CN113480918A - Preparation process of epoxy corrosion-resistant waterproof coating - Google Patents

Preparation process of epoxy corrosion-resistant waterproof coating Download PDF

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Publication number
CN113480918A
CN113480918A CN202110843657.4A CN202110843657A CN113480918A CN 113480918 A CN113480918 A CN 113480918A CN 202110843657 A CN202110843657 A CN 202110843657A CN 113480918 A CN113480918 A CN 113480918A
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parts
stirring
component
corrosion
resistant waterproof
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王和山
王和政
李子荣
朱小姣
王厚国
王和东
殷东楼
曹文强
张萍
张万霞
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Anhui Kailin New Material Co Ltd
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Anhui Kailin New Material Co Ltd
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Abstract

The invention provides a preparation process of an epoxy corrosion-resistant waterproof coating, and relates to the technical field of waterproof coating processing. The epoxy corrosion-resistant waterproof coating comprises a component A and a component B which are equal in mass, wherein the component A is as follows: epoxy resin, modified polyurethane, zinc oxide, nano silicon dioxide, ethyl acetate, nano molybdenum disulfide, graphene oxide, sodium lignosulfonate and barium titanate; the component B comprises a reactive diluent, a curing agent, a cross-linking agent and a plasticizer. The preparation process mainly comprises the following steps: the preparation method comprises the steps of preparation of modified graphene oxide, preparation of composite epoxy resin, compounding of modified polyurethane, preparation of a component A, preparation of a component B and the like. The invention overcomes the defects of the prior art, improves the hydrophobicity of the coating after the coating is used while effectively improving the corrosion resistance of the coating, further improves the waterproof effect of the coating, ensures the cohesiveness of the coating and prevents the coating from cracking and falling off.

Description

Preparation process of epoxy corrosion-resistant waterproof coating
Technical Field
The invention relates to the technical field of waterproof coating processing, in particular to a preparation process of an epoxy corrosion-resistant waterproof coating.
Background
The waterproof coating is a coating which can prevent rainwater or underground water from leaking through a coating film formed by the coating; the waterproof coating can be divided into the following according to the coating state and form: emulsion, solvent, reactive and modified asphalts.
Common waterproof coatings are epoxy, polyurethane, and acrylic coatings. Among them, epoxy resin coating is a coating commonly used in construction owing to its good protective physicochemical properties, adhesive properties and very comprehensive chemical resistance.
The epoxy resin coating mainly refers to a film-forming substance mainly comprising bisphenol A epoxy resin and a curing agent, and contains a certain amount of reactive diluent, auxiliary agent, filler, accelerator and coupling agent. When the epoxy resin coating is used, the epoxy resin coating is coated on the surface of concrete, and in the process of curing, part of base materials react with each other to generate a solidified body with a three-dimensional net structure, so that the effects of preventing water and preventing the external corrosive environment from being damaged are achieved; part of the base material can penetrate into the concrete to form a firm whole at the interface, so that excellent bonding strength is achieved.
However, the epoxy resin coating has poor weather resistance, and the surface water resistance is reduced after the epoxy resin coating is corroded by acid and alkali, and meanwhile, the coating cracks, and the service life of the coating is seriously influenced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation process of an epoxy corrosion-resistant waterproof coating, which can effectively improve the corrosion resistance of the coating, improve the hydrophobicity of the coating after the coating is used, further improve the waterproof effect of the coating, ensure the cohesiveness of the coating and prevent the coating from cracking and falling off.
In order to achieve the above purpose, the technical scheme of the invention is realized by the following technical scheme:
the epoxy corrosion-resistant waterproof coating comprises a component A and a component B which are equal in mass, wherein the component A comprises the following materials in parts by weight: 25-30 parts of epoxy resin, 12-14 parts of modified polyurethane, 4-8 parts of zinc oxide, 3-6 parts of nano silicon dioxide, 8-10 parts of ethyl acetate, 2-3 parts of nano molybdenum disulfide, 2-4 parts of graphene oxide, 2-6 parts of sodium lignosulfonate and 2-3 parts of barium titanate; the component B comprises the following substances in parts by weight: 12-24 parts of reactive diluent, 2-6 parts of curing agent, 2-3 parts of cross-linking agent and 1-4 parts of plasticizer.
Preferably, the reactive diluent is a mixture of phenyl glycidyl ether and resorcinol diglycidyl ether in a mass ratio of 2: 1.
Preferably, the curing agent is one or more of aminoethyl piperazine, diethylenetriamine and diethylaminopropylamine.
Preferably, the preparation of the modified polyurethane comprises the following steps:
(1) dehydrating polypropylene glycol in a reaction kettle in vacuum, adding toluene diisocyanate and a dibutyltin laurate catalyst into the reaction kettle, controlling the temperature to be 80 ℃, and reacting for 2 hours;
(2) continuously adding 2, 2-bis (hydroxymethyl) propionic acid and acetone into the reaction kettle, and preserving heat for 2 hours at the temperature of 80 ℃;
(3) and (3) continuously adding the hydroxyl silicone oil into the reaction kettle, and continuously reacting for 2 hours to obtain the modified polyurethane.
