CN113321987B - High-tolerance epoxy primer for water-jet rust removal surface and preparation method and application thereof - Google Patents

High-tolerance epoxy primer for water-jet rust removal surface and preparation method and application thereof Download PDF

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CN113321987B
CN113321987B CN202110740540.3A CN202110740540A CN113321987B CN 113321987 B CN113321987 B CN 113321987B CN 202110740540 A CN202110740540 A CN 202110740540A CN 113321987 B CN113321987 B CN 113321987B
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epoxy resin
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epoxy
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CN113321987A (en
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赵祥龙
张阳波
邬宵宵
王书传
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XINHE NEW MATERIAL CO Ltd
Xinhe New Material Suzhou Co ltd
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Xinhe New Material Suzhou Co ltd
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    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
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Abstract

The invention discloses a high-tolerance epoxy primer for a water-jet rust removal surface, and a preparation method and application thereof. The high-tolerance epoxy primer comprises a first component and a second component, wherein the first component comprises modified epoxy resin, a rheological additive, a dispersing agent, a filler, an antirust pigment, an antifoaming agent, a graphene dispersion liquid, a solvent and the like, and the second component comprises amine resin, micromolecule epoxy resin, a catalyst and the like. The high-tolerance epoxy primer disclosed by the invention is suitable for moderate or light flash rust surfaces of steel structures with residual corrosion inhibitors on the surfaces after water spraying rust removal treatment, and can generate a good corrosion prevention effect.

Description

High-tolerance epoxy primer for water-jet rust removal surface and preparation method and application thereof
Technical Field
The invention relates to an anticorrosive paint, in particular to a high-tolerance epoxy primer suitable for a water-jet rust removal surface, a preparation method and application thereof, and belongs to the technical field of heavy anticorrosive paints.
Background
Since the innovation is open, with the steady promotion of the economy of China, the infrastructure construction is also greatly developed. In particular, in nearly fifteen years, large-scale steel structure bridges in China develop rapidly, and a large number of large-span bridges are formed in succession.
The bridge in China mostly adopts heavy anti-corrosion paint to carry out the anti-corrosion protection of the steel structure, and the protection period of the coating is generally 15-25 years. When the coating reaches the anti-corrosion service life, the coating part which is rusted needs to be recoated. Because the sand blasting rust removal can generate a large amount of dust and noise pollution and cannot meet the requirement of environmental protection, in recent years, the base material is usually treated by adopting modes such as manual rust removal or water jet rust removal.
Manual descaling often fails to achieve sufficient roughness and clean surfaces, and in some cases even fails to polish the steel substrate, with a significant amount of pitting and old paint films. Water jets or water sand jets can achieve a more desirable surface treatment rating. However, the presence of water may cause flash rust to rapidly develop on the surface of the treated steel material in a short time. In order to suppress flash rust, it is a conventional practice to add a corrosion inhibitor such as sodium nitrite to water. When water is volatilized, the corrosion inhibitor is remained on the surface of the steel, so that the phenomena of foaming, peeling and the like of the anticorrosive coating are caused, good adhesive force and anticorrosive effect cannot be ensured, and the anticorrosive service life is reduced.
Disclosure of Invention
The invention mainly aims to provide a high-tolerance epoxy primer for a water-jet rust removal surface, a preparation method and application thereof, so as to overcome the defects in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
one aspect of an embodiment of the present invention provides a highly tolerant epoxy primer for water jet rust removal surfaces comprising a first component and a second component;
wherein the first component comprises the following components in parts by weight:
Figure BDA0003141095970000011
Figure BDA0003141095970000021
the second component comprises the following components in parts by weight:
Figure BDA0003141095970000022
in some embodiments, the modified epoxy resin includes, but is not limited to, any one of or a combination of two of an alkylcyclotetrasiloxane-modified bisphenol F epoxy resin, an alkylcyclotetrasiloxane-modified bisphenol a epoxy resin.
In some embodiments, the rheological aid includes, but is not limited to, a combination of any one or more of an organobentonite, a polyamide wax, a polyethylene wax, a fumed silica, and a hydrogenated castor oil.
In some embodiments, the dispersant includes, but is not limited to, any one of high molecular block copolymers containing amine groups or carboxyl groups, which may be specifically selected according to the properties of the filler and the rust-preventive pigment, particularly the surface acid and alkali properties thereof.
In some embodiments, the filler includes, but is not limited to, any one or combination of talc, silica powder, quartz powder, sericite powder, barium sulfate, feldspar powder.
In some embodiments, the rust inhibiting pigment includes, but is not limited to, a combination of any one or more of ferrophosphorus powder, zinc phosphate, aluminum tripolyphosphate, strontium chromate.
In some embodiments, the defoamer includes, but is not limited to, a combination of any one or more of a silicone defoamer, a higher alcohol defoamer, a polyether defoamer.
In some embodiments, the graphene dispersion liquid contains 5-20 microns of graphene sheet layer diameter, less than or equal to 10 layers, and less than 15% of oxygen content.
In some embodiments, the solvent includes, but is not limited to, any one or combination of benzene-based solvents, n-butanol, butyl ester, propylene glycol monomethyl ether.
In some embodiments, the amine resin includes, but is not limited to, any one or a combination of mannich base type curing agents, cardanol modified amine type curing agents, aliphatic polyamine type curing agents, aliphatic amine adduct type curing agents, amido amine type curing agents, amino polyamide curing agents, alicyclic amine type curing agents, aromatic amine type curing agents, araliphatic amine type curing agents, and ketimine type curing agents.
