CN113072868A - Wear-resistant and water-skid-resistant floor paint for civil air defense and preparation method thereof - Google Patents
Wear-resistant and water-skid-resistant floor paint for civil air defense and preparation method thereof Download PDFInfo
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- CN113072868A CN113072868A CN202110361153.9A CN202110361153A CN113072868A CN 113072868 A CN113072868 A CN 113072868A CN 202110361153 A CN202110361153 A CN 202110361153A CN 113072868 A CN113072868 A CN 113072868A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
Abstract
The invention discloses a wear-resistant waterproof and skid-resistant floor paint for civil air defense and a preparation method thereof, wherein the paint is prepared from a main coating, a solvent and a curing agent according to the mass ratio of (2-3): 12-15 parts of a mixture of 1.5-2.5 parts of a main coating, wherein the main coating comprises, by weight, 50-60 parts of polyurethane, 20-30 parts of bio-based epoxy resin, 5-7 parts of a filler, 2-3 parts of an auxiliary agent and 0.5-1.5 parts of an emulsifier, the solvent is one of absolute ethyl alcohol and acetone, and the curing agent comprises, by weight, 10-15 parts of ethylenediamine, 1-3 parts of diethylenetriamine, 15-20 parts of an anhydride curing agent and 4-5 parts of a kaolinite curing agent. This application has modified epoxy, uses the dehydrogenated rosin amine to modify it, obtains the epoxy that has the bio-based, and it has the effect of more excellent stability for traditional epoxy.
Description
Technical Field
The invention relates to the technical field of floor paint preparation, in particular to wear-resistant waterproof skid-resistant floor paint for civil air defense and a preparation method thereof.
Background
The floor paint is mainly prepared from oil, tree materials, colors, solvents and the like, and the main base material in the market at present is epoxy resin, because the epoxy resin has excellent chemical properties, the paint film has strong adhesive capacity and excellent heat resistance and electrical insulation performance, the floor paint has wide application in the paint field.
The epoxy floor paint is generally composed of epoxy resin, a solvent, a curing agent, a pigment and an auxiliary agent, has strong binding power, excellent water resistance and chemical properties, and very good physical and mechanical properties of a coating film, wherein the selection of the curing agent is very important, most of the common curing agents on the market at present are polyamine curing agents, but the effect achieved by the curing of the traditional polyamine curing agents cannot meet the requirements of people along with the change of a base material, so that the invention of the wear-resistant and water-skid-resistant floor paint for civil defense and the preparation method thereof are very important.
Disclosure of Invention
The invention aims to provide wear-resistant waterproof and slippery floor paint for civil air defense and a preparation method thereof, and aims to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: the wear-resistant waterproof and antiskid floor paint for civil air defense comprises 2-3 mass percent of main coating, solvent and curing agent: 12-15: 1.5-2.5;
the main coating comprises the following raw materials, by weight, 50-60 parts of polyurethane, 20-30 parts of bio-based epoxy resin, 5-7 parts of filler, 2-3 parts of auxiliary agent and 0.5-1.5 parts of emulsifier;
the solvent is one of absolute ethyl alcohol and acetone;
the curing agent comprises, by weight, 10-15 parts of ethylenediamine, 1-3 parts of diethylenetriamine, 15-20 parts of anhydride curing agent and 4-5 parts of kaolinite curing agent.
Further, the bio-based epoxy resin is prepared from dehydroabietylamine and epoxy chloropropane.
Further, the filler is a mixture of ceramic powder and titanium dioxide, and the ceramic powder is formed by mixing aluminum oxide and silicon carbide according to a mass ratio of 1.3-1.5: 1.
Further, the acid anhydride curing agent is methylhexahydrophthalic anhydride.
Further, the kaolinite curing agent is prepared from kaolinite and 3-aminopropyltriethoxysilane.
Furthermore, the auxiliary agent is formed by mixing a defoaming agent and a flatting agent according to the mass ratio of 1-2:2-4: 1-3.
Furthermore, the defoaming agent is one of an organic silicon defoaming agent and a mineral oil defoaming agent, and the leveling agent is one or a mixture of polyacrylate and cellulose acetate butyrate.
