KR102511372B1 - A method for producing a water-soluble epoxy composition containing nano-silica and a method for constructing a flooring material using the same - Google Patents

Abstract

The present invention relates to a manufacturing method of a water-soluble epoxy composition containing nano-silica, and more specifically, it is a technical challenge to provide a manufacturing method of an epoxy composition having low VOCs levels and excellent semi-incombustible properties applied to floors of parking lots and rooftops of buildings and the like. The manufacturing method of the water-soluble epoxy composition containing the nano-silica comprises the following steps of: manufacturing a water-soluble hybrid resin; stabilizing the resin; dispersing the composition; manufacturing a main agent part; manufacturing a curing agent part; and mixing the main agent part and the curing agent part in a weight ratio of 3 to 5 : 1.

Description

A method for producing a water-soluble epoxy composition containing nano-silica and a method for constructing a flooring material using the same}

The present invention relates to a method for preparing a water-soluble epoxy composition containing nano-silica and a method for constructing a flooring material using the same.

Flooring is a material that is constructed on the floor of a building, such as corridors, warehouses, schools, factories, hospitals, parking lots, and rooftops. .

Among them, in the case of parking lot flooring, it is common to be composed of concrete materials. In relation to this, the concrete floor has low chemical resistance, such as acid resistance and chemical resistance, and a poor structure, which is not only harmful to the environment but also deteriorates by carbon dioxide gas in the air. Accordingly, by constructing a separate flooring material on the surface of the concrete, effects such as aesthetic improvement and practicality, surface durability, smoothness, light weight, and stain resistance can be imparted.

In relation to this, flooring paint using epoxy or urethane resin is a polymer type that forms room temperature curing crosslinking, and is a flooring material that has excellent texture and can realize a color desired by a user. Among them, in the case of widely used epoxy flooring materials, in addition to strong adhesion and high hardness of the coating film, there is little reaction shrinkage, and excellent physical properties such as dimensional stability, water resistance, chemical resistance and abrasion resistance. In addition, there is little cracking, elasticity and anti-slip function can be given as needed, and it dries quickly and maintenance after construction is relatively easy.

In this regard, according to the construction method of the epoxy coating material composition reinforced with inorganic substances registered in the Republic of Korea Patent No. 10-1146905, a bisphenol-F-based epoxy resin, a phenol novolac epoxy resin, and a bisphenol-A-based epoxy resin are mixed as the main composition, and cement and silica sand are mixed. It is characterized by including about 4 times more inorganic reinforcing material than the main weight.

In addition, according to the Korean Patent Publication No. 10-2022-0075886, a solvent-free water-soluble epoxy flooring material, it is intended to provide a solvent-free water-soluble epoxy flooring material that is eco-friendly and has excellent dust resistance, storability and precipitation prevention, and calcium carbonate in the curing agent as an inorganic flooring material. In the case of the calcium carbonate, the calcium carbonate is characterized by mixing a first calcium carbonate having a diameter of 0.1 to 3 μm, a second calcium carbonate having a diameter of 4 to 8 μm, and a third calcium carbonate having a diameter of 9 to 15 μm.

However, in the case of the above technology, there is a problem that the range of use is gradually limited according to the strengthening VOCs regulation. In addition, as the construction company's requirements such as safety and non-combustibility requirements increase, the development of products that convert conventional epoxy paints into water-based types is continuously being performed.

However, the problem of the water-based epoxy paint is that the water-based paint has a large surface tension and a slow evaporation rate due to the essential characteristics of water as the organic solvent is substituted with water, so that popping or cratering occurs, There is a problem that adhesion failure occurs. In addition, compared to general oil-based epoxy-based flooring materials, the structure is not dense, resulting in poor chemical resistance and water resistance. Even if the mechanical properties are satisfied, the inclusion of a flame retardant in the coating film affects the mechanical properties, so both There is a need for product development.

Republic of Korea Patent Registration 10-1146905 Construction method of epoxy coating composition reinforced with inorganic materials Korean Patent Publication 10-2022-0075886 Solvent-free water-soluble epoxy flooring

The present invention focuses on the above-mentioned technical requirements and aims to provide a method for manufacturing an epoxy composition having low VOCs levels and excellent semi-incombustible characteristics applied to floors such as parking lots and rooftops of buildings.

In addition, the present invention makes it a technical solution to provide a method of efficiently constructing flooring in a parking lot and rooftop of a building using the water-soluble epoxy flooring composition.

In order to solve the above technical problems, the present invention relates to a method for manufacturing a water-soluble epoxy composition containing nano-silica, and to prepare a water-soluble hybrid resin by mixing 1 to 10 parts by weight of a fluororesin with 100 parts by weight of a water-based polyamide resin by a dropwise method. doing; Resin stabilization step of mixing 20 to 40 parts by weight of the water-soluble hybrid resin, 10 to 20 parts by weight of water, and 0.1 to 1 part by weight of additives; A composition dispersion step of mixing and dispersing 15 to 25 parts by weight of a colored pigment and 5 to 10 parts by weight of an extender pigment in the stabilized resin; Preparing a main part by adding 1 to 10 parts by weight of a vegetable plasticizer, 1 to 10 parts by weight of a composite flame retardant, 0.5 to 7 parts by weight of a non-slip agent, 20 to 40 parts by weight of water, and 0.4 to 1 part by weight of an additive to the dispersed composition; Preparing a curing agent unit comprising 60 to 80 parts by weight of an epoxy resin, 20 to 30 parts by weight of a reactive diluent, 0.5 to 1.5 parts by weight of a surfactant, and 0.1 to 3 parts by weight of a non-slip agent in a separate container; and mixing the prepared main part and the curing agent part in a weight ratio of 3 to 5:1.