In some embodiments, the catalyst includes, but is not limited to, any one or combination of tertiary amine catalysts, phenol catalysts, crosslinking catalysts.
In some embodiments, the epoxy value of the small molecule epoxy is 0.44 to 0.59, and may be selected from, for example and without limitation, E44, E51, E55, and the like.
In some embodiments, the mass ratio of the first component to the second component is 7.5-9.5: 1.
In the high-tolerance epoxy primer, on one hand, the adopted modified epoxy resin is formed by modifying bisphenol F epoxy resin or modified bisphenol A epoxy resin through alkyl cyclotetrasiloxane, on the other hand, the wetting and permeability of the resin to flash rust on the surface of a metal base material can be enhanced, so that a large amount of flash rust can be quickly coated on the surface of the metal base material after the surface of the metal base material is coated by the primer, and meanwhile, after the alkyl cyclotetrasiloxane is hydrolyzed, firm covalent bonds can be formed among the resin, the flash rust and the metal base material, so that on the one hand, the diffusion of the rust is prevented, and on the other hand, the compactness and the adhesive force of a coating film are also enhanced; on the other hand, the adopted amido or carboxyl macromolecular block copolymer dispersant can effectively improve the dispersion performance of various pigments and fillers in a coating system, and prevent the pigments and fillers from flocculating to influence the continuity of a coating film; on the other hand, because the polarity difference of the modified epoxy resin and the amine curing agent is large, the direct mixing of the modified epoxy resin and the amine curing agent can cause phase separation under normal conditions, the curing effectiveness is influenced, the polarity of the amine curing agent can be changed by adding a small amount of small-molecular epoxy resin into the second component, the compatibility of the first component and the second component is greatly improved, and all components in the primer can be well and uniformly mixed, so that the effectiveness of the coating film in a crosslinking process is improved, the crosslinking density of the coating film is increased, and the actual drying speed and the long-term resistance of the coating film are further improved.
Particularly, in the high tolerance epoxy primer, the modified epoxy resin, the dispersant, the graphene and the small molecular epoxy resin are adopted simultaneously, and are cooperated with each other, and the rest components in the primer are matched, so that the primer and a paint film formed by the primer can be well adhered to the surface of a steel product after water jet treatment, the primer is not influenced by flash rust and a corrosion inhibitor, the chloride ion permeability resistance, the salt spray resistance and the cyclic corrosion resistance which are far higher than those of the existing epoxy primer are obtained, and finally, the paint film formed by the primer simultaneously shows excellent flexibility, hardness, impact resistance, thick coating property, drawing strength, water resistance, salt spray resistance and the like, which is very surprising.
Another aspect of the embodiments of the present invention provides a method for preparing the high tolerance epoxy primer for water jet rust removing surface, which comprises:
heating bisphenol F type epoxy resin or bisphenol A epoxy resin, uniformly mixing the heated bisphenol F type epoxy resin or bisphenol A epoxy resin with alkyl cyclotetrasiloxane, and reacting in the presence of at least dibutyltin dilaurate to prepare modified epoxy resin;
uniformly mixing the modified epoxy resin with a rheological additive, a dispersing agent, a defoaming agent, a graphene dispersion liquid, an anti-rust pigment and a filler in sequence to obtain a first component;
and (3) uniformly mixing the amine resin and the micromolecule epoxy resin, adding a catalyst, and uniformly dispersing to obtain a second component.
In some embodiments, the recipe specifically includes: heating bisphenol F type epoxy resin or bisphenol A epoxy resin to 80-90 ℃, adding alkyl cyclotetrasiloxane under the condition of stirring, uniformly mixing, dropwise adding dibutyltin dilaurate and distilled water, and continuously heating to 95-100 ℃ for 30-60min to prepare the modified epoxy resin, wherein the mass ratio of the bisphenol F type epoxy resin or the bisphenol A epoxy resin to the dibutyltin dilaurate to the distilled water is (90-110) to (2.5-4.5) to (0.3-0.6) to (0-1);
in some embodiments, the recipe specifically includes: and dispersing the graphene powder and xylene at a high speed for 1-1.5h under the condition of 2500-.
In some embodiments, the recipe specifically includes: adding a rheological additive into the modified epoxy resin under the condition of stirring, dispersing at a high speed of 20-30m/s for 10-15min after uniformly mixing, then adding a dispersing agent and a defoaming agent, stirring until uniformly mixing, then sequentially adding a graphene dispersion liquid, an anti-rust pigment and a filler under the condition of stirring, uniformly mixing, dispersing at a high speed of 20-30m/s for 25-30min, ensuring that the temperature is controlled at 45-55 ℃ during the second high-speed dispersion, keeping for 15-20min, and then adjusting the viscosity of the mixture to 115-125KU by using a solvent to obtain the first component.
In some embodiments, the recipe specifically includes: slowly adding the small-molecular epoxy resin into the amine resin under the stirring condition, continuously stirring for 1.5-2.5h at the linear speed of 3-5m/s, adding the catalyst after the heat release is finished and cooling to the room temperature, and uniformly dispersing to obtain the second component.
