CN114539885B - Special high-permeability moisture-curing seal primer for concrete and preparation method and application thereof - Google Patents
Special high-permeability moisture-curing seal primer for concrete and preparation method and application thereof Download PDFInfo
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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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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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
- 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
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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
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- 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
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The invention discloses a special high-permeability moisture curing seal primer for concrete and a preparation method and application thereof. The special high-permeability moisture curing seal primer for concrete comprises a component A and a component B; the component A comprises quaternary ammonium salt modified epoxy resin, graphene, basalt flakes, silver-loaded zirconium phosphate, a wetting dispersant, a grafting coupling agent, an anti-settling agent, an active diluent, a pigment and filler, butanol and xylene; the component B comprises phenolic amine, phenolic amide, graphene, basalt flakes, a wetting dispersant, an anti-settling agent, a pigment filler, butanol and xylene. The special high-permeability moisture curing seal primer for concrete provided by the invention is green and environment-friendly, has low requirement on surface treatment of a matrix, can be cured in a moisture way, can realize single-coating thickening, and can be used for surface protection of concrete matrixes in severe environments such as marine environments.
Description
Technical Field
The invention belongs to the technical field of concrete surface protection, and particularly relates to a special high-permeability moisture curing seal primer for concrete, and a preparation method and application thereof.
Background
With the continuous development and utilization of marine resources by human beings, the marine engineering construction industry such as harbor buildings, marine tunnels, sea-crossing bridges, seashore dams and the like keeps a fast growth rate, the large-scale infrastructures are basically of reinforced concrete structures, are mostly undetachable and immovable, are exposed to the C-5 marine atmospheric environment with the highest corrosion level in the ISO 12944-2 atmospheric environment corrosivity classification all year round, have high salinity and humidity and are influenced by rising and falling tides, the concrete structure is very easy to deteriorate and destroy, the durability of the concrete structure is seriously influenced, and the application of the concrete anticorrosive paint is the simplest, effective and economic protection measure. At present, the concrete surface is mostly treated by high-pressure (pressure is not less than 20MPa) fresh water, sand blasting or manual polishing and the like, the concrete surface in a tidal range and a splash range is basically cleaned by the high-pressure fresh water, the traditional anticorrosive paint can not simultaneously meet the requirements of high infiltration, moisture curing (tidal range and splash range) on a concrete substrate under high solid content, and the performance requirements of heavy corrosion resistance are considered, and various defects or single performance exist, for example, a penetration crosslinking type concrete protective paint and a preparation method thereof are disclosed in a patent CN105110815A, a penetration type anticorrosive paint for concrete protection is disclosed in a patent CN 110484082A, a water-based transparent concrete waterproof mildew-proof carbonization-proof paint and a preparation method thereof are disclosed in a patent CN111234670A, the above disclosed concrete protective paint is a single-component water-based paint, and the penetration performance and the wet surface coating performance of the above can meet the requirements, however, the corrosion resistance of the water-based coating is general, and the water-based coating cannot be suitable for corrosion protection in severe environments such as marine atmospheric environment (C5). Patent CN103224742A discloses a permeable transparent concrete protective coating and a preparation method thereof, wherein the concrete protective coating is transparent fluorocarbon varnish, the VOC content of the coating is high, the coating does not meet the environmental protection requirement, moreover, no shielding functional material is added in the coating, a compact coating can not be formed, the requirement of chlorine ion permeability resistance under the marine atmospheric environment can not be met, and wet coating can not be realized.
Therefore, research and development of the high-solid-content moisture-cured sealing primer which can realize high penetration to the concrete base material are significant for corrosion protection of concrete structure engineering in the severe environment of C5.
Disclosure of Invention
The invention mainly aims to provide a special high-permeability moisture curing seal primer for concrete and a preparation method and application thereof, so as to overcome the defects of the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a special high-permeability moisture curing seal primer for concrete, which comprises a component A and a component B;
wherein the component A comprises the following components in parts by weight: 30.0-50.0 parts of quaternary ammonium salt modified epoxy resin, 0.2-1.5 parts of graphene, 4.5-12.0 parts of basalt flakes, 0.1-2.0 parts of silver-loaded zirconium phosphate, 0.1-1.5 parts of wetting dispersant, 0.5-3.5 parts of grafting coupling agent, 0.1-2.0 parts of anti-settling agent, 1.0-5.0 parts of active diluent, 10.0-35.0 parts of pigment and filler, 1.0-10.0 parts of butanol and 5.0-25.0 parts of xylene;
the component B comprises the following components in parts by weight: 10.0-30.0 parts of phenolic aldehyde amine, 10.0-30.0 parts of phenolic aldehyde amide, 0.5-1.5 parts of graphene, 7.0-17.0 parts of basalt flake, 0.5-2.0 parts of wetting dispersant, 0.8-4.8 parts of anti-settling agent, 20.0-30.0 parts of pigment and filler, 2.0-6.7 parts of butanol and 9.0-18.0 parts of dimethylbenzene.