A preparation method of wear-resistant waterproof and skidproof floor paint for civil air defense, which comprises the following steps,
(1) preparation of bio-based epoxy resin: mixing dehydroabietylamine and epoxy chloropropane, adding deionized water, stirring, heating to 40-42 ℃, stirring for 3-4 days, cooling to 23-25 ℃, adding tetraethylammonium bromide and sodium hydroxide, stirring, heating to 35-37 ℃, reacting for 3-4 hours, separating after the reaction is finished, and washing to obtain the bio-based epoxy resin;
(2) preparation of the curing agent:
mixing ethylenediamine and acetic acid, adding a catalyst, heating at the temperature of 225 ℃ and 230 ℃, reacting for 2-3h, filtering to obtain a mixture A, and washing and recycling the filtered solid;
when the curing agent is selected, the acid anhydride curing agent is used as a main body, the ethylenediamine and the diethylenetriamine are added, the acetic acid is added in the preparation process, the added acetic acid can react with the ethylenediamine to generate the 4-methylimidazole, and the 4-methylimidazole can reduce the curing temperature, so that the effect of accelerating curing is achieved.
Secondly, grinding the kaolinite, adding cyclohexane, stirring, adding 3-aminopropyl triethoxysilane after stirring uniformly, stirring, heating at the temperature of 80-82 ℃, centrifuging, and washing to obtain the kaolinite curing agent;
the anti-skidding performance of product can be strengthened in the addition of kaolinite to 3-aminopropyl triethoxysilane has been added on the basis of this application adding kaolinite, carries out the silane modification to kaolinite, and kaolinite can promote the curing effect of curing agent, avoids the consumption of ethylenediamine, leads to the problem that the curing effect of product descends, and can also strengthen the mechanical properties of product.
According to the method, when the curing agent is mainly an acid anhydride curing agent, the generated 4-methylimidazole is used as a catalyst, when the curing agent is cured, the 4-methylimidazole can generate carboxylic acid groups, the groups can promote the opening of an acid anhydride ring, and the acid anhydride ring reacts with an epoxy compound to generate alkoxide ions, the alkoxide ions can react with another acid anhydride to generate the carboxylic acid groups, and the steps are repeated, the modified kaolinite has hydroxyl groups on the surface, and the hydroxyl groups can promote the reaction of the epoxy groups and the acid anhydride, so that the curing efficiency is enhanced, and the activation energy is reduced.
Mixing the mixture A, the kaolinite curing agent, the diethylenetriamine and the anhydride curing agent, and stirring to obtain a curing agent;
the conventional curing agent is usually selected mainly from polyamine, while the curing agent in the application is mainly an acid anhydride curing agent, because the component of the coating in the application is epoxy resin containing a biological group modified by dehydroabietylamine, the conventional polyamine is used as the curing agent to form a poor crosslinking network, and the acid anhydride curing agent is used for curing the biological epoxy resin to enable the biological epoxy resin to have a small curing shrinkage rate, and the mechanical strength after curing is higher than that of the conventional amine curing.
According to the application, methylhexahydrophthalic anhydride is selected from anhydride curing agents, the methylhexahydrophthalic anhydride can be matched with 4-methylimidazole, and the 4-methylimidazole can be used as a catalyst, so that the curing temperature can be reduced, and the service life of a product coating can be prolonged.
(3) Preparing a main coating: adding the obtained bio-based epoxy resin and polyurethane into a reaction kettle, heating, adding a filler and an auxiliary agent, and stirring at a high speed to obtain a main coating;
(4) preparing floor paint: and mixing the obtained main coating with a solvent and a curing agent according to a mass ratio, coating the mixture on the surface of a matrix, and heating and curing to obtain the floor paint.
Further, in the step (2), the mass ratio of the added acetic acid to the ethylenediamine is 1.3-1.5: 1.
In the preparation process of the curing agent, acetic acid and ethylenediamine are mixed and dehydrogenated in the presence of a catalyst to generate methyl imidazole, but imidazoline is also generated as a byproduct, 225-230 ℃ is limited in reaction temperature, and imidazoline as the byproduct can be mixed with acetic acid to generate the ethylenediamine compound at the temperature, so that the added acetic acid amount needs to be limited, the mass ratio of the added amount to the ethylenediamine is limited to 1.3-1.5:1, the minimum content of the byproduct is ensured, and the generated ethylenediamine compound can also be used as the curing agent.
Further, the mass ratio of the added kaolinite powder to the 3-aminopropyltriethoxysilane is 0.8-0.95: 1.
Compared with the prior art, the invention has the following beneficial effects: the epoxy resin has excellent chemical properties, a paint film has strong adhesive capacity, and the epoxy resin also has excellent heat resistance and electrical insulation performance and is widely applied in the field of paint.