In some more specific embodiments, the recipe includes the steps of:
(1) filling a certain amount of bisphenol F epoxy resin into a reaction vessel, heating to 80 ℃, adding alkyl cyclotetrasiloxane under the condition of stirring, dropwise adding a certain amount of dibutyltin dilaurate and a proper amount of distilled water after uniformly stirring, continuously heating to 95-100 ℃, keeping for 30-60min, then carrying out reduced pressure distillation, and cooling to obtain modified epoxy resin;
(2) adding modified epoxy resin into a stirring kettle, starting low-speed stirring, adding a rheological aid under the stirring condition, uniformly mixing, dispersing at a high speed for 10-15min, then adding a dispersing agent and a defoaming agent, and stirring for more than 5min to be uniform;
(3) under the condition of low-speed stirring, sequentially adding the graphene dispersion liquid, the anti-rust pigment and the filler into the mixture obtained in the step (2), dispersing at a high speed for 25-30min, ensuring that the temperature is controlled at 45-55 ℃ for 15-20min, and then adjusting the viscosity by using a solvent to obtain a first component;
(4) adding amine resin into a container, slowly adding the small molecular epoxy resin under stirring, continuously stirring at a low speed for 1.5-2.5h, cooling to room temperature after heat release is finished, adding a catalyst, and dispersing for 5-10min to be uniform to obtain a second component.
Another aspect of embodiments of the present invention provides the use of the highly tolerant epoxy primer in the field of metal corrosion protection, particularly in water jet rust removing surface corrosion protection.
Another aspect of embodiments of the invention provides an anticorrosive coating formed from the high tolerance epoxy primer for water jet rust removal surfaces.
According to another aspect of the embodiment of the invention, a protective structure of a metal substrate is provided, which comprises the anticorrosion coating, wherein the anticorrosion coating covers the surface of the metal substrate, and the surface of the metal substrate is subjected to water spraying rust removal treatment in advance.
Another aspect of an embodiment of the present invention provides a method for protecting a water jet rust removing surface, including: the high-tolerance epoxy primer is provided, the first component and the second component are uniformly mixed, and then the obtained mixture is coated on the surface of the metal substrate subjected to the water jet rust removal treatment and is cured to form the protective coating.
The water spraying rust removal treatment mode comprises water spraying or water sand spraying rust removal treatment, wherein the adopted water contains a corrosion inhibitor.
In this specification, the metal substrate includes a steel substrate, such as a steel structure.
Compared with the prior art, the technical scheme provided by the invention at least has the following advantages:
(1) the provided high-tolerance epoxy primer is suitable for the medium or light flash rust surface of a steel structure with residual corrosion inhibitor on the surface after water jet rust removal treatment, and can generate good anticorrosion effect;
(2) the provided high-tolerance epoxy primer has good stability, is easy for large-scale production and preparation, and is convenient to use;
(3) the anticorrosive coating formed by the provided high-tolerance epoxy primer is firmly combined with steel structure and other substrates, and has excellent mechanical property and anticorrosive property.
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In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is the results of a salt spray resistance test on the surface of a water jet rust removing steel material coated with an epoxy primer of comparative example 1;
FIG. 2 shows the results of salt spray resistance tests on the surface of water-jet rust-removing steel coated with the epoxy primer of example 3 with high tolerance.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The reagents and starting materials used in the following examples are commercially available, and the test methods in which specific conditions are not specified are generally carried out under conventional conditions or conditions recommended by the respective manufacturers. In the following examples, the linear velocity of the low-speed stirring means is 10 m/sec or less, the linear velocity of the high-speed stirring means is 20 m/sec or more, and the stirring is carried out at a medium speed of 10 to 20 m/sec.
Example 1 a method for preparing a highly tolerant epoxy primer suitable for water jet rust removal surfaces, comprising the steps of:
(1) 100g of bisphenol F epoxy resin is put into a four-neck flask with a thermometer, a stirrer, a constant pressure dropping funnel and a reflux condenser, condensed water is started and heated to 80 ℃, 3.8g of alkyl cyclotetrasiloxane is added under the stirring condition, 0.48g of dibutyltin dilaurate and 0.1g of distilled water are dropwise added after uniform stirring, the temperature is continuously raised to 95 ℃ and kept for 30min, the reflux condenser is removed and reduced pressure distillation is carried out, and the modified epoxy resin is obtained after cooling.
(2) And (2) adding 270g of the modified epoxy resin prepared in the step (1) into a stirring kettle, starting low-speed stirring, adding 9g of polyamide wax powder and 3g of organic bentonite under the stirring condition, uniformly mixing, dispersing at a high speed for 15min, then adding 2.8g of dispersing agent BYK-161 and 1.2g of organic silicon defoaming agent AFCONA-2722, and stirring for 5min to be uniform.
(3) And dispersing 35g of graphene powder and 65g of dimethylbenzene at a high speed for 1.5h under the condition of 3200r/min, and transferring to ultrasonic dispersion for 40min to prepare the graphene dispersion liquid. The graphene powder has the advantages that the diameter of a sheet layer is 5-20 micrometers, the number of layers is less than or equal to 10, and the oxygen content is less than 15%. The same applies to the graphene powder used in the following examples 2 to 4.
(4) And (3) under the condition of low-speed stirring, sequentially adding 3.5g of graphene dispersion liquid prepared in the step (3), 50g of zinc phosphate, 55g of titanium dioxide, 2g of iron oxide black, 45g of talcum powder, 40g of xylene and 400g of silicon micropowder prepared in the step (2) into the mixture prepared in the step (2), dispersing at a high speed for 25min, ensuring that the temperature is controlled at 50-55 ℃ for 15min during the period, cooling, and then adjusting the viscosity to 125KU by using 12g of mixed liquid of xylene and n-butyl alcohol in a mass ratio of 7: 3 to obtain a first component.
(5) Adding 710g of polyamide resin Ancamide350A into a container, slowly adding 150g of small molecular epoxy resin (E51) with the epoxy value of 0.51 under the stirring condition, continuously stirring at a low speed for 2 hours, adding 40g of catalyst D0590, 30g of n-butyl alcohol and 70g of xylene after heat release is finished and cooling to room temperature, and dispersing for 5min until the mixture is uniform to obtain a second component.