The embodiment of the invention also provides a preparation method of the special high-permeability moisture curing seal primer for concrete, which comprises the following steps:
mixing quaternary ammonium salt modified epoxy resin, butanol and xylene, sequentially adding a wetting dispersant, a grafting coupling agent, an anti-settling agent, an active diluent, graphene, silver-loaded zirconium phosphate and basalt flakes, mixing, stirring and dispersing, then adding a pigment and a filler, mixing and adjusting the viscosity of the obtained mixture to form a component A;
mixing phenolic aldehyde amine, a phenolic aldehyde amide curing agent, butanol and xylene, sequentially adding a wetting dispersant, an anti-settling agent, graphene and basalt flakes, mixing, stirring and dispersing, adding a pigment and a filler, mixing and adjusting the viscosity of the obtained mixture to form a component B;
and mixing the component A and the component B, and curing to obtain the special high-permeability moisture curing seal primer for concrete.
The embodiment of the invention also provides a special protective coating for concrete, which is formed by the special high-permeability moisture curing seal primer for concrete.
The embodiment of the invention also provides application of the special high-permeability moisture curing seal primer for concrete or the special protective coating for concrete in the field of concrete structure engineering in the severe environment of C5.
Compared with the prior art, the invention has the beneficial effects that: the special high-permeability moisture curing seal primer for concrete provided by the invention is green and environment-friendly, has low requirements on surface treatment of a matrix, can be firmly attached only by removing loose gravel, green moss stains and the like, and reduces the difficulty of surface treatment; the paint can be cured in a moist manner, can be constructed on the moist surface of a substrate with water, can be immediately contacted with water after film forming, and can realize underwater curing, so that the paint requirement of a surface wet area can be met; in addition, the coating can realize single-time coating and thickening, the obtained coating has the advantages of compact structure and reduction of corrosion medium permeation, and can be used for surface protection of concrete substrates in severe environments such as marine environment and the like.
Detailed Description
In view of the defects of the prior art, the inventor of the present invention has long studied and largely practiced to provide the technical solutions of the present invention, which will be clearly and completely described below. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Specifically, as one aspect of the technical scheme of the invention, the special high-permeability moisture curing seal primer for concrete comprises a component A and a component B;
wherein the component A comprises the following components in parts by weight: 30.0-50.0 parts of quaternary ammonium salt modified epoxy resin, 0.2-1.5 parts of graphene, 4.5-12.0 parts of basalt flakes, 0.1-2.0 parts of silver-loaded zirconium phosphate, 0.1-1.5 parts of wetting dispersant, 0.5-3.5 parts of grafting coupling agent, 0.1-2.0 parts of anti-settling agent, 1.0-5.0 parts of active diluent, 10.0-35.0 parts of pigment and filler, 1.0-10.0 parts of butanol and 5.0-25.0 parts of xylene;
the component B comprises the following components in parts by weight: 10.0-30.0 parts of phenolic aldehyde amine, 10.0-30.0 parts of phenolic aldehyde amide, 0.5-1.5 parts of graphene, 7.0-17.0 parts of basalt flake, 0.5-2.0 parts of wetting dispersant, 0.8-4.8 parts of anti-settling agent, 20.0-30.0 parts of pigment and filler, 2.0-6.7 parts of butanol and 9.0-18.0 parts of xylene.
In some preferred embodiments, the quaternary ammonium salt modified epoxy resin is prepared by reacting dimethylamino ethyl acrylate quaternary ammonium salt, benzoyl peroxide and epoxy resin.
Further, the epoxy resin includes a bisphenol a epoxy resin, and is not limited thereto.
Still further, the epoxy resin includes E51 epoxy resin, and is not limited thereto.
In some preferred embodiments, the mass ratio of the component A to the component B is 5-1: 1.
In some preferred embodiments, the graphene has a thickness of 0.3 to 2.0nm, a sheet diameter of 5.0 to 10.0 μm, and a specific surface area of 100 to 500m 2 /g。
Further, the graphene may be FLGA-01 by garifen nanotechnology, inc.
In some preferred embodiments, the basalt scales have a thickness of 1 to 7 μm and a plate diameter of 10 to 5 mm.
Further, the basalt flakes may be produced by chendtai navigation new materials technologies ltd.
In some preferred embodiments, the pigment and filler includes any one or a combination of two or more of titanium dioxide, carbon black, iron oxide red, barium sulfate, mica powder, talcum powder, silica powder, feldspar powder and zinc phosphate, and is not limited thereto.
In some preferred embodiments, the anti-settling agent includes any one or a combination of two or more of fumed silica, organic bentonite, and polyamide wax powder, and is not limited thereto.
In some preferred embodiments, the graft coupling agent comprises any one or a combination of two or more of KH550, KH560, Adherant 1051, Adherant 1121, KBM-403, and KBM-603, without limitation thereto.
Further, the graft coupling agent can be any one of south Beijing eosino KH550/KH560, Haimaiches Adherant 1051/1121, and Xinyue KBM-403/KBM-603.
In some preferred embodiments, the wetting and dispersing agent includes any one or a combination of two or more of ANTI-tera-U, DISPERBYK-110, Disponer904S, Disponer923S, RG-5150, RG-5172, and is not limited thereto.
Further, the wetting and dispersing agent can be any one of Bicke chemical ANTI-TERRA-U/DISPERBYK-110, Haimax Disponer904S/923S, Changzhou Rongguan RG-5150/RG-5172.