Realize that terrace paint has wear-resisting, skid-proof effect accessible adds the filler realization, the purposeful ceramic powder of having selected of this application when selecting the filler, the reason can not react with the bio-based epoxy that this application added with ceramic powder, polyurethane and solvent, can not react in the preparation process, lead to the quality of product coating unqualified, ceramic powder is because its self nature, has better wear-resisting and anti-skidding performance for quartz sand, and ceramic powder has certain spatial structure, can increase the adhesive force of product.
In order to enhance the curing efficiency of the product and accelerate the curing time, the curing agent is processed, the temperature rise rate can reach 15 ℃/min during curing after the curing, and the best curing effect can be achieved after the curing at the temperature rise rate.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and 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 utility model provides a people's air defense is with wear-resisting, waterproof smooth terrace paint, by 2 of main coating, solvent and curing agent according to the mass ratio: 12: 1.5;
the main coating comprises the following raw materials, by weight, 50 parts of polyurethane, 20 parts of bio-based epoxy resin, 5 parts of filler, 2 parts of auxiliary agent and 0.5 part of emulsifier;
the solvent is one of absolute ethyl alcohol and acetone;
the curing agent comprises the following raw materials, by weight, 10 parts of ethylenediamine, 1 part of diethylenetriamine, 15 parts of anhydride curing agent and 4 parts of kaolinite curing agent.
The bio-based epoxy resin is prepared from dehydroabietylamine and epoxy chloropropane.
The filler is a mixture of ceramic powder and titanium dioxide, and the ceramic powder is formed by mixing aluminum oxide and silicon carbide according to the mass ratio of 1.3-1.5: 1.
The acid anhydride curing agent is methylhexahydrophthalic anhydride.
The kaolinite curing agent is prepared from kaolinite and 3-aminopropyl triethoxysilane.
The auxiliary agent is formed by mixing a defoaming agent and a flatting agent according to the mass ratio of 1:2: 1.
The defoaming agent is one of an organic silicon defoaming agent and a mineral oil defoaming agent, and the leveling agent is one or a mixture of polyacrylate and cellulose acetate butyrate.
A preparation method of wear-resistant waterproof and skidproof floor paint for civil air defense, which comprises the following steps,
(1) preparation of bio-based epoxy resin: mixing dehydroabietylamine and epoxy chloropropane, adding deionized water, stirring, heating to 40 ℃, stirring for 3 days, cooling to 23 ℃, adding tetraethylammonium bromide and sodium hydroxide, stirring, heating to 35 ℃, reacting for 3 hours, separating after the reaction is finished, and washing to obtain the bio-based epoxy resin;
(2) preparation of the curing agent:
mixing ethylenediamine and acetic acid, adding a catalyst into the mixture at a mass ratio of 1.3:1, heating the mixture at 225 ℃ for 2 hours, filtering the mixture to obtain a mixture A, and washing the filtered solid for recycling;
grinding kaolinite, adding cyclohexane, stirring, adding 3-aminopropyltriethoxysilane after stirring uniformly, wherein the mass ratio of the added kaolinite powder to the 3-aminopropyltriethoxysilane is 0.8:1, stirring, heating at the temperature of 80 ℃, centrifuging, and washing to obtain a kaolinite curing agent;
mixing the mixture A, the kaolinite curing agent, the diethylenetriamine and the anhydride curing agent, and stirring to obtain a curing agent;
(3) preparing a main coating: adding the obtained bio-based epoxy resin and polyurethane into a reaction kettle, heating, adding a filler and an auxiliary agent, and stirring at a high speed to obtain a main coating;
(4) preparing floor paint: and mixing the obtained main coating with a solvent and a curing agent according to a mass ratio, coating the mixture on the surface of a matrix, and heating and curing to obtain the floor paint.
Example 2
The utility model provides a people's air defense is with wear-resisting, waterproof smooth terrace paint, by 2.5 of main coating, solvent and curing agent according to the mass ratio: 13: 2;
the main coating comprises the following raw materials, by weight, 55 parts of polyurethane, 25 parts of bio-based epoxy resin, 6 parts of filler, 3 parts of auxiliary agent and 1.0 part of emulsifier;
the solvent is one of absolute ethyl alcohol and acetone;
the curing agent comprises the following raw materials, by weight, 13 parts of ethylenediamine, 2 parts of diethylenetriamine, 17 parts of anhydride curing agent and 5 parts of kaolinite curing agent.
The bio-based epoxy resin is prepared from dehydroabietylamine and epoxy chloropropane.
The filler is a mixture of ceramic powder and titanium dioxide, and the ceramic powder is formed by mixing aluminum oxide and silicon carbide according to the mass ratio of 1.3-1.5: 1.