(6) The first component and the second component are uniformly mixed according to the mass ratio of 8: 1 to obtain the high-tolerance epoxy primer suitable for the water-jet rust removal surface.
Example 2 a method for preparing a highly tolerant epoxy primer suitable for water jet rust removal surfaces, comprising the steps of:
(1) putting 90g of bisphenol A epoxy resin into a four-neck flask with a thermometer, a stirrer, a constant-pressure dropping funnel and a reflux condenser, starting condensed water, heating to 80 ℃, adding 4.5g of alkylcyclotetrasiloxane under the condition of stirring, dropwise adding 0.6g of dibutyltin dilaurate and 0.05g of distilled water after uniformly stirring, continuously heating to 95 ℃, keeping for 35min, removing the reflux condenser, distilling under reduced pressure, and cooling to obtain the modified epoxy resin.
(2) 262g of the modified epoxy resin prepared in the step (1) is added into a stirring kettle, and low-speed stirring is started. Adding 9g of polyamide wax powder and 3g of organic bentonite under the stirring condition, uniformly mixing, dispersing at a high speed for 15min, then adding 3.3g of dispersing agent BYK-110 and 1g of organic silicon defoaming agent BYK-141, and stirring for 5min to be uniform.
(3) And dispersing 20g of graphene powder and 80g of dimethylbenzene at a high speed for 1.5h under the condition of 3200r/min, and transferring to ultrasonic dispersion for 40min to obtain the graphene dispersion liquid.
(4) And (3) under the condition of low-speed stirring, sequentially adding 3.5g of graphene dispersion liquid prepared in the step (3), 50g of zinc phosphate, 55g of titanium dioxide, 2g of iron oxide black, 45g of 500-mesh talcum powder, 40g of xylene and 400g of silicon micropowder prepared in the step (2) into the mixture prepared in the step (2), dispersing at a high speed for 25min, controlling the temperature to be 50-55 ℃ for 15min, cooling, and adjusting the viscosity to 125KU by using 25g of mixed liquid of xylene and n-butyl alcohol in a mass ratio of 7: 3 to obtain a first component.
(5) Adding 710g of polyamide resin Ancamide350A into a container, slowly adding 150g of small molecular epoxy resin with the epoxy value of 0.59 under the stirring condition, continuously stirring at a low speed for 2h, adding 40g of catalyst D0590, 30g of n-butanol and 70g of xylene after heat release is finished and the mixture is cooled to room temperature, and dispersing for 5min to be uniform to obtain a second component.
(6) The first component and the second component are uniformly mixed according to the mass ratio of 7.5: 1 to obtain the high tolerance epoxy primer suitable for the water-jet rust removal surface.
Example 3 a method of preparing a highly tolerant epoxy primer suitable for water jet rust removal surfaces, comprising the steps of:
(1) putting 110g of bisphenol F epoxy resin into a four-neck flask with a thermometer, a stirrer, a constant-pressure dropping funnel and a reflux condenser, starting condensed water, heating to 85 ℃, adding 2.5g of alkylcyclotetrasiloxane under the stirring condition, dropwise adding 0.4g of dibutyltin dilaurate and 1g of distilled water after uniformly stirring, continuously heating to 100 ℃ and keeping for 45min, removing the reflux condenser, carrying out reduced pressure distillation, and cooling to obtain the modified epoxy resin.
(2) Adding 280g of the modified epoxy resin prepared in the step (1) into a stirring kettle, and starting low-speed stirring. Adding 11g of polyamide wax powder and 3g of organic bentonite under the stirring condition, uniformly mixing, dispersing at a high speed for 15min, then adding 4g of dispersing agent BYK-ATU and 2.2g of organic silicon defoaming agent BYK-066N, and stirring for 5min to be uniform.
(3) And dispersing 40g of graphene powder and 60g of dimethylbenzene at a high speed for 1.5h under the condition of 3200r/min, and transferring to ultrasonic dispersion for 40min to prepare the graphene dispersion liquid.
(4) Under the condition of low-speed stirring, 4.5g of graphene dispersion liquid prepared in the step (3), 60g of zinc phosphate, 45g of titanium dioxide, 2g of iron oxide black, 40g of 800-mesh sericite powder, 40g of xylene and 350g of silicon micropowder prepared in the step (2) are sequentially added into the liquid prepared in the step (2), high-speed dispersion is carried out for 25min, the temperature is controlled to be 50-55 ℃ for 15min in the period, after cooling, 14g of mixed liquid with the mass ratio of xylene to n-butyl alcohol being 7: 3 is used for adjusting the viscosity to 125KU, and the first component is obtained.
(5) Adding 600g of phenolic aldehyde amine resin NC-558 into a container, slowly adding 120g of small molecular epoxy resin with the epoxy value of 0.44 under the stirring condition, continuously stirring at a low speed for 2h, after heat release is finished and the temperature is cooled to room temperature, adding 30g of catalyst DMP-30, 30g of n-butanol and 70g of xylene, and dispersing for 5min to be uniform to obtain a second component.
(6) The first component and the second component are uniformly mixed according to the mass ratio of 8.5: 1 to obtain the high tolerance epoxy primer suitable for the water jet rust removal surface.