Preferably, the composite flame retardant comprises at least one of antimony oxide, magnesium hydroxide, and aluminum hydroxide and nano-silica having a particle size of 10 to 900 nm.

In order to solve the above other technical problem, the present invention relates to a floor covering construction method, a pretreatment step of removing foreign substances from the floor including cracks; An undercoating step of applying an epoxy undercoating composition to the pretreated floor surface; and a top coat coating step of applying a water-soluble epoxy paint composition containing nano-silica to the applied undercoat at least twice, wherein the water-soluble epoxy paint composition containing nano-silica includes 20 to 40 parts by weight of a water-soluble hybrid resin, water 30 to 60 parts by weight, 0.5 to 2 parts by weight of additives, 15 to 25 parts by weight of colored pigments, 5 to 10 parts by weight of extender pigments, 1 to 10 parts by weight of vegetable plasticizers, 1 to 10 parts by weight of composite flame retardants, and 0.5 to 7 parts by weight of non-slip agent A main part containing parts by weight; and a curing agent part containing 60 to 80 parts by weight of an epoxy resin, 20 to 30 parts by weight of a reactive diluent, 0.5 to 1.5 parts by weight of a surfactant, and 0.1 to 3 parts by weight of a non-slip agent; The part and the curing agent part are mixed in a weight ratio of 3 to 5: 1, and the hybrid resin of the main part is mixed with 100 parts by weight of the aqueous polyamide resin and 1 to 10 parts by weight of the fluororesin by a dropwise method.

Preferably, in the pretreatment step, when a phenomenon including at least one of peeling, layer separation, and exfoliation occurs on the bottom surface, a matrix strengthening step of applying a permeability enhancer to the surface of the bottom surface; further comprising the The penetration enhancer is characterized by including 10 to 20 parts by weight of distilled water, 40 to 50 parts by weight of a silicate binder, 15 to 20 parts by weight of an extender pigment, 1 to 5 parts by weight of a solvent, and 0.5 to 5 parts by weight of a silane coupling agent.

Preferably, in the pretreatment step, the epoxy undercoating composition includes 50 to 75 parts by weight of an epoxy resin, 10 to 20 parts by weight of a non-reactive diluent, 15 to 20 parts by weight of an extender pigment, and 1 to 5 parts by weight of a colored pigment. and a curing agent comprising 50 to 75 parts by weight of a modified amine, 25 to 50 parts by weight of an extender pigment, and 1 to 5 parts by weight of a colored pigment, wherein the main part and the curing agent part are mixed in a weight ratio of 1 to 5: 1 to be characterized

According to the present invention, by using a water-soluble hybrid resin, it has a low VOCs level, and by including a vegetable plasticizer, a composite flame retardant, and a non-slip agent in the composition, the following coating film physical properties are obtained.

First, by including a fluororesin in the polyamide resin in the main part, it has excellent mechanical properties and has excellent mechanical properties even when a flame retardant is included.

Second, as a composite flame retardant, a metal hydroxide such as aluminum hydroxide or magnesium hydroxide and nano-sized silica can be added together to produce a quasi-incombustible effect with only a small amount.

Third, it is environmentally friendly by including vegetable plasticizers instead of phthalate-based plasticizers, and in particular, even in semi-enclosed spaces such as underground parking lots, workers can work in a relatively comfortable environment as no harmful substances and organic solvents are included during construction. there is. In particular, it can be installed in parking lots and indoors, and it does not harm indoor air quality, so there is no amine smell unique to epoxy, so it has an effect that can be installed on indoor interiors and factory floors.

1 is a schematic diagram showing a method for preparing a water-soluble epoxy composition containing nano-silica.
Figure 2 is a schematic diagram showing a flooring construction method using a water-soluble epoxy composition containing nano-silica.
Figure 3 shows the test method and period as a test report of a water-soluble epoxy sample and specimen containing nano-silica according to a preferred embodiment.
Figure 4 shows the test result values with test reports of water-soluble epoxy samples and specimens containing nano-silica according to a preferred embodiment.
5 is a heat release test condition for confirming the semi-incombustible characteristics of a water-soluble epoxy coating film containing nano-silica according to a preferred embodiment.
Figure 6 is a graph of the total calorific value for confirming the quasi-incombustible characteristics of the water-soluble epoxy coating film containing nano-silica according to a preferred embodiment.
7 shows gas hazard test conditions and test results of a water-soluble epoxy coating film containing nano-silica according to a preferred embodiment.
8 is a photograph of a specimen before/after a heat release test of a water-soluble epoxy coating film containing nano-silica according to a preferred embodiment.
9 is a test report of a water-soluble epoxy sample containing nano-silica according to a preferred embodiment, showing test conditions and result values.
10 is a test report of a water-soluble epoxy sample containing nano-silica according to a preferred embodiment, showing detailed test conditions and analysis result values.
11 is a photograph of a sample and a test piece installation of a water-soluble epoxy sample containing nano-silica according to a preferred embodiment.
12 shows test results according to inspection items of a water-soluble epoxy sample containing nano-silica according to a preferred embodiment.

Since the present invention can make various changes and have various embodiments, specific embodiments will be illustrated in the drawings and described in detail. However, this is not intended to limit the present invention to specific embodiments, and should be understood to include all modifications, equivalents, or substitutes included in the spirit and technical scope of the present invention. Like reference numerals have been used for like elements throughout the description of each figure.