In some preferred embodiments, the reactive diluent is an aliphatic glycidyl ether epoxy reactive diluent, which includes any one or a combination of two or more of cadles NC-513, shanghai friendship 6360, jiangsu sammu SM-60, and is not limited thereto.
In some preferred embodiments, the silver content of the silver-loaded zirconium phosphate is 6.0 ± 1.0 wt%.
In some preferred embodiments, the phenalkamine includes any one or a combination of two or more of cadilenx 2040, NX2041, LITE 2001, dow d.e.h.85, holy T-31, and is not limited thereto.
In some preferred embodiments, the phenolic amide cadrillite 3060, LITE 3100, LITE-3005, any one or combination of two or more thereof, and is not limited thereto.
In another aspect of the embodiments of the present invention, there is provided a method for preparing the special high-infiltration type moisture-curing sealer for concrete, including:
mixing quaternary ammonium salt modified epoxy resin, butanol and xylene, sequentially adding a wetting dispersant, a grafting coupling agent, an anti-settling agent, an active diluent, graphene, silver-loaded zirconium phosphate and basalt flakes, mixing, stirring and dispersing, then adding a pigment and a filler, mixing and adjusting the viscosity of the obtained mixture to form a component A;
mixing phenolic aldehyde amine, a phenolic aldehyde amide curing agent, butanol and xylene, sequentially adding a wetting dispersant, an anti-settling agent, graphene and basalt flakes, mixing, stirring and dispersing, adding a pigment and a filler, mixing and adjusting the viscosity of the obtained mixture to form a component B;
and mixing the component A and the component B, and curing to obtain the special high-permeability moisture curing seal primer for concrete.
In some preferred embodiments, the method for preparing the quaternary ammonium salt-modified epoxy resin comprises:
(1) mixing ethanol, n-butanol, xylene, dimethylaminoethyl acrylate quaternary ammonium salt and benzoyl peroxide, and stirring and mixing at room temperature to form a first mixture;
(2) mixing n-butanol, xylene and epoxy resin, adding the first mixture at 80 ℃, and then continuously reacting for 2.5 hours to obtain quaternary ammonium salt modified epoxy resin;
further, the weight portion ratio of the ethanol, the n-butanol, the xylene, the dimethylaminoethyl acrylate quaternary ammonium salt and the benzoyl peroxide in the step (1) is 0-10:20-40:50-70:10-20: 5-15.
Further, the weight portion ratio of the n-butanol, the xylene and the epoxy resin in the step (2) is 20-40:50-60: 400-600.
In some more specific embodiments, the method for preparing the quaternary ammonium salt-modified epoxy resin may include:
s1, adding 0-10 parts of ethanol, 20-40 parts of n-butanol, 50-70 parts of xylene, 10-20 parts of dimethylaminoethyl acrylate quaternary ammonium salt and 5-15 parts of Benzoyl Peroxide (BPO) into a stirring pot, stirring at 2000r/min at room temperature until the materials are completely dissolved, standing for confirmation, and taking out for later use.
S2, adding 20-40 parts of n-butyl alcohol, 50-60 parts of xylene and 400-600 parts of E51 epoxy resin into a stirring pot, maintaining the rotating speed at 2000r/min, setting the water bath at 80 +/-2 ℃ for constant temperature, firstly heating to 80 ℃ and adjusting the stirring speed to 4000r/min, then dripping the mixture of S1 into the stirring pot at the speed of 5 drops/min, paying attention to the exothermic reaction, closely paying attention to the temperature and viscosity change in the stirring pot to prevent the viscosity from rising too fast to cause implosion, adjusting the rotating speed to 2000r/min after S1 is completely dripped, continuing to keep the water bath at the constant temperature for 2.5h, and standing to obtain the quaternary ammonium salt modified epoxy resin for later use.
In some preferred embodiments, the smear-4 cup viscosity of the A component is from 30 to 90 s.
Further, the coating-4 cup viscosity of the component A is 50-70 s.
In some preferred embodiments, the smear-4 cup viscosity of the B component is from 30 to 90 s.
Further, the coating-4 cup viscosity of the component B is 50-70 s.
In some preferred embodiments, the coating-4 cup viscosity of the special high-permeability moisture curing seal primer for concrete obtained after the component A and the component B are mixed is 30-90 s.
Further, the coating-4 cup viscosity of the special high-permeability moisture curing seal primer for concrete obtained by mixing the component A and the component B is 50-70 s.
In some preferred embodiments, the concrete specific high penetration moisture curing seal primer has a solid content above 65 wt%.