Example 4 a method of preparing a highly tolerant epoxy primer suitable for water jet rust removal surfaces, comprising the steps of:
(1) 100g of bisphenol F epoxy resin is put into a four-neck flask with a thermometer, a stirrer, a constant pressure dropping funnel and a reflux condenser, condensed water is started and heated to 90 ℃, 3.3g of alkyl cyclotetrasiloxane is added under the condition of stirring, 0.3g of dibutyltin dilaurate and a proper amount of distilled water are added dropwise after uniform stirring, the temperature is continuously raised to 95 ℃ and is kept for 60min, the reflux condenser is removed, reduced pressure distillation is carried out, and the modified epoxy resin is obtained after cooling.
(2) And (2) adding 300g of the modified epoxy resin prepared in the step (1) into a stirring kettle, and starting low-speed stirring. Adding 12g of polyethylene wax and 5g of fumed silica under the stirring condition, uniformly mixing, dispersing at a high speed for 20min, then adding 5g of dispersing agent BYK-ATU and 1.5g of defoaming agent BYK-066N, and stirring for 5min to be uniform.
(3) And dispersing 35g of graphene powder and 65g of dimethylbenzene at a high speed for 1.5h under the condition of 3200r/min, and transferring to ultrasonic dispersion for 40min to prepare the graphene dispersion liquid.
(4) And (3) under the condition of low-speed stirring, sequentially adding 3.5g of graphene dispersion liquid prepared in the step (3), 45g of zinc phosphate, 20g of aluminum tripolyphosphate, 40g of titanium dioxide, 1.5g of iron oxide black, 30g of 500-mesh talcum powder, 30g of 800-mesh mica powder, 60g of xylene and 300g of silicon micropowder into the mixture prepared in the step (2), dispersing at a high speed for 25min, controlling the temperature to be 50-55 ℃ for 15min, cooling, and adjusting the viscosity to 120KU by using 15g of mixed liquid with the mass ratio of the xylene to the n-butyl alcohol being 7: 3 to obtain a first component.
(5) Adding 660g of polyamide resin ANCAMD2353 into a container, slowly adding 145g of small molecular epoxy resin with the epoxy value of 0.51 under the stirring condition, continuously stirring at a low speed for 2 hours, after heat release is finished and the mixture is cooled to room temperature, adding 40g of catalyst DMP-30, 30g of n-butanol and 70g of xylene, and dispersing for 5min to be uniform to obtain a second component.
(6) And uniformly mixing the first component and the second component according to the mass ratio of 8: 1 to obtain the high-tolerance epoxy primer suitable for the water-jet rust removal surface.
Comparative example 1 this comparative example provides a method for preparing an epoxy primer in which the bisphenol F type modified epoxy resin of example 1 was replaced with an unmodified bisphenol F type epoxy resin NPEF-170, and the other components were kept in accordance with example 1. The preparation method comprises the following steps:
(1) 270g of bisphenol F type epoxy NPEF-170 resin was added to the stirred tank, and low-speed stirring was started. Adding 9g of polyamide wax powder and 3g of organic bentonite under the stirring condition, uniformly mixing, dispersing at a high speed for 15min, then adding 2.8g of dispersing agent BYK-161 and 1.2g of organic silicon defoaming agent AFCONA-2722, and stirring for 5min to be uniform.
(2) And dispersing 35g of graphene powder and 65g of dimethylbenzene at a high speed for 1.5h under the condition of 3200r/min, and transferring to ultrasonic dispersion for 40min to prepare the graphene dispersion liquid.
(3) And (3) under the condition of low-speed stirring, sequentially adding 3.5g of graphene dispersion liquid prepared in the step (3), 50g of zinc phosphate, 55g of titanium dioxide, 2g of iron oxide black, 45g of talcum powder, 40g of xylene and 400g of silicon micropowder prepared in the step (2) into the liquid prepared in the step (2), and dispersing at a high speed for 25min, wherein the temperature is controlled at 50-55 ℃ for 15 min. After cooling, the viscosity is adjusted to 125KU by 12g of mixed solution of solvent xylene and n-butanol with the mass ratio of 7: 3 to obtain the first component.
(4) Adding 710g of polyamide resin Ancamide350A into a container, slowly adding 150g of small molecular epoxy resin with the epoxy value of 0.51 under the stirring condition, continuously stirring at a low speed for 2h, adding 40g of catalyst D0590, 30g of n-butanol and 70g of xylene after heat release is finished and the mixture is cooled to room temperature, and dispersing for 5min to be uniform to obtain a second component.
(5) And uniformly mixing the first component and the second component according to the mass ratio of 8: 1 to obtain the epoxy primer product.
Comparative example 2 this comparative example provides a method for preparing an epoxy primer wherein the small molecule epoxy resin is omitted and the second component is adjusted to an active hydrogen equivalent of 140-150, the other components being identical to those of example 1. The preparation method comprises the following steps:
(1) 100g of bisphenol F epoxy resin is put into a four-neck flask with a thermometer, a stirrer, a constant pressure dropping funnel and a reflux condenser, condensed water is started and heated to 80 ℃, 3.8g of alkyl cyclotetrasiloxane is added under the condition of stirring, 0.48g of dibutyltin dilaurate and a proper amount of distilled water are added dropwise after uniform stirring, the temperature is continuously raised to 95 ℃ and kept for 35min, the reflux condenser is removed, reduced pressure distillation is carried out, and the modified epoxy resin is obtained after cooling.
(2) And (2) adding 270g of the modified epoxy resin prepared in the step (1) into a stirring kettle, and starting low-speed stirring. Adding 9g of polyamide wax powder and 3g of organic bentonite under the stirring condition, uniformly mixing, dispersing at a high speed for 15min, then adding 2.8g of dispersing agent BYK-161 and 1.2g of organic silicon defoaming agent AFCONA-2722, and stirring for 5min to be uniform.