Terms used in this application are only used to describe specific embodiments, and are not intended to limit the present invention. Singular expressions include plural expressions unless the context clearly dictates otherwise. In this application, the terms "include" or "have" are intended to designate that there is a feature, number, step, operation, component, part, or combination thereof described in the specification, but one or more other features It should be understood that the presence or addition of numbers, steps, operations, components, parts, or combinations thereof is not precluded.

Unless defined otherwise, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention belongs. Terms such as those defined in commonly used dictionaries should be interpreted as having a meaning consistent with the meaning in the context of the related art, and unless explicitly defined in this application, it should not be interpreted in an ideal or excessively formal meaning. don't

Hereinafter, the present invention will be described in detail.

As one aspect, the present invention relates to a method for preparing a water-soluble epoxy composition containing nano-silica. Hereinafter, the present invention will be described in detail with reference to the drawings.

1 is a schematic diagram of a method for preparing a water-soluble epoxy composition containing nano-silica according to an embodiment of the present invention, preparing a water-soluble hybrid resin; (S100) stabilizing the resin by mixing the resin with additives Step; (S200), a dispersion step of dispersing a pigment in the stabilized resin; (S300), a subject part preparation step further comprising a vegetable plasticizer, a composite flame retardant and a non-slip agent, etc. in the dispersed composition; (S400), separate A step of preparing a curing agent unit in a container; (S500) and mixing the prepared main unit and a curing agent unit; (S600).

Hereinafter, the manufacturing step will be described in detail for each step.

First, preparing a water-soluble hybrid resin; (S100).

In this step, a water-soluble hybrid resin is prepared by adding a small amount of fluororesin to the aqueous polyamide resin.

Specifically, the water-based polyamide resin is a resin having excellent strength, chemical resistance, and processability when formed into a coating film, and in the present invention, it is applied to a water-soluble paint by using a modified polyamide resin.

Next, the fluororesin is a resin having excellent heat resistance, chemical resistance, and weather resistance and excellent mechanical strength, and serves to improve chemical resistance and mechanical strength as it is included in a certain amount of polyamide resin.

Particularly, in the present invention, as a part of the fluororesin is included, there is an effect of improving the hardness and wear resistance of the coating film.

In this regard, the fluororesin is preferably included in 1 to 10 parts by weight of the fluororesin in 100 parts by weight of the polyamide resin, but if it is included in less than 1 part by weight, the effect is insignificant, and if it is included in more than 10 parts by weight, the polyamide resin This is because the color of the resin is opaque and may affect the mechanical properties as it is unstablely included in the resin.

In relation to the fluororesin, it is preferable to use a copolymer of tetrafluoroethylene and ethylene or a copolymer of tetrafluoroethylene, ethylene and hexafluoropropylene, which has excellent fluidity compared to fluororesin and improves workability In the case of tetrafluoroethylene and ethylene copolymerized fluororesin, it has flame retardant properties and can impart mechanical strength.

On the other hand, it is preferable to use a dropping method in which the fluororesin is included little by little in the polyamide resin. This is because when an excessive amount of fluororesin is added at once, the opaque color and unreacted fluororesin affect mechanical properties as the fluororesin is included in an unstable state in the polyamide resin. Therefore, preferably, the fluororesin is preferably dropped at the same rate for 4 to 6 hours, and more preferably mixed at a constant rate to maintain the reaction for 1 to 2 hours after the drop is completed. it is more preferable

Next, a resin stabilization step of mixing the prepared water-soluble hybrid resin with additives and the like; (S200).

More specifically, it is preferable to mix 20 to 40 parts by weight of the water-soluble hybrid resin prepared above, 10 to 20 parts by weight of water, and 0.1 to 1 part by weight of additives.

In relation to this, the additive is an additive included to compensate for problems such as the process of transforming the water-soluble hybrid resin into a coating film or the long-term storage of the paint, and preferably includes a stabilizer, an anti-settling agent, a thickener, and the like. It is preferably included in an amount of 0.1 to 1 part by weight, but it is more preferable to include a dispersant, which is an additive whose properties are not changed or destroyed even when affected by temperature in the dispersing process described later, to help the dispersing process.

In this regard, the additive preferably includes a surfactant because the surfactant exhibits both emulsifying and dispersing effects, thereby improving the dispersibility described below and bringing about stability of the hybrid resin.

In addition, the surfactant is a compound having a hydrophilic part that is easy to dissolve in water and a hydrophobic part that is easy to dissolve in oil at the same time. In the present invention, a main part containing polyamide resin and water and a curing agent part containing epoxy resin and reactive diluent are mixed. play a role in making

In relation to this, the surfactant preferably includes a nonionic surfactant with low stimulation, more preferably, a surfactant having a molecular weight of 300 to 600 g/eq is used, and more preferably, the total weight of additives is used. It is preferable not to exceed 1 part by weight per part.

On the other hand, it is preferable to stir the water and additives at a low speed of 500 rpm, which is for reducing risks such as yield reduction caused by temperature rise due to high-speed stirring by stirring at a low speed, and at the same time making the water-soluble hybrid resin stable with the additives. It is to stir with In relation to the stirring condition, it is most preferable to stir for 10 to 30 minutes at a speed of 200 to 300 rpm.

Next, a dispersing step of dispersing a pigment in the stabilized resin; (S300).

Specifically, it is a step of mixing 15 to 25 parts by weight of a colored pigment and 5 to 15 parts by weight of an extender pigment with the stabilized resin and dispersing them.