The acid anhydride curing agent is methylhexahydrophthalic anhydride.
The kaolinite curing agent is prepared from kaolinite and 3-aminopropyl triethoxysilane.
The auxiliary agent is formed by mixing a defoaming agent and a flatting agent according to the mass ratio of 2:3: 2.
The defoaming agent is one of an organic silicon defoaming agent and a mineral oil defoaming agent, and the leveling agent is one or a mixture of polyacrylate and cellulose acetate butyrate.
A preparation method of wear-resistant waterproof and skidproof floor paint for civil air defense, which comprises the following steps,
(1) preparation of bio-based epoxy resin: mixing dehydroabietylamine and epoxy chloropropane, adding deionized water, stirring, heating to 41 ℃, stirring for 3.5 days, cooling to 24 ℃, adding tetraethylammonium bromide and sodium hydroxide, stirring, heating to 36 ℃, reacting for 3.5 hours, separating after the reaction is finished, and washing to obtain the bio-based epoxy resin;
(2) preparation of the curing agent:
mixing ethylenediamine and acetic acid, adding a catalyst into the mixture, heating the mixture at the temperature of 227 ℃ for 2.5 hours, filtering the mixture to obtain a mixture A, and washing the filtered solid for recycling, wherein the mass ratio of the added acetic acid to the ethylenediamine is 1.4: 1;
grinding kaolinite, adding cyclohexane, stirring, adding 3-aminopropyltriethoxysilane after stirring uniformly, wherein the mass ratio of the added kaolinite powder to the 3-aminopropyltriethoxysilane is 0.9:1, stirring, heating at the temperature of 81 ℃, centrifuging, and washing to obtain a kaolinite curing agent;
mixing the mixture A, the kaolinite curing agent, the diethylenetriamine and the anhydride curing agent, and stirring to obtain a curing agent;
(3) preparing a main coating: adding the obtained bio-based epoxy resin and polyurethane into a reaction kettle, heating, adding a filler and an auxiliary agent, and stirring at a high speed to obtain a main coating;
(4) preparing floor paint: and mixing the obtained main coating with a solvent and a curing agent according to a mass ratio, coating the mixture on the surface of a matrix, and heating and curing to obtain the floor paint.
Example 3
The utility model provides a people's air defense is with wear-resisting, waterproof and slippery floor paint, by main coating, solvent and curing agent according to 3 of mass ratio: 15: 2.5;
the main coating comprises the following raw materials, by weight, 60 parts of polyurethane, 30 parts of bio-based epoxy resin, 7 parts of filler, 3 parts of auxiliary agent and 1.5 parts of emulsifier;
the solvent is one of absolute ethyl alcohol and acetone;
the curing agent comprises the following raw materials, by weight, 15 parts of ethylenediamine, 3 parts of diethylenetriamine, 20 parts of anhydride curing agent and 5 parts of kaolinite curing agent.
The bio-based epoxy resin is prepared from dehydroabietylamine and epoxy chloropropane.
The filler is a mixture of ceramic powder and titanium dioxide, and the ceramic powder is formed by mixing aluminum oxide and silicon carbide according to the mass ratio of 1.5: 1.
The acid anhydride curing agent is methylhexahydrophthalic anhydride.
The kaolinite curing agent is prepared from kaolinite and 3-aminopropyl triethoxysilane.
The auxiliary agent is formed by mixing a defoaming agent and a flatting agent according to the mass ratio of 2:4: 3.
The defoaming agent is one of an organic silicon defoaming agent and a mineral oil defoaming agent, and the leveling agent is one or a mixture of polyacrylate and cellulose acetate butyrate.
A preparation method of wear-resistant waterproof and skidproof floor paint for civil air defense, which comprises the following steps,
(1) preparation of bio-based epoxy resin: mixing dehydroabietylamine and epoxy chloropropane, adding deionized water, stirring, heating to 42 ℃, stirring for 4 days, cooling to 25 ℃, adding tetraethylammonium bromide and sodium hydroxide, stirring, heating to 37 ℃, reacting for 4 hours, separating after the reaction is finished, and washing to obtain the bio-based epoxy resin;
(2) preparation of the curing agent:
mixing ethylenediamine and acetic acid, adding a catalyst into the mixture, heating the mixture at 230 ℃ for 3 hours, filtering the mixture to obtain a mixture A, and washing the filtered solid for recycling, wherein the mass ratio of the added acetic acid to the ethylenediamine is 1.5: 1;
grinding kaolinite, adding cyclohexane, stirring, adding 3-aminopropyltriethoxysilane after stirring uniformly, wherein the mass ratio of the added kaolinite powder to the 3-aminopropyltriethoxysilane is 0.95:1, stirring, heating at 82 ℃, centrifuging, and washing to obtain a kaolinite curing agent;
mixing the mixture A, the kaolinite curing agent, the diethylenetriamine and the anhydride curing agent, and stirring to obtain a curing agent;
(3) preparing a main coating: adding the obtained bio-based epoxy resin and polyurethane into a reaction kettle, heating, adding a filler and an auxiliary agent, and stirring at a high speed to obtain a main coating;
(4) preparing floor paint: and mixing the obtained main coating with a solvent and a curing agent according to a mass ratio, coating the mixture on the surface of a matrix, and heating and curing to obtain the floor paint.