The preparation process of the epoxy corrosion-resistant waterproof coating comprises the following steps:
(1) preparing modified graphene oxide: adding graphene oxide into distilled water, heating to 60 ℃, adding sodium lignosulfonate, mixing and stirring uniformly, performing ultrasonic dispersion for 10-15min, placing in a stirring kettle, mechanically stirring at a high speed, and performing vacuum drying in a vacuum drying oven to obtain modified graphene oxide for later use;
(2) preparing the composite epoxy resin: adding the modified graphene oxide into distilled water, adjusting the pH value to acidity, then adding zinc oxide, placing the mixture into a water bath kettle at 80 ℃ for ultrasonic homogenization, taking out the mixture for high-speed centrifugation, placing the centrifuged precipitate into a hot air drying box for drying to obtain a dried precipitate, adding epoxy resin into the dried precipitate, heating the dried precipitate to 50-60 ℃, then performing magnetic stirring for 2 hours, and then placing the dried precipitate into a high-pressure reaction kettle for high-pressure stirring for 20-30min to obtain composite epoxy resin for later use;
(3) compounding modified polyurethane: adding nano silicon dioxide into ethyl acetate, fully stirring, adding modified polyurethane, placing in a high-pressure reaction kettle, mixing and stirring at high pressure in the atmosphere of nitrogen for 30min to obtain a composite material for later use;
(4) preparation of component A: adding the composite epoxy resin into nano molybdenum disulfide and barium titanate, mixing, placing in a high-temperature water bath environment, stirring uniformly, continuing to stir for 20-30min in a low-temperature environment, taking out, recovering to normal temperature, adding the composite material, heating to 60-80 ℃, and stirring uniformly to obtain a component A for later use;
(5) preparation of the component B: mixing the reactive diluent, the curing agent, the cross-linking agent and the plasticizer, mechanically stirring the mixture evenly in a high-temperature environment, and then cooling the mixture to the normal temperature to obtain the component B for later use.
Preferably, the rotation speed of the high-speed mechanical stirring in the step (1) is 1200-1800r/min, and the stirring time is 15-20 min.
Preferably, the pressure of the high-pressure stirring in the step (2) is 8-10MPa, and the rotation speed of the stirring is 200-400 r/min.
Preferably, the pressure of the high-pressure mixing and stirring in the step (3) is 6-8MPa, and the rotating speed of the stirring is 120-180 r/min.
Preferably, in the step (4), the stirring temperature of the high-temperature water bath environment is 60-80 ℃, and the continuous stirring temperature in the low-temperature environment is 2-6 ℃.
The invention provides a preparation process of an epoxy corrosion-resistant waterproof coating, which has the advantages that compared with the prior art:
(1) according to the application, the zinc oxide loaded graphene oxide is adopted to compound the epoxy resin, so that the mechanical property and the thermal stability of the coating can be effectively improved, meanwhile, the graphene oxide is firstly modified by sodium lignosulfonate, the hardness and the adhesiveness of the coating can be effectively improved, meanwhile, the corrosion resistance of the coating can be further improved by adopting the zinc oxide loaded modified graphene oxide, and the service life of a product is prolonged;
(2) according to the invention, the organic silicon modified polyurethane is added, the composite epoxy resin is mixed with other materials in the application, so that the hydrophobicity of a material coating can be effectively improved, and the nano silicon dioxide and the molybdenum sulfide and the barium titanate which are added at the later stage are mixed, so that the waterproof performance and the corrosion resistance are further enhanced.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. 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.
Example 1:
the epoxy corrosion-resistant waterproof coating comprises a component A and a component B which are equal in mass, wherein the component A comprises the following materials in parts by weight: 25 parts of epoxy resin, 12 parts of modified polyurethane, 4 parts of zinc oxide, 3 parts of nano silicon dioxide, 8 parts of ethyl acetate, 2 parts of nano molybdenum disulfide, 2 parts of graphene oxide, 2 parts of sodium lignosulfonate and 2 parts of barium titanate; the component B comprises the following substances in parts by weight: 12 parts of reactive diluent, 2 parts of curing agent, 2 parts of cross-linking agent and 1 part of plasticizer.
Wherein the reactive diluent is a mixture of phenyl glycidyl ether and resorcinol diglycidyl ether in a mass ratio of 2: 1; and the curing agent is one or a mixture of more of aminoethylpiperazine, diethylenetriamine and diethylaminopropylamine.