In some more specific embodiments, the method for preparing the concrete-specific high-infiltration moisture-curing primer sealer comprises the following steps:
adding quaternary ammonium salt modified epoxy resin, butanol and xylene into a material mixing pot, dispersing at a high speed of 2000-4000 r/min for 5min under a stirrer, sequentially adding a wetting dispersant, a grafting coupling agent, an anti-settling agent, an active diluent, graphene, silver-loaded zirconium phosphate and basalt flakes, continuously dispersing at a high speed for 30min while keeping the same rotating speed, then adding a pigment and a filler, continuously dispersing at a high speed for 15min, grinding until the fineness is qualified, adjusting the viscosity of the obtained mixture by using xylene, cooling to room temperature, filtering and packaging to obtain a component A;
adding phenolic aldehyde amine, a phenolic amide curing agent, butanol and xylene into a material mixing pot, dispersing at a high speed of 2000-4000 r/min for 5min under a stirrer, sequentially adding a wetting dispersant, an anti-settling agent, graphene and basalt flakes, continuing to disperse at a high speed for 30min at the same rotating speed, then adding a pigment and a filler, continuing to disperse at a high speed for 15min, grinding until the fineness is qualified, adjusting the viscosity of the obtained mixture by using xylene, cooling to room temperature, filtering and packaging to obtain a component B;
the component A and the component B are mixed and prepared according to the equivalent principle of epoxy and active hydrogen and the mass ratio of 5-1: 1, high-speed rotation stirring and dispersion are adopted, the rotating speed is 500-1000 r/min, the dispersion time is 5-10 min, and the components are uniformly stirred and cured for 15min and then coated.
In another aspect of the embodiment of the invention, a special protective coating for concrete is further provided, and the special protective coating for concrete is formed by the special high-permeability moisture curing seal primer for concrete.
Further, the dry film thickness of the concrete special protective coating formed by coating the concrete special high-permeability moisture curing seal primer for one time is more than 200 mu m, and the penetration depth is more than 3.0 mm.
The special high-permeability moisture curing seal primer for concrete is coated on the surface of a concrete substrate, the permeability and the hydrophilicity in a concrete capillary structure are enhanced by the side chain of the quaternary ammonium acrylate, meanwhile, the water pulled from the hydrophilic structure is extruded outwards by the hydrophobicity of the main chain epoxy structure, the moisture curing and low-temperature curing characteristics of the coating are realized by curing with the phenol aldehyde amine and the phenol aldehyde amide, and the rapid permeability and curing are realized under the action of the silane grafted coupling agent, water, pigment and filler and the concrete hydroxyl to form Si-O-Si chemical bonds. During the infiltration process, the nano silver loaded by the nano silver-loaded zirconium phosphate (Ag-ZrP) and the chloride ions which are already infiltrated in the deep capillary of the concrete can generate stable silver chloride, so that the in-situ fixation of the chloride ions is realized, and the corrosion hazard is not generated any more. More importantly, the enhanced antibacterial function is realized through the synergistic effect of the quaternary ammonium salt and the silver-loaded zirconium phosphate. And secondly, under the catalytic action of silver-loaded zirconium phosphate, active groups on the components such as quaternary ammonium salt modified epoxy resin, a curing agent, a coupling agent and the like are subjected to accelerated reaction with active groups such as carboxyl, hydroxyl, epoxy bond and the like on graphene, so that a more compact shielding network is formed. Therefore, the organic coating is finally formed after crosslinking and curing, and has the functions of reinforcing and corrosion protection on the concrete layer.
Further, the coating mode is not limited, and includes spraying, rolling and brushing, and preferably adopts an airless spraying mode.
The invention adopts the sealing primer formed by mixing two components in proportion, wherein the sealing primer comprises quaternary ammonium salt modified epoxy resin, nano-grade graphene, micron-grade basalt flakes, silver-loaded zirconium phosphate, phenolic aldehyde amine and phenolic amide curing agent, the contents of the components are controlled, and the sealing primer has the following remarkable effects:
(1) according to the invention, quaternary ammonium acrylate is introduced to a bisphenol A epoxy resin main chain in a side chain free radical polymerization manner to form a special structure with a side chain hydrophilic main chain hydrophobic, so that the coating has the epoxy resin anticorrosion property, the permeability and the hydrophilicity in a concrete capillary structure are enhanced by the side chain, and simultaneously, the water pulled from the hydrophilic structure is extruded outwards by the hydrophobicity of the main chain to form rapid penetration and solidification.
(2) In the invention, nano silver-loaded zirconium phosphate (Ag-ZrP) is added, and the nano silver-loaded zirconium phosphate is an inorganic antibacterial agent prepared by using layered zirconium phosphate as a carrier, using various metal ions such as silver, zinc and the like as antibacterial ions and various auxiliaries. When the nano silver chloride is used in the coating, on one hand, the nano silver can play a role in sterilization, and meanwhile, the loaded nano silver and chloride ions which have penetrated from the capillary deep part of concrete generate stable silver chloride, so that the in-situ fixation of the chloride ions is realized, and the corrosion hazard is not generated any more.
(3) In the seal primer composition, the quaternary ammonium salt modified epoxy resin and the silver-loaded zirconium phosphate can respectively play the inherent roles, and the synergistic effect of the quaternary ammonium salt and the silver-loaded zirconium phosphate can enhance the antibacterial function, and the catalytic effect of the silver-loaded zirconium phosphate can accelerate the reaction of active groups on components such as the modified epoxy resin quaternary ammonium salt group, a curing agent, a coupling agent and the like and active groups such as carboxyl, hydroxyl, epoxy bonds and the like on graphene, so that a more compact shielding layer is formed, and the chloride ion permeability resistance of the coating is improved.