In relation to this, colored pigments and extender pigments are means for imparting color to paints and forming coatings.

First, as a preferred example of the colored pigment, it is preferable to use organic and inorganic pigments such as titanium dioxide and carbon black, and it is preferable to include them in a range of 15 to 25 parts by weight in a range that does not impair the physical properties of the coating film.

Next, in the case of the extender pigment, an extender pigment widely used as an oil-based paint such as calcium carbonate, talc, boron arsenate, etc. is used, and it is preferably included in an amount of 5 to 10 parts by weight. Regarding the selection of the extender pigment, it is preferable to mix and use talc and calcium carbonate or calcium carbonate and boron arsenate in consideration of the oil absorption amount of the pigment and the denseness of the coating film.

In this regard, it is preferable to avoid using calcium carbonate alone in the case of the extender pigment, because it has a higher oil absorption than talc or boron arsenate, which may impair the workability of the coating film.

On the other hand, it is necessary to ensure that the colored pigment and the extender pigment are evenly mixed with the resin before dispersing. This is to improve the dispersibility of the pigment, and in the case of colored pigments, they have vivid colors without color separation, and in the case of extender pigments, the dispersibility is improved to improve the density of the coating film, thereby improving the waterproofness.

In this regard, the mixing is stirred at high speed at a speed of 800 to 1,200 rpm, but mixing is preferably performed for 10 to 20 minutes. This can improve the density of the coating film by considering the sufficient wettability of the pigment.

On the other hand, the mixture preferably disperses the pigment through high-speed stirring at a speed of 1,200 ~ 2,000rpm, it is more preferable to disperse the pigment by high-speed dispersion for 60 ~ 120 minutes. At this time, it is preferable that the particle size of the dispersed composition has a particle size of 100 μm or less, which is due to the fact that when the particle size exceeds 100 μm, the color of the colored pigment is not clear, and the extender pigment is not evenly dispersed in the resin. This is because it can affect mechanical properties.

In this regard, in the dispersion process, temperature management is very important, and it is most preferable to disperse by managing the temperature at a temperature of less than 100 ° C. This is because the problem of reducing the yield of the paint due to the high temperature may occur.

Next, a subject part preparation step further comprising a vegetable plasticizer, a composite flame retardant, and a non-slip agent in the dispersed composition; (S400).

More specifically, 1 to 10 parts by weight of a vegetable plasticizer, 1 to 10 parts by weight of a composite flame retardant, 0.5 to 7 parts by weight of a non-slip agent, 20 to 40 parts by weight of water, and 0.4 to 1 part by weight of additives are added to the dispersed composition to prepare the main part It is a step to

In relation to this, the vegetable plasticizer used in the present invention does not contain ortho-phthalate, a suspected endocrine disruptor, as a raw material, or the final product is non-regulated substances such as DEHP, DINP, DIDP, DBP, BBPP, DnOP, and DiBP. By meaning that it is not limited to, but not limited to, even if used alone or in a mixture.

In relation to this, it is preferable that the vegetable plasticizer is included in an amount of 1 to 10 parts by weight, but if it is included in less than 1 part by weight, there is a problem in that the strength of the coating film is too high due to the small content of the plasticizer, and if it is included in more than 10 parts by weight Since there is a problem that the strength is rather reduced, it is desirable to maintain an appropriate range.

On the other hand, the composite flame retardant used in the present invention is a flame retardant containing antimony oxide, magnesium hydroxide, aluminum hydroxide, and inorganic flame retardants that are mixtures thereof and nano-silica, and is less harmful to workers due to low detection of harmful substances.

In this regard, in the case of a general phosphorus-based flame retardant, instead of imparting flame retardancy to a flooring coating film, mechanical properties of the coating film are deteriorated. Therefore, in the case of the present invention, the above-mentioned inorganic flame retardants such as antimony oxide, magnesium hydroxide, and aluminum hydroxide and silica having a size of 10 to 900 nm are included, and the excellent flame retardant effect and mechanical properties of the coating film can not be damaged in a small amount, and the raw material Due to its characteristics, it has a relatively small advantage compared to phosphorus-based flame retardants.

In relation to this, the silica having a nanoparticle size has its own flame retardant properties and properties of an extender pigment by functioning to lower the weight loss rate even under high temperature conditions when forming a coating film as it is included in the paint. Specifically, in the case of the formed coating film, the nanoparticle-sized silica fills the gaps to improve the bonding force between the particles, thereby improving the physical properties of the coating film and having its own flame retardant property, thereby reducing the weight loss rate of the coating film due to high temperature.

In relation to the size of the silica contained in the composite flame retardant, adjusting the particle size to less than 10 nm has problems with the increase in raw material prices and difficulty in managing raw materials, and in the case of a size exceeding 900 nm, there is a problem in reducing the flame retardant effect of silica Bar It is preferable to use nano-silica in the corresponding range.

It is preferable that the inorganic flame retardant and nano-silica contain more inorganic flame retardant than the ratio of nano-silica, more preferably inorganic flame retardant: nano-silica is included in a weight ratio of 55 to 90: 45 to 10, which is inorganic flame retardant This is because when the ratio of is low, the effect is insignificant as the flame retardant properties of the paint are lowered.

On the other hand, the composite flame retardant is preferably included in an amount of 1 to 10 parts by weight. If it is included in an amount of less than 1 part by weight, there is a problem in that the flame retardant property is lowered. can affect physical properties.

Next, the non-slip agent is an additional raw material for improving the non-slip property on the surface of the coating film, and is a raw material for imparting the non-slip property to the flooring material.