The preparation of the modified polyurethane comprises the following steps:
(1) dehydrating polypropylene glycol in a reaction kettle in vacuum, adding toluene diisocyanate and a dibutyltin laurate catalyst into the reaction kettle, controlling the temperature to be 80 ℃, and reacting for 2 hours;
(2) continuously adding 2, 2-bis (hydroxymethyl) propionic acid and acetone into the reaction kettle, and preserving heat for 2 hours at the temperature of 80 ℃;
(3) and continuously adding the hydroxyl silicone oil into the reaction kettle, and continuously reacting for 2 hours to obtain the organic silicon modified polyurethane.
The preparation process of the epoxy corrosion-resistant waterproof coating comprises the following steps:
(1) preparing modified graphene oxide: adding graphene oxide into distilled water, heating to 60 ℃, adding sodium lignosulfonate, uniformly mixing and stirring, performing ultrasonic dispersion for 10min, then placing in a stirring kettle, mechanically stirring at a high speed of 1200r/min for 15min, and then performing vacuum drying in a vacuum drying oven to obtain modified graphene oxide for later use;
(2) preparing the composite epoxy resin: adding the modified graphene oxide into distilled water, adjusting the pH value to acidity, adding zinc oxide, placing the mixture into a water bath kettle at 80 ℃ for ultrasonic homogenization, taking out the mixture for high-speed centrifugation, placing the centrifuged precipitate into a hot air drying box for drying to obtain a dried precipitate, adding epoxy resin, heating to 50 ℃, performing magnetic stirring for 2 hours, then placing the dried precipitate into a high-pressure reaction kettle, and performing high-pressure stirring for 20 minutes at the rotating speed of 200r/min and the pressure of 8MPa to obtain composite epoxy resin for later use;
(3) compounding modified polyurethane: adding nano silicon dioxide into ethyl acetate, fully stirring, adding modified polyurethane, placing in a high-pressure reaction kettle, mixing and stirring at the high pressure of 6MPa and the rotating speed of 120r/min for 30min in the atmosphere of nitrogen, and obtaining a composite material for later use;
(4) preparation of component A: adding the composite epoxy resin into nano molybdenum disulfide and barium titanate, mixing, placing in a high-temperature water bath environment at 60 ℃, uniformly stirring, further continuously stirring for 20min in a low-temperature environment at 2 ℃, taking out, recovering to normal temperature, adding the composite material, heating to 60 ℃, and uniformly stirring to obtain a component A for later use;
(5) preparation of the component B: mixing the reactive diluent, the curing agent, the cross-linking agent and the plasticizer, mechanically stirring the mixture evenly in a high-temperature environment, and then cooling the mixture to the normal temperature to obtain the component B for later use.
Example 2:
the epoxy corrosion-resistant waterproof coating comprises a component A and a component B which are equal in mass, wherein the component A comprises the following materials in parts by weight: 30 parts of epoxy resin, 14 parts of modified polyurethane, 8 parts of zinc oxide, 6 parts of nano silicon dioxide, 10 parts of ethyl acetate, 3 parts of nano molybdenum disulfide, 4 parts of graphene oxide, 6 parts of sodium lignosulfonate and 3 parts of barium titanate; the component B comprises the following substances in parts by weight: 24 parts of reactive diluent, 6 parts of curing agent, 3 parts of cross-linking agent and 4 parts of plasticizer.
Wherein the reactive diluent is a mixture of phenyl glycidyl ether and resorcinol diglycidyl ether in a mass ratio of 2: 1; and the curing agent is one or a mixture of more of aminoethylpiperazine, diethylenetriamine and diethylaminopropylamine.
The preparation of the modified polyurethane comprises the following steps:
(1) dehydrating polypropylene glycol in a reaction kettle in vacuum, adding toluene diisocyanate and a dibutyltin laurate catalyst into the reaction kettle, controlling the temperature to be 80 ℃, and reacting for 2 hours;
(2) continuously adding 2, 2-bis (hydroxymethyl) propionic acid and acetone into the reaction kettle, and preserving heat for 2 hours at the temperature of 80 ℃;
(3) and continuously adding the hydroxyl silicone oil into the reaction kettle, and continuously reacting for 2 hours to obtain the organic silicon modified polyurethane.