(4) According to the invention, the phenolic aldehyde amine and phenolic aldehyde amide curing agents are compounds prepared by performing Mannich reaction on cardanol, formaldehyde, characteristic amine and the like extracted from cashew nut shell oil, have various advantages of the Mannich curing agents, can realize rapid and low-temperature curing (below 0 ℃), and have the advantages of good chemical resistance, no blushing during high-humidity surface curing and the like. Due to the special long aliphatic side chain of cardanol, the phenolic aldehyde amine and the phenolic amide curing agent also have the advantages of long operation period, good toughness, low surface treatment requirement, excellent water resistance, excellent salt water resistance and the like. In addition, the phenolic aldehyde amine and the phenolic aldehyde amide curing agent have the characteristic of stronger hydrophobicity, and provide a plurality of advantages for the coating formula. The water sensitivity of phenolic hydroxyl and other formula components can be mutually offset, so that the damage probability of a resin bonding protective layer is reduced, better adhesive force can be shown on the surface of a base material which is processed poorly or is wet, and the corrosion resistance is improved.
(5) According to the invention, two-dimensional structure functional materials comprising nanoscale graphene, micron-sized basalt flakes and the like are adopted to perform grafting reaction with organic resin in a fully wet state, and after dispersion, the nanoscale graphene and the micron-sized basalt flakes are compounded with each other and uniformly dispersed in a resin system to form a compact labyrinth effect with a filler, so that the coating structure is compact, and the chloride ion permeability resistance is greatly improved. In addition, the added inorganic pigment and filler has high inertia and low water content, the deformation is small during crosslinking and curing, the residual stress of the coating after curing is small, and the heavy-duty anticorrosion performance of the coating is enhanced.
(6) In the invention, the solid content of the mixed A component and B component is not less than 65%, the VOC content is not more than 420g/L, and the mixed A component and B component do not contain heavy metal ions, so that the environment-friendly concept is better met, and the thickness of a dry film coated on the surface of a base material for one time reaches more than 200 mu m, so that the combination of a sealing primer and a primer can be realized, the construction number is reduced, and the construction efficiency is improved.
In another aspect of the embodiment of the present invention, the application of the aforementioned special high-infiltration type moisture-cured sealer for concrete or the special protective coating for concrete in the field of concrete structure engineering under the severe environment of C5 is further provided.
The technical solution of the present invention is further described in detail with reference to several preferred embodiments, which are implemented on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given, but the scope of the present invention is not limited to the following embodiments.
The experimental materials used in the examples used below were all available from conventional biochemical reagents companies, unless otherwise specified.
The quaternary ammonium salt modified epoxy resin in the following embodiment is prepared from dimethylaminoethyl acrylate quaternary ammonium salt, Benzoyl Peroxide (BPO), epoxy resin and a solvent, and specifically comprises the following components:
s1, adding 10 parts of ethanol, 30 parts of n-butanol, 60 parts of xylene, 15 parts of dimethylaminoethyl acrylate quaternary ammonium salt and 10 parts of Benzoyl Peroxide (BPO) into a material mixing pot, stirring at the rotating speed of 2000r/min at room temperature until the materials are completely dissolved, standing for confirmation, and taking out for later use.
S2, adding 30 parts of n-butyl alcohol, 70 parts of xylene and 500 parts of E51 epoxy resin into a stirring pot, maintaining the rotating speed at 2000r/min, setting a water bath at 80 +/-2 ℃ for constant temperature, firstly heating to 80 ℃ and adjusting the stirring speed to 4000r/min, then uniformly dripping the mixture of S1 into the stirring pot at the speed of 5 drops/min, paying attention to the fact that the reaction is exothermic, paying close attention to the temperature and viscosity change in the stirring pot to prevent the viscosity from rising too fast to cause implosion, adjusting the rotating speed to 2000r/min after all drops of S1 are dripped, continuing to keep the water bath at the constant temperature for 2.5h, and standing to obtain the quaternary ammonium salt modified epoxy resin for later use.
Example 1
The special high-permeability moisture curing seal primer for concrete in the embodiment comprises a component A and a component B, wherein the component A is prepared from the following components in parts by weight of 100: adding 30.0 parts of quaternary ammonium salt modified epoxy resin, 6.0 parts of butanol and 5.0 parts of xylene into a material mixing pot, stirring at the speed of 3000r/min for 5min, sequentially adding 1.5 parts of ANTI-TERRA-U dispersing agent, 0.5 part of KH560 coupling agent, 2.0 parts of polyamide wax ANTI-settling agent, 5.0 parts of NC-513 active diluent, 2.0 parts of silver-loaded zirconium phosphate, 1.0 part of graphene and 12.0 parts of basalt scale while stirring, continuously stirring at the same rotating speed for 30min, continuously adding 10.0 parts of iron oxide red, 8.0 parts of silica micropowder, 9.0 parts of mica powder and 8.0 parts of zinc phosphate, continuously stirring at the same rotating speed for 15min, grinding by a sand mill until the fineness is less than or equal to 80 mu m, adjusting the viscosity to a coating-4 cup viscosity for 60s by using xylene, cooling to room temperature, filtering and packaging to obtain the component A.