Comparative example 1
The utility model provides a people's air defense is with wear-resisting, waterproof and slippery floor paint, by main coating, solvent and curing agent according to 3 of mass ratio: 15: 2.5;
the main coating comprises the following raw materials, by weight, 60 parts of polyurethane, 30 parts of bio-based epoxy resin, 7 parts of filler, 3 parts of auxiliary agent and 1.5 parts of emulsifier;
the solvent is one of absolute ethyl alcohol and acetone;
the curing agent comprises the following raw materials, by weight, 15 parts of ethylenediamine and 3 parts of diethylenetriamine.
The bio-based epoxy resin is prepared from dehydroabietylamine and epoxy chloropropane.
The filler is a mixture of ceramic powder and titanium dioxide, and the ceramic powder is formed by mixing aluminum oxide and silicon carbide according to the mass ratio of 1.5: 1.
The acid anhydride curing agent is methylhexahydrophthalic anhydride.
The auxiliary agent is formed by mixing a defoaming agent and a flatting agent according to the mass ratio of 2:4: 3.
The defoaming agent is one of an organic silicon defoaming agent and a mineral oil defoaming agent, and the leveling agent is one or a mixture of polyacrylate and cellulose acetate butyrate.
A preparation method of wear-resistant waterproof and skidproof floor paint for civil air defense, which comprises the following steps,
(1) preparation of bio-based epoxy resin: mixing dehydroabietylamine and epoxy chloropropane, adding deionized water, stirring, heating to 42 ℃, stirring for 4 days, cooling to 25 ℃, adding tetraethylammonium bromide and sodium hydroxide, stirring, heating to 37 ℃, reacting for 4 hours, separating after the reaction is finished, and washing to obtain the bio-based epoxy resin;
(2) preparation of the curing agent: mixing ethylenediamine and diethylenetriamine, and stirring to obtain a curing agent;
(3) preparing a main coating: adding the obtained bio-based epoxy resin and polyurethane into a reaction kettle, heating, adding a filler and an auxiliary agent, and stirring at a high speed to obtain a main coating;
(4) preparing floor paint: and mixing the obtained main coating with a solvent and a curing agent according to a mass ratio, coating the mixture on the surface of a matrix, and heating and curing to obtain the floor paint.
Comparative example 2
The utility model provides a people's air defense is with wear-resisting, waterproof and slippery floor paint, by main coating, solvent and curing agent according to 3 of mass ratio: 15: 2.5;
the main coating comprises the following raw materials, by weight, 60 parts of polyurethane, 30 parts of bio-based epoxy resin, 7 parts of filler, 3 parts of auxiliary agent and 1.5 parts of emulsifier;
the solvent is one of absolute ethyl alcohol and acetone;
the curing agent comprises the following raw materials, by weight, 15 parts of ethylenediamine, 3 parts of diethylenetriamine and 20 parts of anhydride curing agent.
The bio-based epoxy resin is prepared from dehydroabietylamine and epoxy chloropropane.
The filler is a mixture of ceramic powder and titanium dioxide, and the ceramic powder is formed by mixing aluminum oxide and silicon carbide according to the mass ratio of 1.5: 1.
The acid anhydride curing agent is methylhexahydrophthalic anhydride.
The auxiliary agent is formed by mixing a defoaming agent and a flatting agent according to the mass ratio of 2:4: 3.
The defoaming agent is one of an organic silicon defoaming agent and a mineral oil defoaming agent, and the leveling agent is one or a mixture of polyacrylate and cellulose acetate butyrate.