In general, polymer type nonslip agents and silica nonslip agents may be used as nonslip agents, but in the present invention, it is preferable to use silica nonslip agents rather than polymer type nonslip agents in order to improve nonslip properties and impart inflammability.

In addition, more preferably, it is preferable to use a non-slip agent having a particle size of 1 mm to 0.1 μm, which has a problem of reduced durability when forming a coating film when the particle size of the non-slip agent is 1 mm larger, and less than 0.1 μm In the case of non-slip properties are extremely low, it is most preferable to use a non-slip agent of the above size. In addition, the non-slip agent is preferably included in an amount of 0.5 to 7 parts by weight as it is also partly included in the curing agent part. Because.

Next, the additive is an additive included in the same meaning as the additive included in the resin stabilization step, and it is preferable to include an additive sensitive to high temperature at this time. Types of additives included in this case preferably include a leveling agent, an antifoaming agent, an antisettling agent, and a viscosity modifier.

On the other hand, water included in the subject part plays the same role as the organic solvent of the organic solvent paint as it is included for efficient dispersion during the improvement of fluidity and dispersion of the main subject part. Therefore, both the resin stabilization step (S200) and the subject part manufacturing step (S400) may be included in a small amount if necessary.

However, in the case of the ratio in which water is included in each manufacturing step, in the resin stabilization step (S200), it is included in a small proportion (10 to 20 parts by weight) compared to the hybrid resin to play a role in stabilizing the resin and additives and smooth the dispersion described later. do. On the other hand, in the case of the subject part manufacturing step (S400), 20 to 40 parts by weight are included as a paint for improving workability, and it is included in each step to improve dispersibility as needed, and it is preferable to adjust the ratio of water at each step. do.

Next, the curing agent part preparation step; (S500).

Specifically, the curing agent unit preferably includes 60 to 80 parts by weight of an epoxy resin, 20 to 30 parts by weight of a reactive diluent, 0.5 to 1.5 parts by weight of an additive, and 0.1 to 3 parts by weight of a non-slip agent in a separate container.

The epoxy resin is a main resin that is cured to form a coating film, and is one of the main materials that determine the hardness, adhesion, strength, and waterproofness of a flooring material. In this regard, the epoxy resin is preferably included in an amount of 60 to 80 parts by weight, which has a problem affecting adhesion when included in less than 60 parts by weight, and when included in more than 85 parts by weight, in the process of mixing the subject and the curing agent part. As the amount of resin compared to the pigment of one main part increases, not only does it affect drying, but also a problem in that strength and hardness are reduced rather than when an appropriate amount of resin is included may occur. In addition, it is preferable to use an epoxy resin having an equivalent weight of 230 to 270 g/eq because it may affect waterproofness and workability of the flooring material.

The reactive diluent serves to reinforce the physical properties of the epoxy resin, such as weather resistance, chemical resistance, and impact resistance. Preferably, diglycidyl ether is preferably used as the reactive diluent, but is not limited thereto.

In this regard, the reactive diluent is preferably included in an amount of 20 to 30 parts by weight. If the amount of the reactive diluent is less than 20 parts by weight, the effect of enhancing physical properties is insufficient, and if it is included in more than 30 parts by weight, drying may be affected. It is preferable to include an appropriate amount because it can be.

On the other hand, the additive and the non-slip agent are the same as those included in the subject part, and a detailed description thereof will be omitted.

Finally, mixing the prepared main part and the curing agent part; (S600).

Specifically, the subject part and the curing agent part are preferably included in a weight ratio of 3 to 5: 1. When the subject part is included in a weight ratio of less than 3, there is a problem of affecting the physical properties of the coating film, and when the subject part is included in a weight ratio of more than 5, drying is delayed. There is a problem.

As another aspect, the present invention relates to a method for constructing a flooring material using the prepared water-soluble epoxy composition. Hereinafter, the present invention will be described in detail with reference to the drawings.

2 is a schematic diagram of a flooring construction method using a water-soluble epoxy composition containing nano-silica according to an embodiment of the present invention. Referring to this, the construction method of the present invention includes a floor pretreatment step; (S10), applying a primer to the pretreated floor surface; (S20) and applying a water-soluble epoxy paint composition containing nano-silica to the applied primer. It includes a top coat application step; (S30).

Hereinafter, each step of the construction method will be described in detail.

First, the bottom surface pre-processing step; (S10).

At this time, the foreign matter removal method may be performed by various methods, and smoothing the surface of the cracked floor surface. That is, the floor surface can be processed smoothly using power tools and other manual tools, and in the case of laitance, deformation, peeling, and weathered parts, after removal, a compressor or high-pressure water washing is performed to go through a chipping process can

At this time, when a phenomenon including one or more of peeling, layer separation, and exfoliation occurs as the concrete is neutralized on the floor surface, a matrix reinforcement step of applying a permeable reinforcing agent to the surface of the floor surface; (S11) may be further included. there is.

In this regard, the permeability enhancer includes 10 to 20 parts by weight of distilled water, 40 to 50 parts by weight of a silicate binder, 15 to 20 parts by weight of an extender pigment, 1 to 5 parts by weight of a solvent, and 0.5 to 5 parts by weight of a silane coupling agent. .