(3) And dispersing 35g of graphene powder and 65g of dimethylbenzene at a high speed for 1.5h under the condition of 3200r/min, and transferring to ultrasonic dispersion for 40min to prepare the graphene dispersion liquid.
(4) And (3) under the condition of low-speed stirring, sequentially adding 3.5g of graphene dispersion liquid prepared in the step (3), 50g of zinc phosphate, 55g of titanium dioxide, 2g of iron oxide black, 45g of talcum powder, 40g of xylene and 400g of silicon micropowder prepared in the step (2) into the liquid prepared in the step (2), dispersing at a high speed for 25min, ensuring that the temperature is controlled at 50-55 ℃ for 15min, cooling, and then adjusting the viscosity to 125KU by using 12g of mixed liquid with the mass ratio of xylene to n-butyl alcohol being 7: 3 to obtain the first component.
(5) Adding 400g polyamide resin Ancamide350A into a container, adding 20g catalyst D0590, 60g n-butanol and 140g xylene under stirring, and dispersing for 5min to obtain the second component.
(6) And uniformly mixing the first component and the second component according to the mass ratio of 8: 1 to obtain the epoxy primer product.
Comparative example 3 an epoxy primer provided in this comparative example was prepared substantially the same as in example 1, except that: step (3) is omitted, and no graphene dispersion liquid is added in step (4). The preparation method comprises the following steps:
(1) 100g of bisphenol F epoxy resin is put into a four-neck flask with a thermometer, a stirrer, a constant pressure dropping funnel and a reflux condenser, condensed water is started and heated to 85 ℃, 2.5g of alkyl cyclotetrasiloxane is added under the condition of stirring, 0.4g of dibutyltin dilaurate and a proper amount of distilled water are added dropwise after uniform stirring, the temperature is continuously raised to 95 ℃ and kept for 45min, the reflux condenser is removed and reduced pressure distillation is carried out, and the modified epoxy resin is obtained after cooling.
(2) Adding 280g of the modified epoxy resin prepared in the step (1) into a stirring kettle, and starting low-speed stirring. Adding 11g of polyamide wax powder and 3g of organic bentonite under the stirring condition, uniformly mixing, dispersing at a high speed for 15min, adding 4g of dispersing agent BYK-ATU and 2.2g of organic silicon defoamer BYK-066N, and stirring for 5min until uniform.
(3) Under the condition of low-speed stirring, sequentially adding 60g of zinc phosphate, 45g of titanium dioxide, 2g of iron oxide black, 40g of 800-mesh sericite powder, 40g of xylene and 350g of silicon micropowder into the liquid prepared in the step (2), dispersing at a high speed for 25min, controlling the temperature to be 50-55 ℃ for 15min, cooling, and adjusting the viscosity to 125KU by using 14g of mixed liquid with the mass ratio of the xylene to the n-butyl alcohol being 7: 3 to obtain the first component.
(4) Adding 600g of phenolic aldehyde amine resin NC-558 into a container, slowly adding 120g of small molecular epoxy resin with the epoxy value of 0.44 under the stirring condition, continuously stirring at a low speed for 2h, after heat release is finished and the temperature is cooled to room temperature, adding 30g of catalyst DMP-30, 30g of n-butanol and 70g of xylene, and dispersing for 5min to be uniform to obtain a second component.
(5) The first component and the second component are uniformly mixed according to the mass ratio of 9.5:1 to obtain the epoxy primer product.
Comparative example 4: the preparation method of the epoxy primer provided by the comparative example is basically the same as that of the example 1, and the difference is that: after the step (1) is finished, the first component and the second component of the epoxy primer are respectively and completely mixed uniformly at one time without adopting the operations of low-speed and high-speed stirring, temperature control, activation and the like in steps.
(1) 100g of bisphenol F epoxy resin is put into a four-neck flask with a thermometer, a stirrer, a constant pressure dropping funnel and a reflux condenser, condensed water is started and heated to 80 ℃, 3.8g of alkyl cyclotetrasiloxane is added under the stirring condition, 0.48g of dibutyltin dilaurate and 0.1g of distilled water are dropwise added after uniform stirring, the temperature is continuously raised to 95 ℃ and kept for 30min, the reflux condenser is removed and reduced pressure distillation is carried out, and the modified epoxy resin is obtained after cooling.
(2) Adding 270g of modified epoxy resin prepared in the step (1), 9g of polyamide wax powder, 3g of organic bentonite, 2.8g of dispersant BYK-161, 1.2g of organic silicon defoamer AFCONA-2722, 3.5g of graphene dispersion liquid, 50g of zinc phosphate, 55g of titanium dioxide, 2g of iron oxide black, 45g of talcum powder, 40g of dimethylbenzene, 400g of silicon micropowder and 12g of mixed solution of dimethylbenzene and n-butyl alcohol in a mass ratio of 7: 3 into a stirring kettle, and uniformly stirring to obtain a first component.
(3) Adding 710g polyamide resin Ancamide350A into a container, adding 150g of small molecular epoxy resin (E51) with the epoxy value of 0.51, 40g of catalyst D0590, 30g of n-butanol and 70g of xylene under the condition of stirring, and uniformly dispersing to obtain a second component.
(4) And uniformly mixing the first component and the second component according to the mass ratio of 8: 1 to obtain the epoxy primer product.