The preparation process of the epoxy corrosion-resistant waterproof coating comprises the following steps:
(1) preparing modified graphene oxide: adding graphene oxide into distilled water, heating to 60 ℃, adding sodium lignosulfonate, uniformly mixing and stirring, performing ultrasonic dispersion for 15min, mechanically stirring in a stirring kettle at a high speed of 1800r/min for 20min, and performing vacuum drying in a vacuum drying oven to obtain modified graphene oxide for later use;
(2) preparing the composite epoxy resin: adding the modified graphene oxide into distilled water, adjusting the pH value to acidity, adding zinc oxide, placing the mixture into a water bath kettle at 80 ℃ for ultrasonic homogenization, taking out the mixture for high-speed centrifugation, placing the centrifuged precipitate into a hot air drying box for drying to obtain a dried precipitate, adding epoxy resin, heating to 60 ℃, performing magnetic stirring for 2 hours, then placing the dried precipitate into a high-pressure reaction kettle, and performing high-pressure stirring for 30 minutes at the rotating speed of 400r/min and the pressure of 10MPa to obtain composite epoxy resin for later use;
(3) compounding modified polyurethane: adding nano silicon dioxide into ethyl acetate, fully stirring, adding modified polyurethane, placing in a high-pressure reaction kettle, mixing and stirring at the rotating speed of 180r/min under the high pressure of 8MPa in the atmosphere of nitrogen for 30min to obtain a composite material for later use;
(4) preparation of component A: adding the composite epoxy resin into nano molybdenum disulfide and barium titanate, mixing, placing in a high-temperature water bath environment at 80 ℃, uniformly stirring, further continuously stirring for 30min in a low-temperature environment at 6 ℃, taking out, recovering to normal temperature, adding the composite material, heating to 80 ℃, and uniformly stirring to obtain a component A for later use;
(5) preparation of the component B: mixing the reactive diluent, the curing agent, the cross-linking agent and the plasticizer, mechanically stirring the mixture evenly in a high-temperature environment, and then cooling the mixture to the normal temperature to obtain the component B for later use.
Example 3:
the epoxy corrosion-resistant waterproof coating comprises a component A and a component B which are equal in mass, wherein the component A comprises the following materials in parts by weight: 28 parts of epoxy resin, 13 parts of modified polyurethane, 6 parts of zinc oxide, 5 parts of nano silicon dioxide, 9 parts of ethyl acetate, 2.5 parts of nano molybdenum disulfide, 3 parts of graphene oxide, 4 parts of sodium lignosulfonate and 2.5 parts of barium titanate; the component B comprises the following substances in parts by weight: 18 parts of reactive diluent, 4 parts of curing agent, 2.5 parts of cross-linking agent and 3 parts of plasticizer.
Wherein the reactive diluent is a mixture of phenyl glycidyl ether and resorcinol diglycidyl ether in a mass ratio of 2: 1; and the curing agent is one or a mixture of more of aminoethylpiperazine, diethylenetriamine and diethylaminopropylamine.
The preparation of the modified polyurethane comprises the following steps:
(1) dehydrating polypropylene glycol in a reaction kettle in vacuum, adding toluene diisocyanate and a dibutyltin laurate catalyst into the reaction kettle, controlling the temperature to be 80 ℃, and reacting for 2 hours;
(2) continuously adding 2, 2-bis (hydroxymethyl) propionic acid and acetone into the reaction kettle, and preserving heat for 2 hours at the temperature of 80 ℃;
(3) and continuously adding the hydroxyl silicone oil into the reaction kettle, and continuously reacting for 2 hours to obtain the organic silicon modified polyurethane.
The preparation process of the epoxy corrosion-resistant waterproof coating comprises the following steps:
(1) preparing modified graphene oxide: adding graphene oxide into distilled water, heating to 60 ℃, adding sodium lignosulfonate, uniformly mixing and stirring, performing ultrasonic dispersion for 13min, placing in a stirring kettle, mechanically stirring at a high speed of 1400r/min for 18min, and performing vacuum drying in a vacuum drying oven to obtain modified graphene oxide for later use;
(2) preparing the composite epoxy resin: adding the modified graphene oxide into distilled water, adjusting the pH value to acidity, adding zinc oxide, placing the mixture into a water bath kettle at 80 ℃ for ultrasonic homogenization, taking out the mixture for high-speed centrifugation, placing the centrifuged precipitate into a hot air drying box for drying to obtain a dried precipitate, adding epoxy resin, heating to 55 ℃, performing magnetic stirring for 2 hours, then placing the dried precipitate into a high-pressure reaction kettle, and performing high-pressure stirring for 25 minutes at the rotating speed of 300r/min and the pressure of 9MPa to obtain composite epoxy resin for later use;
(3) compounding modified polyurethane: adding nano silicon dioxide into ethyl acetate, fully stirring, adding modified polyurethane, placing in a high-pressure reaction kettle, mixing and stirring at a rotating speed of 150r/min for 30min under the high pressure of 7MPa in the atmosphere of nitrogen, and obtaining a composite material for later use;
(4) preparation of component A: adding the composite epoxy resin into nano molybdenum disulfide and barium titanate, mixing, placing in a high-temperature water bath environment at 70 ℃, uniformly stirring, further continuously stirring for 25min in a low-temperature environment at 4 ℃, taking out, recovering to normal temperature, adding the composite material, heating to 70 ℃, and uniformly stirring to obtain a component A for later use;
(5) preparation of the component B: mixing the reactive diluent, the curing agent, the cross-linking agent and the plasticizer, mechanically stirring the mixture evenly in a high-temperature environment, and then cooling the mixture to the normal temperature to obtain the component B for later use.