The component B is prepared from the following components in parts by weight of 100 parts by weight: adding 30.0 parts of NX-2041 curing agent, 10.0 parts of LITE 3100 curing agent, 4.7 parts of butanol and 18.0 parts of xylene into a stirring pot, stirring at the speed of 3000r/min for 5min, sequentially adding 2.0 parts of ANTI-TERRA-U dispersing agent, 2.8 parts of polyamide wax ANTI-settling agent, 0.5 part of graphene and 7.0 parts of basalt flake, continuously dispersing at the same rotating speed for 30min, then adding 25.0 parts of mica powder, continuously dispersing at high speed for 15min, grinding by a sand mill until the fineness is less than or equal to 80 mu m, adjusting the viscosity to 60s of coating-4 cups by using xylene, cooling to room temperature, filtering and packaging to obtain the component B.
Uniformly mixing the component A and the component B according to the mass ratio of 5: 1, and coating the mixture on the surface of a substrate to form a film so as to obtain the thick paste type wet cured graphene composite basalt flake sealing primer coating.
Example 2
The special high-permeability moisture curing seal primer for concrete in the embodiment comprises a component A and a component B, wherein the component A is prepared from the following components in parts by weight of 100: 39.7 parts of quaternary ammonium salt modified epoxy resin, 10.0 parts of butanol and 25.0 parts of xylene are added into a material mixing pot and stirred for 5min at the speed of 3000r/min, 0.8 part of ANTI-TERRA-U dispersant, 3.5 parts of KH560 coupling agent, 1.0 part of polyamide wax ANTI-settling agent, 3.0 parts of NC-513 active diluent, 1.0 part of silver-loaded zirconium phosphate, 1.5 parts of graphene and 4.5 parts of basalt scale are sequentially added while stirring, stirring is continued for 30min at the same rotating speed, then 3.0 parts of iron oxide red, 2.0 parts of silica micropowder, 3.0 parts of mica powder and 2.0 parts of zinc phosphate are continuously added, stirring is continued for 15min at the same rotating speed, grinding is carried out by a sand mill until the fineness is less than or equal to 80 mu m, the viscosity is adjusted to the coating-4 cup viscosity for 30s by xylene, and after cooling to the room temperature, the component A is obtained by filtering and packaging.
The component B is prepared from the following components in parts by weight of 100 parts by weight: adding 20.0 parts of NX-2041 curing agent, 20.0 parts of LITE 3100 curing agent, 2.0 parts of butanol and 9.0 parts of xylene into a stirring pot, stirring at the speed of 3000r/min for 5min, sequentially adding 1.2 parts of ANTI-TERRA-U dispersing agent, 4.8 parts of polyamide wax ANTI-settling agent, 1.0 parts of graphene and 12.0 parts of basalt flake, continuously dispersing at the same rotating speed for 30min, then adding 30.0 parts of mica powder, continuously dispersing at high speed for 15min, grinding by a sand mill until the fineness is less than or equal to 80 mu m, adjusting the viscosity to 90s in a coating-4 cup by using xylene, cooling to room temperature, filtering and packaging to obtain a component B.
Uniformly mixing the component A and the component B according to the mass ratio of 3: 1, and coating the mixture on the surface of a substrate to form a film so as to obtain the thick paste type wet cured graphene composite basalt flake sealing primer coating.
Example 3
The special high-permeability moisture curing seal primer for concrete in the embodiment comprises a component A and a component B, wherein the component A is prepared from the following components in parts by weight of 100: adding 50.0 parts of quaternary ammonium salt modified epoxy resin, 1.0 part of butanol and 15.0 parts of xylene into a material mixing pot, stirring at the speed of 3000r/min for 5min, sequentially adding 0.1 part of ANTI-TERRA-U dispersant, 2.0 parts of KH560 coupling agent, 0.1 part of polyamide wax ANTI-settling agent, 1.0 part of NC-513 active diluent, 0.1 part of silver-loaded zirconium phosphate, 0.2 part of graphene and 8.5 parts of basalt scale while stirring, continuously stirring at the same rotating speed for 30min, continuously adding 6.0 parts of iron oxide red, 5.0 parts of silicon micropowder, 6.0 parts of mica powder and 5.0 parts of zinc phosphate, continuously stirring at the same rotating speed for 15min, grinding by a sand mill until the fineness is less than or equal to 80 mu m, adjusting the viscosity to 90s of coating-4 cup viscosity by xylene, cooling to room temperature, filtering and packaging to obtain the component A.
The component B is prepared from the following components in parts by weight of 100 parts by weight: 10.0 parts of NX-2041 curing agent, 30.0 parts of LITE 3100 curing agent, 6.7 parts of butanol and 13.5 parts of xylene are taken to be added into a stirring pot to be stirred for 5min at the speed of 3000r/min, 0.5 part of ANTI-TERRA-U dispersing agent, 0.8 part of polyamide wax ANTI-settling agent, 1.5 parts of graphene and 17.0 parts of basalt flake are sequentially added, high-speed dispersion is continuously carried out for 30min under the same rotating speed, 20.0 parts of mica powder are added to be continuously dispersed for 15min under the high speed, the mixture is ground by a sand mill until the fineness is less than or equal to 80 mu m, the viscosity is adjusted to the coating-4 cup viscosity for 30s by xylene, and after the mixture is cooled to the room temperature, the mixture is filtered and packaged to obtain the component B.