The silicate binder has the effect of improving the strength and hardness of concrete by penetrating into the inside of the floor surface and evaporating moisture from the concrete floor surface while filling in fine cracks and voids. In this regard, the silicate binder may be selected from among sodium silicate, potassium silicate, and lithium silicate. At this time, the effect of the binder can be maximized when sodium silicate, potassium silicate and lithium silicate are mixed in a ratio of 1:3 to 5:3 to 5. This is because lithium silicate has the lowest whitening phenomenon among silicates and high heat resistance, so that the fire resistance of sodium silicate and potassium silicate can be improved and adhesion can be improved. In addition, potassium silicate can improve adhesion to the concrete surface and its role as a surface reinforcing agent binder by creating a surface that can withstand moisture while lowering the pores. More preferably, the silicate binder is preferably used in an amount of 40 to 50 parts by weight. At this time, when the amount of the silicate binder used is less than 40 parts by weight, the adhesion to the concrete surface and the role as a surface reinforcing agent binder are reduced. , If it exceeds 50 parts by weight, corrosion resistance and water resistance may be deteriorated, so it is preferably included in the above range.

In addition, in the present invention, the silane coupling agent is used to improve the mixing property when mixing the silicate binder and the extender pigment, and to improve the adhesion to the concrete surface. In this case, when the silane coupling agent is used in less than 0.5 parts by weight, mixing between the silicate binder and the extender pigment is not well achieved, and when it exceeds 5 parts by weight, economic efficiency may be reduced. More preferably, epoxy-containing silane, amine group-containing silane, and mercapto-containing silane can be used as the silane coupling agent. Epoxy containing silanes include 2-(3,4-epoxycyclohexyl)-ethyltrimethoxysilane, γ-glycidoxytrimethoxysilane, γ-glycidoxypropyltrimethoxy silane and γ-glycidoxypropyl triethoxysilane and the like. Examples of the amine group-containing silane include N-2-(aminoethyl)-3-amitopropylmethyldimethoxysilane, N-2-(aminoethyl)-3-aminopropyltrimethoxysilane, and N-2-(aminopropylmethyldimethoxysilane). Ethyl)-3-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, 3-triethoxysilylN-(1,3-dimethylbutylidene)propylamine , N-phenyl-3-aminopropyltrimethoxysilane, etc. can be used. The mercapto-containing silane may include 3-mercaptopropylmethyldimethoxysilane and 3-mercaptopropyltriethoxysilane.

Meanwhile, the extender pigment is the same as the extender pigment mentioned above, and a detailed description thereof will be omitted. In addition, in the case of a solvent, it is preferable to use a general organic solvent, but preferably to use a xylene or toluene series.

On the other hand, rather than being applied alone, the permeability enhancer may be applied to the pretreated floor surface by mixing water at a volume ratio of 0.4 to 1: 1 and selecting one of airless, spray, and brush coating methods. After application, It is preferable to dry for 12 to 16 hours in a climate where the temperature is higher than 20 ° C and for 16 to 24 hours in a climate below 20 ° C.

On the other hand, in the case where the exfoliation part is large or the width of the crack part exceeds 5 cm ² in the pretreatment process, it is preferable to fill the crack part using an elastic putty or the like.

Next, applying a primer to the pretreated floor surface; (S20).

At this time, the undercoating material is an epoxy coating agent that is easy to apply to the wet surface, has excellent waterproof and anticorrosive properties, and has an effect of filling microcracks.

In relation to the undercoating composition, the main part including 50 to 75 parts by weight of an epoxy resin, 10 to 20 parts by weight of a non-reactive diluent, 15 to 20 parts by weight of an extender pigment, and 1 to 5 parts by weight of a colored pigment; and 50 to 75 parts by weight of a modified amine Part by weight, a hardener part containing 25 to 50 parts by weight of an extender pigment and 1 to 5 parts by weight of a colored pigment; preferably, the main part and the hardener part are mixed in a weight ratio of 1 to 5: 1.

In relation to this, the epoxy resin is a high solids epoxy resin having an SVR of 90% or more, an epoxy equivalent of 160 to 250, and preferably has a viscosity of 10,000 to 20,000 cps at a temperature of 25 ° C.

The high-solids epoxy resin is an epoxy resin having a solid content of 95%, and has the effect of minimizing the loss rate during construction to 2% or less and forming a coating film thickness of 400 μm or more with only one application.

In addition, in the case of forming a coating film, the mechanical properties of the coating film are excellent, and the high temperature characteristics and chemical resistance are excellent, so that there is little generation of volatile substances and shrinkage of the coating film during curing, so it can be easily used on the floor of an underground parking lot.

On the other hand, the epoxy resin is preferably included in an amount of 50 to 75 parts by weight, which has a problem in that the strength of the coating film is lowered when it is included in less than 50 parts by weight, and when it is included in more than 75 parts by weight, the workability increases as the viscosity increases. There is a problem with deterioration.

Next, the modified amine of the curing agent part is a modified aliphatic amine, a modified aromatic amine, or a mixture thereof, and the modified aliphatic amine is diethylene triamine (DETA), triethylene tetramine (TETA), diethylaminopropyl Amine (Diethylamino propyl amine: DEAPA), Menthane diamine (MDA), N-aminoethyl piperazine (N-AEP), M-xylene diamine (MXDA) and isophorone diamine ( Isophorone diamine: IPDA), and the modified aromatic amine is meta phenylene diamine (MPD), diaminodiphenyl methane (DDM) and diaminodiphenyl sulfone (Diaminodipheny sulphone: DDS) may be one or more selected from the group consisting of. At this time, it is preferable to use a resin having an amine value of 300 to 400 mg KOH/g, an active hydrogen equivalent of 80 to 100, and a viscosity of 1,000 to 2,500 cps (25° C.) as the modified amine. To include 50 to 75 parts by weight. If it is included in less than the above range, proper curing effect cannot be imparted, and if it is included in more than the above range, there is a problem that the hardness of the coating film becomes excessively high due to excessive curing. let it use

On the other hand, extender pigments, colored pigments, and non-reactive diluents included in the undercoat may be the same as those described above, and detailed descriptions thereof will be omitted.