Comparative example 1:
the epoxy corrosion-resistant waterproof coating comprises a component A and a component B which are equal in mass, wherein the component A comprises the following materials in parts by weight: 28 parts of epoxy resin, 13 parts of modified polyurethane, 6 parts of zinc oxide, 5 parts of nano silicon dioxide, 9 parts of ethyl acetate, 2.5 parts of nano molybdenum disulfide, 3 parts of graphene oxide and 2.5 parts of barium titanate; the component B comprises the following substances in parts by weight: 18 parts of reactive diluent, 4 parts of curing agent, 2.5 parts of cross-linking agent and 3 parts of plasticizer.
Wherein the reactive diluent is a mixture of phenyl glycidyl ether and resorcinol diglycidyl ether in a mass ratio of 2: 1; and the curing agent is one or a mixture of more of aminoethylpiperazine, diethylenetriamine and diethylaminopropylamine.
The preparation of the modified polyurethane comprises the following steps:
(1) dehydrating polypropylene glycol in a reaction kettle in vacuum, adding toluene diisocyanate and a dibutyltin laurate catalyst into the reaction kettle, controlling the temperature to be 80 ℃, and reacting for 2 hours;
(2) continuously adding 2, 2-bis (hydroxymethyl) propionic acid and acetone into the reaction kettle, and preserving heat for 2 hours at the temperature of 80 ℃;
(3) and continuously adding the hydroxyl silicone oil into the reaction kettle, and continuously reacting for 2 hours to obtain the organic silicon modified polyurethane.
The preparation process of the epoxy corrosion-resistant waterproof coating comprises the following steps:
(1) preparing the composite epoxy resin: adding graphene oxide into distilled water, adjusting the pH value to acidity, then adding zinc oxide, placing the mixture into a water bath kettle at 80 ℃ for ultrasonic homogenization, taking out the mixture for high-speed centrifugation, placing the centrifugal precipitate into a hot air drying box for drying to obtain a dried precipitate, adding epoxy resin, heating to 55 ℃, then performing magnetic stirring for 2 hours, then placing the dried precipitate into a high-pressure reaction kettle, and performing high-pressure stirring for 25 minutes at the rotating speed of 300r/min and the pressure of 9MPa to obtain composite epoxy resin for later use;
(2) compounding modified polyurethane: adding nano silicon dioxide into ethyl acetate, fully stirring, adding modified polyurethane, placing in a high-pressure reaction kettle, mixing and stirring at a rotating speed of 150r/min for 30min under the high pressure of 7MPa in the atmosphere of nitrogen, and obtaining a composite material for later use;
(3) preparation of component A: adding the composite epoxy resin into nano molybdenum disulfide and barium titanate, mixing, placing in a high-temperature water bath environment at 70 ℃, uniformly stirring, further continuously stirring for 25min in a low-temperature environment at 4 ℃, taking out, recovering to normal temperature, adding the composite material, heating to 70 ℃, and uniformly stirring to obtain a component A for later use;
(4) preparation of the component B: mixing the reactive diluent, the curing agent, the cross-linking agent and the plasticizer, mechanically stirring the mixture evenly in a high-temperature environment, and then cooling the mixture to the normal temperature to obtain the component B for later use.
Comparative example 2:
the epoxy corrosion-resistant waterproof coating comprises a component A and a component B which are equal in mass, wherein the component A comprises the following materials in parts by weight: 28 parts of epoxy resin, 13 parts of modified polyurethane, 5 parts of nano silicon dioxide, 9 parts of ethyl acetate, 2.5 parts of nano molybdenum disulfide, 3 parts of graphene oxide, 4 parts of sodium lignosulfonate and 2.5 parts of barium titanate; the component B comprises the following substances in parts by weight: 18 parts of reactive diluent, 4 parts of curing agent, 2.5 parts of cross-linking agent and 3 parts of plasticizer.
Wherein the reactive diluent is a mixture of phenyl glycidyl ether and resorcinol diglycidyl ether in a mass ratio of 2: 1; and the curing agent is one or a mixture of more of aminoethylpiperazine, diethylenetriamine and diethylaminopropylamine.
The preparation of the modified polyurethane comprises the following steps:
(1) dehydrating polypropylene glycol in a reaction kettle in vacuum, adding toluene diisocyanate and a dibutyltin laurate catalyst into the reaction kettle, controlling the temperature to be 80 ℃, and reacting for 2 hours;
(2) continuously adding 2, 2-bis (hydroxymethyl) propionic acid and acetone into the reaction kettle, and preserving heat for 2 hours at the temperature of 80 ℃;
(3) and continuously adding the hydroxyl silicone oil into the reaction kettle, and continuously reacting for 2 hours to obtain the organic silicon modified polyurethane.