A preparation method of wear-resistant waterproof and skidproof floor paint for civil air defense, which comprises the following steps,
(1) preparation of bio-based epoxy resin: mixing dehydroabietylamine and epoxy chloropropane, adding deionized water, stirring, heating to 42 ℃, stirring for 4 days, cooling to 25 ℃, adding tetraethylammonium bromide and sodium hydroxide, stirring, heating to 37 ℃, reacting for 4 hours, separating after the reaction is finished, and washing to obtain the bio-based epoxy resin;
(2) preparation of the curing agent:
mixing ethylenediamine and acetic acid, adding a catalyst into the mixture, heating the mixture at 230 ℃ for 3 hours, filtering the mixture to obtain a mixture A, and washing the filtered solid for recycling, wherein the mass ratio of the added acetic acid to the ethylenediamine is 1.5: 1;
mixing the mixture A, diethylenetriamine and an anhydride curing agent, and stirring to obtain a curing agent;
(3) preparing a main coating: adding the obtained bio-based epoxy resin and polyurethane into a reaction kettle, heating, adding a filler and an auxiliary agent, and stirring at a high speed to obtain a main coating;
(4) preparing floor paint: and mixing the obtained main coating with a solvent and a curing agent according to a mass ratio, coating the mixture on the surface of a matrix, and heating and curing to obtain the floor paint.
Comparative example 3
The utility model provides a people's air defense is with wear-resisting, waterproof and slippery floor paint, by main coating, solvent and curing agent according to 3 of mass ratio: 15: 2.5;
the main coating comprises the following raw materials, by weight, 60 parts of polyurethane, 30 parts of bio-based epoxy resin, 7 parts of filler, 3 parts of auxiliary agent and 1.5 parts of emulsifier;
the solvent is one of absolute ethyl alcohol and acetone;
the curing agent comprises the following raw materials, by weight, 15 parts of ethylenediamine, 3 parts of diethylenetriamine, 20 parts of anhydride curing agent and 5 parts of kaolinite curing agent.
The bio-based epoxy resin is prepared from dehydroabietylamine and epoxy chloropropane.
The filler is a mixture of ceramic powder and titanium dioxide, and the ceramic powder is formed by mixing aluminum oxide and silicon carbide according to the mass ratio of 1.5: 1.
The acid anhydride curing agent is methylhexahydrophthalic anhydride.
The kaolinite curing agent is prepared from kaolinite and 3-aminopropyl triethoxysilane.
The auxiliary agent is formed by mixing a defoaming agent and a flatting agent according to the mass ratio of 2:4: 3.
The defoaming agent is one of an organic silicon defoaming agent and a mineral oil defoaming agent, and the leveling agent is one or a mixture of polyacrylate and cellulose acetate butyrate.
A preparation method of wear-resistant waterproof and skidproof floor paint for civil air defense, which comprises the following steps,
(1) preparation of bio-based epoxy resin: mixing dehydroabietylamine and epoxy chloropropane, adding deionized water, stirring, heating to 42 ℃, stirring for 4 days, cooling to 25 ℃, adding tetraethylammonium bromide and sodium hydroxide, stirring, heating to 37 ℃, reacting for 4 hours, separating after the reaction is finished, and washing to obtain the bio-based epoxy resin;
(2) preparation of the curing agent:
mixing ethylenediamine and acetic acid, adding a catalyst into the mixture, heating the mixture at 230 ℃ for 3 hours, filtering the mixture to obtain a mixture A, and washing the filtered solid for recycling, wherein the mass ratio of the added acetic acid to the ethylenediamine is 0.8: 1;
grinding kaolinite, adding cyclohexane, stirring, adding 3-aminopropyltriethoxysilane after stirring uniformly, wherein the mass ratio of the added kaolinite powder to the 3-aminopropyltriethoxysilane is 0.95:1, stirring, heating at 82 ℃, centrifuging, and washing to obtain a kaolinite curing agent;
mixing the mixture A, the kaolinite curing agent, the diethylenetriamine and the anhydride curing agent, and stirring to obtain a curing agent;
(3) preparing a main coating: adding the obtained bio-based epoxy resin and polyurethane into a reaction kettle, heating, adding a filler and an auxiliary agent, and stirring at a high speed to obtain a main coating;
(4) preparing floor paint: and mixing the obtained main coating with a solvent and a curing agent according to a mass ratio, coating the mixture on the surface of a matrix, and heating and curing to obtain the floor paint.
