 1 to 3 were not greatly different from comparative example 2 in other properties, but since comparative example 2 was not added with an adhesion promoter, comparative example 2 was inferior to examples 1 to 3 in properties such as adhesion, water resistance, bending resistance, neutral salt spray resistance, acid salt spray resistance, and heat and humidity resistance; example 3 has no great difference in other properties from comparative example 3, but since nano aluminum oxide is not added in comparative example 3, pencil hardness can only reach HB level. Example 3 has no great difference in other properties from comparative example 4, but the pencil hardness reaches only H-grade since no ultra fine talc was added in comparative example 4. In conclusion, the flexible pressure-sensitive color-changing anti-corrosive primer disclosed by the invention can show good tensile strength and elongation at break, good tearing strength, good bending resistance, excellent neutral salt mist resistance, good acid salt mist resistance, excellent damp-heat resistance and other environmental suitability; the coating system has higher pencil hardness index through the synergistic effect of the superfine talcum powder and the nano aluminum oxide.
Claims (10)
1. A flexible pressure-sensitive color-changing anti-corrosion primer comprises a component A and a component B; the component A comprises flexible resin, a piezochromic indicator, superfine talcum powder, nano aluminum oxide and a wetting dispersant; the component B comprises a flexible curing agent and an adhesion promoter.
2. The flexible pressure sensitive color-changing corrosion resistant primer of claim 1, wherein:
each component in the component A is calculated by taking flexible resin as 100 parts by weight,
100-180 parts by weight of a piezochromic indicator; preferably 120 to 170 parts by weight;
20-80 parts of superfine talcum powder; preferably 30 to 50 parts by weight;
30-80 parts by weight of nano aluminum oxide; preferably 30 to 50 parts by weight;
2-5 parts by weight of wetting dispersant; preferably 2 to 4 parts by weight;
each component in the component B takes a flexible curing agent as 100 parts by weight,
0-10 parts by weight of adhesion promoter; preferably 2 to 10 parts by weight;
the dosage ratio of the component A to the component B is (4-12): 1, preferably (4 to 10): 1.
3. the flexible pressure sensitive color-changing corrosion resistant primer of claim 1, wherein:
the flexible resin is at least one selected from flexible epoxy modified acrylic resin and flexible polyisocyanate prepolymer resin; preferably, the method comprises the steps of,
the preparation method of the flexible polyisocyanate prepolymer resin comprises the following steps:
step 1: reacting isocyanate, a catalyst and part of solvent A to obtain a material 1;
step 2: adding a stabilizer and a cross-linking agent into the material 1 to react to obtain a material 2;
step 3: adding oligomer polyol into the material 2 to react to obtain a material 3;
step 4: adding a coagulant into the material 3 for reaction, and adding the residual solvent A after the reaction is finished to obtain flexible polyisocyanate prepolymer resin;
it is further preferred that the composition comprises,
the isocyanate is selected from one or more of isophorone diisocyanate, hexamethylene diisocyanate, 4' -dicyclohexylmethane diisocyanate and terephthalyl diisocyanate, preferably isophorone diisocyanate and/or terephthalyl diisocyanate; and/or the number of the groups of groups,
the catalyst is selected from one or more of triethylamine and dioctyltin dilaurate; and/or the number of the groups of groups,
the oligomer polyol is selected from one or more of polycaprolactone diol, polyether polyol and polybutadiene polyol; and/or the number of the groups of groups,
the anti-coagulant is selected from one or more of benzoyl chloride and phosphoric acid; and/or the number of the groups of groups,
the solvent A is one or more selected from butyl acetate, ethyl acetate and propylene glycol methyl ether acetate.
4. The flexible pressure sensitive color-changing corrosion resistant primer of claim 1, wherein:
the fineness of the superfine talcum powder is 500-2000 meshes, preferably 1250-2000 meshes; and/or the number of the groups of groups,
the grain diameter of the nano aluminum oxide is 5-500 nm, preferably 10-100 nm; and/or the number of the groups of groups,
the piezochromic indicator is selected from one or two of 2-phenylamino-3-methyl-6-dibutylamino fluoran and 7-diethylamino-3- [4' - (trifluoromethyl) benzoyl ] methylcoumarin.
5. The flexible pressure sensitive color-changing corrosion resistant primer according to any one of claims 1-4, wherein:
the component A also comprises any one of fumed silica, a leveling agent, a defoaming agent and a solvent B.
6. A method of preparing the flexible pressure sensitive color-changing corrosion resistant primer of any of claims 1-5, comprising:
and mixing the component A and the component B respectively, and then mixing the component A and the component B to obtain the flexible pressure-sensitive color-changing anti-corrosion primer.
7. Use of a flexible pressure sensitive color-changing corrosion resistant primer as defined in any one of claims 1 to 5 or prepared by the method of claim 6 in threaded fasteners, rivets, joints and fatigue critical locations.
8. An intelligent threaded fastener with visual fastening degree, wherein the fastener is a screw or comprises a bolt, a nut and optionally a gasket, and the outer layer of the screw or the bolt is coated with the flexible pressure-sensitive color-changing anti-corrosion primer according to any one of claims 1 to 5 or the flexible pressure-sensitive color-changing anti-corrosion primer prepared by the method according to claim 6.
9. The visual fastening level intelligent threaded fastener according to claim 8, wherein:
the bolt comprises a bolt head and a bolt column, wherein the bolt head is positioned at the upper part of the bolt column, an annular groove is formed in the end face of the bolt head, and the center of the annular groove is positioned on the axis of the bolt column; preferably, the method comprises the steps of,
the annular groove penetrates into the bolt column part, and the depth of the annular groove penetrating into the bolt column part is preferably 1/8-1/4 of the length of the bolt column; and/or the width of the annular groove is 1-2 mm; and/or the number of the groups of groups,
the annular groove is filled with a coating of the flexible pressure-sensitive color-changing anti-corrosive primer.
10. The visual fastening level intelligent threaded fastener according to claim 8, wherein:
the screw comprises a screw head and a screw rod, wherein the screw head is positioned at the upper part of the screw rod, an annular groove is formed in the end face of the screw head, and the center of the annular groove is positioned on the axis of the screw rod; preferably, the method comprises the steps of,
the depth of the annular groove penetrating into the screw part is preferably 1/8-1/4 of the length of the screw; and/or the width of the annular groove is 1-2 mm; and/or the number of the groups of groups,
the annular groove is filled with a coating of the flexible pressure-sensitive color-changing anti-corrosive primer.
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