The preparation process of the epoxy corrosion-resistant waterproof coating comprises the following steps:
(1) preparing modified graphene oxide: adding graphene oxide into distilled water, heating to 60 ℃, adding sodium lignosulfonate, uniformly mixing and stirring, performing ultrasonic dispersion for 13min, placing in a stirring kettle, mechanically stirring at a high speed of 1400r/min for 18min, and performing vacuum drying in a vacuum drying oven to obtain modified graphene oxide for later use;
(2) preparing the composite epoxy resin: adding the modified graphene oxide into epoxy resin, heating to 55 ℃, performing magnetic stirring for 2 hours, and then placing in a high-pressure reaction kettle to perform high-pressure stirring for 25 minutes at the rotating speed of 300r/min and the pressure of 9MPa to obtain composite epoxy resin for later use;
(3) compounding modified polyurethane: adding nano silicon dioxide into ethyl acetate, fully stirring, adding modified polyurethane, placing in a high-pressure reaction kettle, mixing and stirring at a rotating speed of 150r/min for 30min under the high pressure of 7MPa in the atmosphere of nitrogen, and obtaining a composite material for later use;
(4) preparation of component A: adding the composite epoxy resin into nano molybdenum disulfide and barium titanate, mixing, placing in a high-temperature water bath environment at 70 ℃, uniformly stirring, further continuously stirring for 25min in a low-temperature environment at 4 ℃, taking out, recovering to normal temperature, adding the composite material, heating to 70 ℃, and uniformly stirring to obtain a component A for later use;
(5) preparation of the component B: mixing the reactive diluent, the curing agent, the cross-linking agent and the plasticizer, mechanically stirring the mixture evenly in a high-temperature environment, and then cooling the mixture to the normal temperature to obtain the component B for later use.
Comparative example 3:
the epoxy corrosion-resistant waterproof coating comprises a component A and a component B which are equal in mass, wherein the component A comprises the following materials in parts by weight: 28 parts of epoxy resin, 13 parts of modified polyurethane, 6 parts of zinc oxide, 5 parts of nano silicon dioxide, 9 parts of ethyl acetate, 2.5 parts of nano molybdenum disulfide, 3 parts of graphene oxide and 4 parts of sodium lignosulfonate; the component B comprises the following substances in parts by weight: 18 parts of reactive diluent, 4 parts of curing agent, 2.5 parts of cross-linking agent and 3 parts of plasticizer.
Wherein the reactive diluent is a mixture of phenyl glycidyl ether and resorcinol diglycidyl ether in a mass ratio of 2: 1; and the curing agent is one or a mixture of more of aminoethylpiperazine, diethylenetriamine and diethylaminopropylamine.
The preparation of the modified polyurethane comprises the following steps:
(1) dehydrating polypropylene glycol in a reaction kettle in vacuum, adding toluene diisocyanate and a dibutyltin laurate catalyst into the reaction kettle, controlling the temperature to be 80 ℃, and reacting for 2 hours;
(2) continuously adding 2, 2-bis (hydroxymethyl) propionic acid and acetone into the reaction kettle, and preserving heat for 2 hours at the temperature of 80 ℃;
(3) and continuously adding the hydroxyl silicone oil into the reaction kettle, and continuously reacting for 2 hours to obtain the organic silicon modified polyurethane.
The preparation process of the epoxy corrosion-resistant waterproof coating comprises the following steps:
(1) preparing modified graphene oxide: adding graphene oxide into distilled water, heating to 60 ℃, adding sodium lignosulfonate, uniformly mixing and stirring, performing ultrasonic dispersion for 13min, placing in a stirring kettle, mechanically stirring at a high speed of 1400r/min for 18min, and performing vacuum drying in a vacuum drying oven to obtain modified graphene oxide for later use;
(2) preparing the composite epoxy resin: adding the modified graphene oxide into distilled water, adjusting the pH value to acidity, adding zinc oxide, placing the mixture into a water bath kettle at 80 ℃ for ultrasonic homogenization, taking out the mixture for high-speed centrifugation, placing the centrifuged precipitate into a hot air drying box for drying to obtain a dried precipitate, adding epoxy resin, heating to 55 ℃, performing magnetic stirring for 2 hours, then placing the dried precipitate into a high-pressure reaction kettle, and performing high-pressure stirring for 25 minutes at the rotating speed of 300r/min and the pressure of 9MPa to obtain composite epoxy resin for later use;
(3) compounding modified polyurethane: adding nano silicon dioxide into ethyl acetate, fully stirring, adding modified polyurethane, placing in a high-pressure reaction kettle, mixing and stirring at a rotating speed of 150r/min for 30min under the high pressure of 7MPa in the atmosphere of nitrogen, and obtaining a composite material for later use;
(4) preparation of component A: adding the composite epoxy resin into nano molybdenum disulfide, mixing, placing in a high-temperature water bath environment at 70 ℃, uniformly stirring, further continuously stirring for 25min in a low-temperature environment at 4 ℃, taking out, recovering to normal temperature, adding the composite material, heating to 70 ℃, and uniformly stirring to obtain a component A for later use;
(5) preparation of the component B: mixing the reactive diluent, the curing agent, the cross-linking agent and the plasticizer, mechanically stirring the mixture evenly in a high-temperature environment, and then cooling the mixture to the normal temperature to obtain the component B for later use.