On the other hand, if water pools on the floor before the undercoating or moisture is not continuously removed, it is preferable to further include a water collection device installation step (S21) to install a water collector or degassing device to remove moisture from the floor. .

Finally, a top coat application step of applying a water-soluble epoxy paint composition containing nano-silica to the applied undercoat; (S30).

Specifically, the water-soluble epoxy paint composition containing the nano-silica applied as a top coat is a paint of the above-described manufacturing method, and a detailed description thereof will be omitted.

In relation to the construction method, it is preferable to additionally apply the top coat paint after curing for at least 12 hours after the first application, which is applied at least twice or more in order to fill all the bubble phenomenon caused by the bubbles generated in the first application. More preferably, it is preferable to apply a total of three times.

On the other hand, it is preferable that the top coat paint is applied at least 500 μm or more at one time of coating, because it exhibits the most stable physical properties of the coating film when considering mechanical properties such as abrasion resistance due to the characteristics of the flooring material.

On the other hand, the applied top coat paint can be applied by brush, roller, or airless application methods.

Hereinafter, the effects of the present invention will be described in more detail through examples.

<Preparation Examples 1 to 3> Preparation of water-soluble hybrid resin

Preparation Examples 1 to 3 relate to the preparation of a water-soluble hybrid resin, and a water-soluble hybrid resin was prepared by mixing 1 kg of a fluororesin (manufacturer: Daikin) with 10 kg of an aqueous polyamide resin (manufacturer: Kukdo Chemical).

At this time, in the case of Preparation Example 1, the fluororesin was added dropwise, and the time for all the fluororesins to be dropped was 4 hours.

In the case of Preparation Example 2, a fluororesin and an aqueous polyamide resin were added at once in the same amount as in Preparation Example 1, followed by mixing and stirring. At this time, the stirring was stirred while maintaining the temperature of 30 ~ 35 ℃ for 1 hour.

Finally, in the case of Preparation Example 3, the surfactant was added to Preparation Example 2 at 10-minute intervals by 0.1 kg units while stirring.

▶ Resin manufacturing result

According to the resin production results, in the case of Preparation Example 1, it was confirmed that the resin was not gelated while clearing.

On the other hand, in the case of Preparation Example 2, it was confirmed that the resin became cloudy, which was confirmed as a result of some unreacted fluororesin.

Finally, in the case of Preparation Example 3, it was confirmed that the surfactant was changed clearly when 0.2 kg was included, but the viscosity was lower than that of Preparation Example 1 and the color was confirmed to be cloudy compared to Preparation Example 1.

As a result, it was confirmed that the water-soluble hybrid resins prepared by Preparation Examples 2 and 3 had difficulty in applying to paints.

<Example 1 and Comparative Examples 1 to 5> Preparation of water-soluble epoxy flooring composition (main agent, curing agent)

1) Example 1: Water-soluble epoxy flooring composition containing composite flame retardant and fluororesin

Example 1 is a water-soluble epoxy flooring composition containing a composite flame retardant, and the formulation for the specific composition is shown in Table 1 below.

At this time, the composite flame retardant was used by mixing magnesium hydroxide and silica having an average particle size of 100 to 200 nm in a weight ratio of 9:1.

Next, the prepared main part and the curing agent part were mixed at a weight ratio of 4:1 and used.

More specific mixing ratios are shown in Table 1 below.

2) Comparative Examples 1 and 2: Water-soluble epoxy flooring composition containing phosphorus-based flame retardant and fluororesin

In Comparative Examples 1 and 2, flooring compositions were prepared by replacing the general phosphorus-based flame retardant instead of the composite flame retardant when preparing the flooring composition in Example 1. Formulations for more specific compositions are shown in Table 1 below.

3) Comparative Examples 3 and 4: Water-soluble epoxy flooring composition containing phosphorus-based flame retardant and not containing fluorine resin

In Comparative Examples 3 and 4, the fluororesin was not included in the resin in Comparative Examples 1 and 2, and a flooring composition was prepared by replacing the general phosphorus-based flame retardant instead of the composite flame retardant. Formulations for more specific compositions are shown in Table 1 below.

4) Comparative Examples 5 and 6: Water-soluble epoxy flooring composition containing only inorganic flame retardant or nano-silica

In Comparative Examples 5 and 6, flooring compositions were prepared by including the inorganic flame retardant or nano-silica alone in Example 1. Formulations for more specific compositions are shown in Table 1 below.

5) Comparative Example 7: Oil-Based Epoxy Flooring Composition

Comparative Example 7 is an oil-based epoxy flooring composition, and the product was tested using DNC's oil epoxy D-107 product.