Comparative example 4
The utility model provides a people's air defense is with wear-resisting, waterproof and slippery floor paint, by main coating, solvent and curing agent according to 3 of mass ratio: 15: 2.5;
the main coating comprises the following raw materials, by weight, 60 parts of polyurethane, 30 parts of bio-based epoxy resin, 7 parts of filler, 3 parts of auxiliary agent and 1.5 parts of emulsifier;
the solvent is one of absolute ethyl alcohol and acetone;
the curing agent comprises the following raw materials, by weight, 15 parts of ethylenediamine, 3 parts of diethylenetriamine, 20 parts of anhydride curing agent and 5 parts of kaolinite curing agent.
The bio-based epoxy resin is prepared from dehydroabietylamine and epoxy chloropropane.
The filler is a mixture of quartz sand and titanium dioxide.
The acid anhydride curing agent is methylhexahydrophthalic anhydride.
The kaolinite curing agent is prepared from kaolinite and 3-aminopropyl triethoxysilane.
The auxiliary agent is formed by mixing a defoaming agent and a flatting agent according to the mass ratio of 2:4: 3.
The defoaming agent is one of an organic silicon defoaming agent and a mineral oil defoaming agent, and the leveling agent is one or a mixture of polyacrylate and cellulose acetate butyrate.
A preparation method of wear-resistant waterproof and skidproof floor paint for civil air defense, which comprises the following steps,
(1) preparation of bio-based epoxy resin: mixing dehydroabietylamine and epoxy chloropropane, adding deionized water, stirring, heating to 42 ℃, stirring for 4 days, cooling to 25 ℃, adding tetraethylammonium bromide and sodium hydroxide, stirring, heating to 37 ℃, reacting for 4 hours, separating after the reaction is finished, and washing to obtain the bio-based epoxy resin;
(2) preparation of the curing agent:
mixing ethylenediamine and acetic acid, adding a catalyst into the mixture, heating the mixture at 230 ℃ for 3 hours, filtering the mixture to obtain a mixture A, and washing the filtered solid for recycling, wherein the mass ratio of the added acetic acid to the ethylenediamine is 1.5: 1;
grinding kaolinite, adding cyclohexane, stirring, adding 3-aminopropyltriethoxysilane after stirring uniformly, wherein the mass ratio of the added kaolinite powder to the 3-aminopropyltriethoxysilane is 0.95:1, stirring, heating at 82 ℃, centrifuging, and washing to obtain a kaolinite curing agent;
mixing the mixture A, the kaolinite curing agent, the diethylenetriamine and the anhydride curing agent, and stirring to obtain a curing agent;
(3) preparing a main coating: adding the obtained bio-based epoxy resin and polyurethane into a reaction kettle, heating, adding a filler and an auxiliary agent, and stirring at a high speed to obtain a main coating;
(4) preparing floor paint: and mixing the obtained main coating with a solvent and a curing agent according to a mass ratio, coating the mixture on the surface of a matrix, and heating and curing to obtain the floor paint.
Experiment of
And a comparative example 1, a comparative example 2, a comparative example 3 and a comparative example 4 are set by using the comparison of the example 3, wherein a conventional ethylenediamine curing agent is used in the comparative example 1, a kaolinite curing agent is not added in the comparative example 2, the addition amount of acetic acid is reduced in the comparative example 3, the mass ratio of the acetic acid to the ethylenediamine is reduced to 0.8:1, and quartz sand and titanium dioxide are used as fillers in the comparative example 4 to carry out a control experiment.
The impact resistance test was carried out according to GB/T1731-1993 for example 1, example 2, example 3, comparative example 1, comparative example 2, comparative example 3 and comparative example 4, and the abrasion resistance test was carried out according to GB/T1768-2006, with the following results,
| experimental group | Impact resistance (cm) | Abrasion resistance (750g/500r) |
| Example 1 | 66 | ≤0.01 |
| Example 2 | 65 | ≤0.01 |
| Example 3 | 68 | ≤0.01 |
| Comparative example 1 | 62 | ≤0.01 |
| Comparative example 2 | 59 | 0.03 |
| Comparative example 3 | 63 | ≤0.01 |
| Comparative example 4 | 61 | 0.07 |
Watch 1
The use of the conventional ethylenediamine curing agent in comparative example 1 resulted in impact resistance relative to examples 1, 2 and 3, because the amine curing agent forms a poor cross-linked network with epoxy groups, resulting in a decrease in impact resistance of the product.
In comparative example 2, no kaolinite-based curing agent was added, resulting in a decrease in impact resistance and abrasion resistance of the product.
In comparative example 3, decreasing the amount of acetic acid added to decrease the mass ratio of ethylenediamine to 0.8:1 resulted in a decrease in impact resistance of the product because the by-products were not further reacted during the preparation process, resulting in a decrease in curing effect.