The highly tolerant epoxy primers of examples 1-4 above and the paint films formed therefrom were tested for a number of properties and the results are shown in Table 1 below. The tests in table 1 were conducted on the products of examples 1-4, which were consistent in test results 1, 7, 8, while test results 2-6 were the average of the test data relating to the products.
TABLE 1
Figure BDA0003141095970000101
Figure BDA0003141095970000111
The performance of the high tolerance epoxy primers of examples 1-4 and the epoxy primers of comparative examples 1-3 were further tested, and the corresponding test results are shown in tables 2 and 3. The test results in tables 2-3 are the average of the test results for multiple batches of product.
TABLE 2
Flexibility Hardness of Impact resistance Thick coating property Drawing strength
Example 1 1mm H 50cm 525μm 10.6MPa
Example 2 2mm 2H 50cm 600μm 11.1MPa
Example 3 2mm 2H 50cm 575μm 11.3MPa
Example 4 1mm H 50cm 575μm 10.8MPa
Comparative example 1 2mm H 50cm 575μm 8.6MPa
Comparative example 2 2mm H 50cm 575μm 6.5MPa
Comparative example 3 2mm 2H 50cm 525μm 10.5MPa
Comparative example 4 3mm H 50cm 150μm 5.2MPa
TABLE 3
Figure BDA0003141095970000112
Figure BDA0003141095970000121
The test method employed in this specification is as follows:
flexibility was tested according to GB/T1731-; the hardness is tested according to the GB/T6739-2006 standard; the impact resistance is tested according to GB/T1732-1993 standard; the thick coating property is tested according to the GB/T9264-1988 standard; the drawing strength is tested according to the GB/T5210-2006 standard; the salt water resistance is tested according to the GB/T10834-2008 standard; the salt spray resistance is tested according to the GB/T1771-2008 standard; the chloride ion permeability resistance is tested according to the method of appendix C.2 of the JTJ275-2000 standard; the cyclic corrosion test was tested according to the method of appendix A of the ISO 20340-2009 standard, with 25 cycles tested.
In the test items shown in Table 3 above, the substrates were all water-sprayed steel plates, 0.5 wt% of sodium nitrite corrosion inhibitor was added to the water to have a roughness of 40-75 μ M, the steel plates were allowed to stand at room temperature until moderate flash rust (M) was generated on the steel surfaces as specified in SSPC-SP 12/NACE No.5 standard, and high-tolerance epoxy primer was directly sprayed thereon. Wherein, one time of water resistance and salt spray resistance air spraying reaches the thickness of a dry film of 90-100 μm, the test of chloride ion permeability resistance and cyclic corrosion is divided into 3 times of air spraying to the thickness of the dry film of 300-320 μm, the coating interval is 24h, and the test is carried out after air drying for 7 d.
The high tolerance epoxy primers prepared in the above examples 1-4 have flexibility less than 2mm, hardness H-2H, impact resistance of 50cm, thick coating property of 525 μm or more, drawing strength of 9MPa or more, water resistance (240H) without abnormality, salt spray resistance (1000H) without foaming, rusting, cracking, peeling and the like, and chloride ion permeability less than 0.8 × 10-3mg/cm2d, the unilateral extension etching widths of the circular corrosion test are all less than 2.6 mm.
The epoxy primers prepared in the above comparative examples 1-3 are slightly inferior to the test results of examples 1-4 in terms of conventional physical properties, and are much inferior to examples 1-4 in terms of various long-term resistance tests, especially the cycle corrosion test has significantly inferior corrosion spreading width, water resistance and salt spray resistance to examples 1-4.
The high tolerance epoxy primer prepared in example 3 has the best performance, and has the advantages of 2mm flexibility, 2H hardness, 50cm impact resistance, 575 mu m thick coating property, 11.3MPa drawing strength and 240H water resistance without abnormityThe salt spray resistance (1000h) paint film has no phenomena of foaming, rusting, cracking, peeling and the like, and the chlorine ion permeability resistance is 0.3 multiplied by 10-3mg/cm2d, unilateral extension etching width of 1.8mm in a circulating corrosion test. The mechanical property and the corrosion resistance of the coating on the surface of flash rust steel treated by water-spraying sand far exceed those of like products in the market.
The high tolerance epoxy primer of example 3 and the epoxy primer of comparative example 1 were coated on the surface of the water-jet rust-removing steel material containing the corrosion inhibitor, and after 7 days of natural drying, the salt spray resistance test was carried out for 1000h, and the surface of the coating of comparative example 1 was rusted (see fig. 1), while the surface of the coating of example 3 was intact (see fig. 2).
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (16)

1. A highly tolerant epoxy primer for water jet rust removing surfaces, characterized in that the primer comprises a first component and a second component;
wherein the first component comprises the following components in parts by weight:
20-35 parts of modified epoxy resin
1-2 parts of rheological additive
0.1 to 1 portion of dispersant
30-40 parts of filler
10-20 parts of antirust pigment
0.1 to 1 portion of defoaming agent
0.1-1 part of graphene dispersion liquid
5-15 parts of a solvent;
the second component comprises the following components in parts by weight:
60-80 parts of amine resin
10-18 parts of small molecular epoxy resin
3-5 parts of catalyst
10-15 parts of a solvent;
wherein the modified epoxy resin is selected from any one or the combination of two of alkyl cyclotetrasiloxane modified bisphenol F epoxy resin and alkyl cyclotetrasiloxane modified bisphenol A epoxy resin, and the preparation method of the modified epoxy resin comprises the following steps: heating bisphenol F epoxy resin or bisphenol A epoxy resin to 80-90 ℃, adding alkyl cyclotetrasiloxane under the condition of stirring, dropwise adding dibutyltin dilaurate and distilled water after uniformly mixing, and continuously heating to 95-100 ℃ for 30-60min to obtain modified epoxy resin, wherein the mass ratio of the bisphenol F epoxy resin or bisphenol A epoxy resin, the alkyl cyclotetrasiloxane, the dibutyltin dilaurate and the distilled water is (90-110): (2.5-4.5): (0.3-0.6): (0-1);
the concentration of the graphene dispersion liquid is 20-40wt%, the diameter of each graphene sheet is 5-20 micrometers, the number of layers is less than or equal to 10, and the oxygen content is less than 15%;
the dispersing agent is selected from any one of high molecular block copolymers containing amino or carboxyl;
the epoxy value of the small molecular epoxy resin is 0.44-0.59.