Comparative example 4:
the epoxy corrosion-resistant waterproof coating comprises a component A and a component B which are equal in mass, wherein the component A comprises the following materials in parts by weight: 28 parts of epoxy resin, 13 parts of modified polyurethane, 6 parts of zinc oxide, 5 parts of nano silicon dioxide, 9 parts of ethyl acetate, 3 parts of graphene oxide, 4 parts of sodium lignosulfonate and 2.5 parts of barium titanate; the component B comprises the following substances in parts by weight: 18 parts of reactive diluent, 4 parts of curing agent, 2.5 parts of cross-linking agent and 3 parts of plasticizer.
Wherein the reactive diluent is a mixture of phenyl glycidyl ether and resorcinol diglycidyl ether in a mass ratio of 2: 1; and the curing agent is one or a mixture of more of aminoethylpiperazine, diethylenetriamine and diethylaminopropylamine.
The preparation of the modified polyurethane comprises the following steps:
(1) dehydrating polypropylene glycol in a reaction kettle in vacuum, adding toluene diisocyanate and a dibutyltin laurate catalyst into the reaction kettle, controlling the temperature to be 80 ℃, and reacting for 2 hours;
(2) continuously adding 2, 2-bis (hydroxymethyl) propionic acid and acetone into the reaction kettle, and preserving heat for 2 hours at the temperature of 80 ℃;
(3) and continuously adding the hydroxyl silicone oil into the reaction kettle, and continuously reacting for 2 hours to obtain the organic silicon modified polyurethane.
The preparation process of the epoxy corrosion-resistant waterproof coating comprises the following steps:
(1) preparing modified graphene oxide: adding graphene oxide into distilled water, heating to 60 ℃, adding sodium lignosulfonate, uniformly mixing and stirring, performing ultrasonic dispersion for 13min, placing in a stirring kettle, mechanically stirring at a high speed of 1400r/min for 18min, and performing vacuum drying in a vacuum drying oven to obtain modified graphene oxide for later use;
(2) preparing the composite epoxy resin: adding the modified graphene oxide into distilled water, adjusting the pH value to acidity, adding zinc oxide, placing the mixture into a water bath kettle at 80 ℃ for ultrasonic homogenization, taking out the mixture for high-speed centrifugation, placing the centrifuged precipitate into a hot air drying box for drying to obtain a dried precipitate, adding epoxy resin, heating to 55 ℃, performing magnetic stirring for 2 hours, then placing the dried precipitate into a high-pressure reaction kettle, and performing high-pressure stirring for 25 minutes at the rotating speed of 300r/min and the pressure of 9MPa to obtain composite epoxy resin for later use;
(3) compounding modified polyurethane: adding nano silicon dioxide into ethyl acetate, fully stirring, adding modified polyurethane, placing in a high-pressure reaction kettle, mixing and stirring at a rotating speed of 150r/min for 30min under the high pressure of 7MPa in the atmosphere of nitrogen, and obtaining a composite material for later use;
(4) preparation of component A: adding barium titanate into the composite epoxy resin, mixing, placing in a high-temperature water bath environment at 70 ℃, uniformly stirring, further continuously stirring for 25min in a low-temperature environment at 4 ℃, taking out, recovering to normal temperature, adding the composite material, heating to 70 ℃, and uniformly stirring to obtain a component A for later use;
(5) preparation of the component B: mixing the reactive diluent, the curing agent, the cross-linking agent and the plasticizer, mechanically stirring the mixture evenly in a high-temperature environment, and then cooling the mixture to the normal temperature to obtain the component B for later use.
And (3) detection:
the coatings prepared in the above examples 1 to 3 and comparative examples 1 to 4 were coated on concrete blocks of the same specification, and the coating thickness was 1.5 to 2.0mm, and the coating was carried out by mixing the component A and the component B in a ratio of 1: 1, and the adhesive strength, thermo-oxidative aging resistance, acid-base aging resistance and hydrophobicity of each coating were measured, and the specific results are shown in the following table:
Figure BDA0003179988900000131
to sum up, this application can effectively promote the acid and alkali resistance and the waterproof performance of coating.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. The corrosion-resistant waterproof epoxy coating is characterized by comprising a component A and a component B which are equal in mass, wherein the component A comprises the following components in parts by weight: 25-30 parts of epoxy resin, 12-14 parts of modified polyurethane, 4-8 parts of zinc oxide, 3-6 parts of nano silicon dioxide, 8-10 parts of ethyl acetate, 2-3 parts of nano molybdenum disulfide, 2-4 parts of graphene oxide, 2-6 parts of sodium lignosulfonate and 2-3 parts of barium titanate; the component B comprises the following substances in parts by weight: 12-24 parts of reactive diluent, 2-6 parts of curing agent, 2-3 parts of cross-linking agent and 1-4 parts of plasticizer.