The quartz sand and the titanium dioxide are used as the filler in the comparative example 4, so that the wear resistance of the product is reduced.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The utility model provides a people's air defense is with wear-resisting, waterproof smooth terrace paint which characterized in that: the floor paint is prepared from a main coating, a solvent and a curing agent according to the mass ratio of 2-3: 12-15: 1.5-2.5;
the main coating comprises the following raw materials, by weight, 50-60 parts of polyurethane, 20-30 parts of bio-based epoxy resin, 5-7 parts of filler, 2-3 parts of auxiliary agent and 0.5-1.5 parts of emulsifier;
the solvent is one of absolute ethyl alcohol and acetone;
the curing agent comprises, by weight, 10-15 parts of ethylenediamine, 1-3 parts of diethylenetriamine, 15-20 parts of anhydride curing agent and 4-5 parts of kaolinite curing agent.
2. The wear-resistant and water-skid-resistant floor paint for civil air defense as claimed in claim 1, which is characterized in that: the bio-based epoxy resin is prepared from dehydroabietylamine and epoxy chloropropane.
3. The wear-resistant and water-skid-resistant floor paint for civil air defense as claimed in claim 1, which is characterized in that: the filler is a mixture of ceramic powder and titanium dioxide, and the ceramic powder is formed by mixing aluminum oxide and silicon carbide according to the mass ratio of 1.3-1.5: 1.
4. The wear-resistant and water-skid-resistant floor paint for civil air defense as claimed in claim 1, which is characterized in that: the acid anhydride curing agent is methylhexahydrophthalic anhydride.
5. The wear-resistant and water-skid-resistant floor paint for civil air defense as claimed in claim 1, which is characterized in that: the kaolinite curing agent is prepared from kaolinite and 3-aminopropyl triethoxysilane.
6. The wear-resistant and water-skid-resistant floor paint for civil air defense as claimed in claim 1, which is characterized in that: the auxiliary agent is formed by mixing a defoaming agent and a flatting agent according to the mass ratio of 1-2:2-4: 1-3.
7. The wear-resistant and water-skid-resistant floor paint for civil air defense as claimed in claim 1, which is characterized in that: the defoaming agent is one of an organic silicon defoaming agent and a mineral oil defoaming agent, and the leveling agent is one or a mixture of polyacrylate and cellulose acetate butyrate.
8. A preparation method of wear-resistant and water-skid-resistant floor paint for civil air defense is characterized by comprising the following steps: the steps are as follows,
(1) preparation of bio-based epoxy resin: mixing dehydroabietylamine and epoxy chloropropane, adding deionized water, stirring, heating to 40-42 ℃, stirring for 3-4 days, cooling to 23-25 ℃, adding tetraethylammonium bromide and sodium hydroxide, stirring, heating to 35-37 ℃, reacting for 3-4 hours, separating after the reaction is finished, and washing to obtain the bio-based epoxy resin;
(2) preparation of the curing agent:
mixing ethylenediamine and acetic acid, adding a catalyst, heating at the temperature of 225 ℃ and 230 ℃, reacting for 2-3h, filtering to obtain a mixture A, and washing and recycling the filtered solid;
secondly, grinding the kaolinite, adding cyclohexane, stirring, adding 3-aminopropyl triethoxysilane after stirring uniformly, stirring, heating at the temperature of 80-82 ℃, centrifuging, and washing to obtain the kaolinite curing agent;
mixing the mixture A, the kaolinite curing agent, the diethylenetriamine and the anhydride curing agent, and stirring to obtain a curing agent;
(3) preparing a main coating: adding the obtained bio-based epoxy resin and polyurethane into a reaction kettle, heating, adding a filler and an auxiliary agent, and stirring at a high speed to obtain a main coating;
(4) preparing floor paint: and mixing the obtained main coating with a solvent and a curing agent according to a mass ratio, coating the mixture on the surface of a matrix, and heating and curing to obtain the floor paint.
9. The preparation method of the wear-resistant and water-skid-resistant floor paint for civil air defense as claimed in claim 9, wherein the preparation method comprises the following steps: in the step (2), the mass ratio of the added acetic acid to the ethylenediamine is 1.3-1.5: 1.
10. The preparation method of the wear-resistant and water-skid-resistant floor paint for civil air defense as claimed in claim 9, wherein the preparation method comprises the following steps: the mass ratio of the added kaolinite powder to the 3-aminopropyltriethoxysilane is 0.8-0.95: 1.
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