Uniformly mixing the component A and the component B according to the mass ratio of 1:1, and coating the mixture on the surface of a substrate to form a film so as to obtain the thick paste type wet cured graphene composite basalt flake sealing primer coating.
Example 4
The special high-permeability moisture curing seal primer for concrete in the embodiment comprises a component A and a component B, wherein the component A is prepared from the following components in parts by weight of 100: adding 50.0 parts of quaternary ammonium salt modified epoxy resin, 1.0 part of butanol and 15.0 parts of xylene into a material mixing pot, stirring for 5min at the speed of 3000r/min, sequentially adding 0.1 part of DISPERBYK-110 dispersant, 2.0 parts of KBM-403 coupling agent, 0.1 part of fumed silica, 1.0 part of Jiangsu Sanmu SM-60 active diluent, 0.1 part of silver-loaded zirconium phosphate, 0.2 part of graphene and 8.5 parts of basalt scale while stirring, continuously stirring for 30min at the same rotating speed, continuously adding 6.0 parts of iron oxide red, 5.0 parts of silicon micropowder, 6.0 parts of mica powder and 5.0 parts of zinc phosphate, continuously stirring for 15min at the same rotating speed, grinding to the fineness of less than or equal to 80 mu m by a sand mill, adjusting the viscosity to a coating-4 cup viscosity for 50s by xylene, cooling to room temperature, filtering and packaging to obtain the component A.
The component B is prepared from the following components in parts by weight of 100 parts by weight: adding 10.0 parts of NX-2041 curing agent, 30.0 parts of LITE 3100 curing agent, 6.7 parts of butanol and 13.5 parts of xylene into a stirring pot, stirring at the speed of 3000r/min for 5min, sequentially adding 0.5 part of ANTI-TERRA-U dispersing agent, 0.8 part of polyamide wax ANTI-settling agent, 1.5 parts of graphene and 17.0 parts of basalt flake, continuously dispersing at the same rotating speed for 30min, then adding 20.0 parts of mica powder, continuously dispersing at high speed for 15min, grinding by a sand mill until the fineness is less than or equal to 80 mu m, adjusting the viscosity to 50s of coating-4 cups by using xylene, cooling to room temperature, filtering and packaging to obtain the component B.
Uniformly mixing the component A and the component B according to the mass ratio of 5: 1, and coating the mixture on the surface of a substrate to form a film so as to obtain the thick paste type wet cured graphene composite basalt flake sealing primer coating.
Comparative example 1
The comparative example 1 and the example 1 adopt the same formula parts and preparation method, and the difference is that silver zirconium phosphate is not added, and the part which is not added is replaced by the pigment and filler silicon micro powder.
Comparative example 2
Comparative example 2 uses the same formulation parts and preparation method as example 2, except that the quaternary ammonium salt modified epoxy resin is replaced by the common E51 bisphenol A epoxy resin in equal parts.
Comparative example 3
Comparative example 3 and example 3 adopt the same formula parts and preparation method, except that phenolic amine and phenolic amide curing agents are replaced by common 650 and 651 polyamide curing agents in equal parts.
Comparative example 4
The comparative example 4 and the example 4 adopt the same formula parts and preparation method, and are different in that graphene and basalt flakes are not added, and the pigment filler silica powder is not added for replacement.
Test experiments:
selecting corresponding test substrates according to test items, adopting a Q235 steel plate for drying time, salt water resistance and chemical resistance, adopting concrete samples for other items, coating various plates once, adopting air spraying for the test, and controlling the thickness of a dry film to be 200 +/-10 mu m. According to the design standard of the durability of a concrete structure, the concrete test piece has a serious action grade under the environment of ocean chloride, the design service life is 100 years, and the strength grade of the concrete is C45. The test results are shown in table 1:
TABLE 1 Performance test results for coatings of examples 1-3 and comparative examples 1-4
As can be seen from comparison between examples 1 to 3 and comparative examples 1 to 4, the selection of the silver-loaded zirconium phosphate, the epoxy resin, the curing agent and the two-dimensional structure material plays a very critical role in the performance of the product, and the proportion of the resin, the curing agent, the two-dimensional structure material, the functional filler and the like determines the crosslinking density and the corrosion resistance of the coating.
In addition, the inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
It should be understood that the technical solution of the present invention is not limited to the above-mentioned specific embodiments, and all technical modifications made according to the technical solution of the present invention fall within the protection scope of the present invention without departing from the spirit of the present invention and the protection scope of the claims.