2. The epoxy corrosion-resistant waterproof coating material of claim 1, wherein: the reactive diluent is a mixture of phenyl glycidyl ether and resorcinol diglycidyl ether in a mass ratio of 2: 1.
3. The epoxy corrosion-resistant waterproof coating material of claim 1, wherein: and the curing agent is one or a mixture of more of aminoethylpiperazine, diethylenetriamine and diethylaminopropylamine.
4. The epoxy corrosion-resistant waterproof coating material of claim 1, wherein: the preparation of the modified polyurethane comprises the following steps:
(1) dehydrating polypropylene glycol in a reaction kettle in vacuum, adding toluene diisocyanate and a catalyst into the reaction kettle, controlling the temperature to be 80 ℃, and reacting for 2 hours;
(2) continuously adding 2, 2-bis (hydroxymethyl) propionic acid and acetone into the reaction kettle, and preserving heat for 2 hours at the temperature of 80 ℃;
(3) and (3) continuously adding the hydroxyl silicone oil into the reaction kettle, and continuously reacting for 2 hours to obtain the modified polyurethane.
5. The epoxy corrosion-resistant waterproof coating material of claim 4, wherein: the catalyst is dibutyltin laurate.
6. The preparation process of the corrosion-resistant waterproof epoxy paint is characterized by comprising the following steps of:
(1) preparing modified graphene oxide: adding graphene oxide into distilled water, heating to 60 ℃, adding sodium lignosulfonate, mixing and stirring uniformly, performing ultrasonic dispersion for 10-15min, placing in a stirring kettle, mechanically stirring at a high speed, and performing vacuum drying in a vacuum drying oven to obtain modified graphene oxide for later use;
(2) preparing the composite epoxy resin: adding the modified graphene oxide into distilled water, adjusting the pH value to acidity, then adding zinc oxide, placing the mixture into a water bath kettle at 80 ℃ for ultrasonic homogenization, taking out the mixture for high-speed centrifugation, placing the centrifuged precipitate into a hot air drying box for drying to obtain a dried precipitate, adding epoxy resin into the dried precipitate, heating the dried precipitate to 50-60 ℃, then performing magnetic stirring for 2 hours, and then placing the dried precipitate into a high-pressure reaction kettle for high-pressure stirring for 20-30min to obtain composite epoxy resin for later use;
(3) compounding modified polyurethane: adding nano silicon dioxide into ethyl acetate, fully stirring, adding modified polyurethane, placing in a high-pressure reaction kettle, mixing and stirring at high pressure in the atmosphere of nitrogen for 30min to obtain a composite material for later use;
(4) preparation of component A: adding the composite epoxy resin into nano molybdenum disulfide and barium titanate, mixing, placing in a high-temperature water bath environment, stirring uniformly, continuing to stir for 20-30min in a low-temperature environment, taking out, recovering to normal temperature, adding the composite material, heating to 60-80 ℃, and stirring uniformly to obtain a component A for later use;
(5) preparation of the component B: mixing the reactive diluent, the curing agent, the cross-linking agent and the plasticizer, mechanically stirring the mixture evenly in a high-temperature environment, and then cooling the mixture to the normal temperature to obtain the component B for later use.
7. The preparation process of the corrosion-resistant waterproof epoxy paint as claimed in claim 6, wherein the corrosion-resistant waterproof epoxy paint is prepared by the following steps: the rotating speed of the high-speed mechanical stirring in the step (1) is 1200-1800r/min, and the stirring time is 15-20 min.
8. The preparation process of the corrosion-resistant waterproof epoxy paint as claimed in claim 6, wherein the corrosion-resistant waterproof epoxy paint is prepared by the following steps: the pressure of high-pressure stirring in the step (2) is 8-10MPa, and the stirring speed is 200-400 r/min.
9. The preparation process of the corrosion-resistant waterproof epoxy paint as claimed in claim 6, wherein the corrosion-resistant waterproof epoxy paint is prepared by the following steps: the pressure of the high-pressure mixing and stirring in the step (3) is 6-8MPa, and the stirring speed is 120-180 r/min.
10. The preparation process of the corrosion-resistant waterproof epoxy paint as claimed in claim 6, wherein the corrosion-resistant waterproof epoxy paint is prepared by the following steps: in the step (4), the stirring temperature of the high-temperature water bath environment is 60-80 ℃, and the continuous stirring temperature in the low-temperature environment is 2-6 ℃.
CN202110843657.4A 2021-07-26 2021-07-26 Preparation process of epoxy corrosion-resistant waterproof coating Pending CN113480918A (en)

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Application publication date: 20211008