2. The highly tolerant epoxy primer of claim 1, wherein: the rheological additive is selected from any one or more of organic bentonite, polyamide wax, polyethylene wax, fumed silica and hydrogenated castor oil.
3. The highly tolerant epoxy primer of claim 1, wherein: the filler is selected from any one or combination of more of talcum powder, silica powder, quartz powder, sericite powder, barium sulfate and feldspar powder.
4. The highly tolerant epoxy primer of claim 1, wherein: the antirust pigment is selected from any one or combination of more of ferrophosphorus powder, zinc phosphate, aluminum tripolyphosphate and strontium chromate.
5. The highly tolerant epoxy primer of claim 1 wherein: the defoaming agent is selected from any one or combination of more of an organic silicon defoaming agent, a high-alcohol defoaming agent and a polyether defoaming agent.
6. The highly tolerant epoxy primer of claim 1, wherein: the solvent is selected from any one or combination of more of benzene solvents, n-butyl alcohol, butyl ester and propylene glycol monomethyl ether.
7. The highly tolerant epoxy primer of claim 1, wherein: the amine resin is selected from any one or combination of more of a Mannich base curing agent, an aliphatic polyamine curing agent, an amido amine curing agent, an alicyclic amine curing agent, an aromatic aliphatic amine curing agent and a ketimine curing agent.
8. The highly tolerant epoxy primer of claim 1, wherein: the catalyst is selected from any one or combination of more of tertiary amine catalysts and phenol catalysts.
9. The highly tolerant epoxy primer of claim 1, wherein: the mass ratio of the first component to the second component is 7.5-9.5: 1.
10. A method for preparing a high tolerance epoxy primer for water jet rust cleaning surface according to any one of claims 1-9, which comprises:
heating bisphenol F epoxy resin or bisphenol A epoxy resin to 80-90 ℃, adding alkyl cyclotetrasiloxane under the condition of stirring, dropwise adding dibutyltin dilaurate and distilled water after uniformly mixing, and continuously heating to 95-100 ℃ for 30-60min to obtain modified epoxy resin, wherein the mass ratio of the bisphenol F epoxy resin or bisphenol A epoxy resin, the alkyl cyclotetrasiloxane, the dibutyltin dilaurate and the distilled water is (90-110): (2.5-4.5): (0.3-0.6): (0-1);
uniformly mixing the modified epoxy resin with a rheological additive, a dispersing agent, a defoaming agent, a graphene dispersion liquid, an anti-rust pigment and a filler in sequence to obtain a first component;
and (3) uniformly mixing the amine resin and the micromolecule epoxy resin, adding a catalyst, and uniformly dispersing to obtain a second component.
11. The method for preparing the high tolerance epoxy primer for the water jet rust removing surface as claimed in claim 10, which comprises the following steps: and dispersing the graphene powder and xylene at a high speed for 1-1.5h under the condition of 2500-.
12. The method for preparing the high tolerance epoxy primer for the water jet rust removing surface as claimed in claim 10, which comprises the following steps: adding a rheological additive into the modified epoxy resin under the condition of stirring, dispersing at a high speed of 20-30m/s for 10-15min after uniformly mixing, then adding a dispersing agent and a defoaming agent, stirring until uniformly mixing, then sequentially adding a graphene dispersion liquid, an anti-rust pigment and a filler under the condition of stirring, uniformly mixing, dispersing at a high speed of 20-30m/s for 25-30min, ensuring that the temperature is controlled at 45-55 ℃ during the second high-speed dispersion, keeping for 15-20min, and then adjusting the viscosity of the mixture to 115-125KU by using a solvent to obtain the first component.
13. The method for preparing the high tolerance epoxy primer for the water jet rust removing surface as claimed in claim 10, which comprises the following steps: slowly adding the small-molecular epoxy resin into the amine resin under the stirring condition, continuously stirring for 1.5-2.5h at the linear speed of 3-5m/s, adding the catalyst after the heat release is finished and cooling to the room temperature, and uniformly dispersing to obtain the second component.
14. An anti-corrosive coating formed from the highly tolerant epoxy primer for water jet rust removing surfaces of any one of claims 1-9.
15. A protective structure for a metal substrate, which is characterized by comprising the anti-corrosion coating layer as claimed in claim 14, wherein the anti-corrosion coating layer covers the surface of the metal substrate, and the surface of the metal substrate is subjected to water jet rust removal treatment in advance; the metal substrate comprises a steel substrate.
16. A protection method for a water-jet rust removing surface is characterized by comprising the following steps: providing the high-tolerance epoxy primer as defined in any one of claims 1 to 9, uniformly mixing the first component and the second component, and then coating the obtained mixture on the surface of the metal substrate subjected to the water jet rust removal treatment and curing to form a protective coating; the metal substrate is a steel substrate.
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