Claims (9)
1. A special high-permeability moisture curing seal primer for concrete is characterized by comprising a component A and a component B;
wherein the component A comprises the following components in parts by weight: 30.0-50.0 parts of quaternary ammonium salt modified epoxy resin, 0.2-1.5 parts of graphene, 4.5-12.0 parts of basalt flakes, 0.1-2.0 parts of silver-loaded zirconium phosphate, 0.1-1.5 parts of wetting dispersant, 0.5-3.5 parts of grafting coupling agent, 0.1-2.0 parts of anti-settling agent, 1.0-5.0 parts of active diluent, 10.0-35.0 parts of pigment and filler, 1.0-10.0 parts of butanol and 5.0-25.0 parts of xylene;
the component B comprises the following components in parts by weight: 10.0-30.0 parts of phenolic aldehyde amine, 10.0-30.0 parts of phenolic aldehyde amide, 0.5-1.5 parts of graphene, 7.0-17.0 parts of basalt flake, 0.5-2.0 parts of wetting dispersant, 0.8-4.8 parts of anti-settling agent, 20.0-30.0 parts of pigment and filler, 2.0-6.7 parts of butanol and 9.0-18.0 parts of xylene;
the preparation method of the quaternary ammonium salt modified epoxy resin comprises the following steps:
(1) mixing ethanol, n-butanol, xylene, dimethylaminoethyl acrylate quaternary ammonium salt and benzoyl peroxide, and stirring and mixing at room temperature to form a first mixture;
(2) mixing n-butanol, xylene and epoxy resin, adding the first mixture at 80 ℃, and then continuously reacting for 2.5 hours to obtain quaternary ammonium salt modified epoxy resin;
in the step (1), the weight ratio of the ethanol, the n-butanol, the xylene, the dimethylaminoethyl acrylate quaternary ammonium salt to the benzoyl peroxide is 0-10:20-40:50-70:10-20: 5-15;
in the step (2), the weight ratio of the n-butanol to the xylene to the epoxy resin is 20-40:50-60: 400-600.
2. The special high-permeability moisture-curing seal primer for concrete according to claim 1, which is characterized in that: the epoxy resin is selected from bisphenol A epoxy resin.
3. The special high-permeability moisture-curable sealer primer for concrete according to claim 1, wherein: the mass ratio of the component A to the component B is 5-1: 1.
4. The special high-permeability moisture-curing seal primer for concrete according to claim 1, which is characterized in that: the thickness of the graphene is 0.3-2.0 nm, the sheet diameter is 5.0-10.0 mu m, and the specific surface area is 100-500 m 2 /g；
The thickness of the basalt scales is 1-7 mu m, and the size of the scale diameter is 10-5 mm;
the pigment and filler comprises any one or the combination of more than two of titanium dioxide, carbon black, iron oxide red, barium sulfate, mica powder, talcum powder, silica powder, feldspar powder and zinc phosphate;
the anti-settling agent is selected from any one or the combination of more than two of fumed silica, organic bentonite and polyamide wax powder;
the grafting coupling agent is selected from any one or the combination of more than two of KH550, KH560, Adherant 1051, Adherant 1121, KBM-403 and KBM-603;
the wetting dispersant is selected from any one or the combination of more than two of ANTI-TERRA-U, DISPERBYK-110, Disponer904S, Disponer923S, RG-5150 and RG-5172;
the reactive diluent is aliphatic glycidyl ether epoxy reactive diluent;
the silver content in the silver-loaded zirconium phosphate is 6.0 +/-1.0 wt%.
5. The special high-permeability moisture-curing seal primer for concrete according to claim 1, which is characterized in that: the phenolic aldehyde amine is selected from one or more of Kadelian NX2040, NX2041, LITE 2001, Dow D.E.H.85 and holy T-31;
the phenolic amide is selected from any one or combination of more than two of cadrillite 3060, LITE 3100 and LITE-3005.
6. The preparation method of the special high-infiltration type moisture curing seal primer for concrete of any one of claims 1 to 5 is characterized by comprising the following steps:
mixing quaternary ammonium salt modified epoxy resin, butanol and xylene, sequentially adding a wetting dispersant, a grafting coupling agent, an anti-settling agent, an active diluent, graphene, silver-loaded zirconium phosphate and basalt flakes, mixing, stirring and dispersing, then adding a pigment and a filler, mixing and adjusting the viscosity of the obtained mixture to form a component A;
mixing phenolic aldehyde amine, a phenolic aldehyde amide curing agent, butanol and xylene, sequentially adding a wetting dispersant, an anti-settling agent, graphene and basalt flakes, mixing, stirring and dispersing, adding a pigment and a filler, mixing and adjusting the viscosity of the obtained mixture to form a component B;
and mixing the component A and the component B, and curing to obtain the special high-permeability moisture curing seal primer for concrete.
7. The method of claim 6, wherein: the coating-4 cup viscosity of the component A is 30-90 s;
the coating-4 cup viscosity of the component B is 30-90 s;
the coating-4 cup viscosity of the special high-permeability moisture curing seal primer for concrete obtained by mixing the component A and the component B is 30-90 s;
the solid content of the special high-permeability moisture curing seal primer for concrete is more than 65 wt%.
8. The special protective coating for concrete is characterized in that: the concrete-specific protective coating is formed from the concrete-specific high-penetration moisture-curable sealer primer of any one of claims 1-5; the dry film thickness of the concrete special protective coating formed by coating the concrete special high-permeability moisture curing seal primer for one time is more than 200 mu m, and the penetration depth is more than 3.0 mm.
9. Use of the special high-infiltration type moisture-curing seal primer for concrete as defined in any one of claims 1 to 5 or the special protective coating for concrete as defined in claim 8 in the field of concrete structure engineering under the severe environment of C5.
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