Example
One comparative example
One comparative example
2 comparative example
3 comparative example
4 comparative example
5 comparative example
6 comparative example
7 Type water soluble epoxy meteor
epoxy subject part water 35 35 35 35 35 35 35 Manufacturer: DC
Product Name: D-107 water soluble polyamide resin
(Kukdo Chemical) 23 23 23 25 25 23 23 Fluorine resin
(Daikin) 2 2 2 - - 2 2 thickener One One One One One One One antifoam 0.2 0.2 0.2 0.2 0.2 0.2 0.2 Color pigment (TiO ₂ ) 19 19 19 19 19 19 19 talc 4 4 4 4 4 4 4 calcium carbonate 4 4 4 4 4 4 4 vegetable plasticizer 3 3 3 3 3 3 3 composite flame retardant flame retardant
(antimony oxide) 1.6 - - - - 2 - nano silica 0.4 - - - - - 2 phosphorus flame retardant
(Kumho Mitsui Chemicals) - 2 10 2 10 - - non-slip agent
(silica sand) 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Curing agent part epoxy resin
(Kukdo Chemical) 70 70 70 70 70 70 70 reactive diluent 29 29 29 29 29 29 29 Surfactants 0.7 0.7 0.7 0.7 0.7 0.7 0.7 non-slip agent
(silica sand) 0.3 0.3 0.3 0.3 0.3 0.3 0.3 mixing ratio
(Subject: Curing agent weight ratio) 4:1

<Test Example 1> Basic physical property test

The physical properties of the epoxy flooring compositions of Example 1 and Comparative Examples 1 to 5 were compared.

The test method according to each comparison item was conducted in accordance with KS and ASTM standards.

Test comparison items and results are shown in Table 2 below.

Test items (remarks and units) environmental conditions Example 1 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Comparative Example 6 Comparative Example 7 Non-volatile content (mixture, %) (105 ± 2)℃, 1h 58.1 58.0 58.2 58.4 58.5 58.1 57.9 63.1 Lead (subject, KU) (25±0.5)℃ 123 125 128 132 135 124 122 127 Touch dry time (h) (23 ± 1) ℃
(50 ± 4)%, RH 2 3 3 3 3 2 3 10 Curing drying time (h) 5 6 6 6 6 6 6 14 Wear resistance - mass loss
(CS-17, 1,000g, 1,000 times, mg) (23 ± 2) ℃
(50 ± 5)%, RH 110 122 125 132 133 122 122 121 pencil hardness B 2B 2B B~
2B B~
2B B~
2B 2B B Adhesion Strength (MPa) (20 ± 2) ℃
(65 ± 20)%, RH 2.4 2.2 2.0 2.3 2.1 2.4 2.2 2.1 <Test method>
1) KS M ISO 3251:2008
2) KS M 5000:2019
3) ASTM D4060-19
4) KS M ISO 15184:2012
5) KS F 4716:2016

According to the above results, it was confirmed that the non-volatile content was similar to Example 1 and Comparative Examples 1 to 7. However, as a result of checking the viscosity of the main part, in the case of Comparative Examples 3 and 4, which did not contain fluororesin, the consistency was about 10 KU.

On the other hand, according to the drying test results, abrasion resistance and pencil hardness test results, in the case of the comparative examples containing the phosphorus-based flame retardant, it was confirmed that the drying was slightly delayed, and the pencil hardness and abrasion resistance were inferior.

In addition, when the specific gravity of the phosphorus-based flame retardant is large, the bond strength value also tends to decrease. From the above results, it was confirmed that the mechanical properties are maintained to some extent when the fluororesin and the composite flame retardant are included in an appropriate amount.

On the other hand, in Comparative Examples 5 and 6 using inorganic flame retardant or nano-silica alone, it was confirmed that the drying time was slightly delayed, and when nano-silica was used alone, mechanical properties (hardness) were lower than those of Example 1. could

In this regard, the results of the test report for the test piece of Example 1 are shown in FIGS. 3 to 4.

<Test Example 2> Quasi-incombustible characteristic confirmation test

The semi-incombustible characteristics of the paint were confirmed through the heat release rate and gas hazard test of Example 1 prepared above.

As a test standard, the test was conducted in accordance with Ministry of Land, Infrastructure and Transport Notice No. 2022-84, and the test confirmed the heat release rate (concalometer method) and gas toxicity test according to Article 24, Item 1.

The test method and result values are shown in Table 3 and Figures 5 to 8 below.

Test Items unit Test result Criteria 1 time Episode 2 3rd time heat dissipation test total heat released MJ/ ^m2 0.5 0.9 2.6 8 or less The time during which the heat release rate continuously exceeds 200 kW/m ² s 0 0 0 less than 10 Presence or absence of harmful factors in the test body - doesn't exist doesn't exist doesn't exist there will be no gas hazard test Mean duration of cessation of behavior in test rats minutes:seconds 14:55 14:50 - Over 9:00 <Test method>
1) Conforms to the semi-noncombustible material performance standards of "Article 24 of Ministry of Land, Infrastructure and Transport Notice No. 2022-84"

According to the test results, the total heat release of the water-soluble epoxy flooring composition containing the composite flame retardant of Example 1 was 2.6 based on 3 times, which was confirmed to be suitable for the criterion,

Even when the heat release rate continuously exceeded 200 kW/m ² , it was confirmed that there was no abnormality at 0 seconds three times.

In addition, it was confirmed that there was no release of harmful factors on fire of the test body, and the gas hazard test was also confirmed to be suitable.

In relation to this, FIGS. 5 to 8 show specific test conditions and results for the test.

<Test Example 3> Indoor air quality confirmation test

Indoor air quality pollution characteristics were confirmed by detecting TVOC (TOTAL Volatile Organic Compounds, total organic volatile compounds), toluene and formaldehyde of Example 1 prepared above.

As a test standard, it was conducted through a test method based on Indoor Air Quality Fair Test Standards-National Institute of Environmental Sciences Notification No. 2020-23 (ES 02131.1d).

The specific method and conditions according to the test are shown in FIG. 10, the test results are shown in FIG. 9, and the samples and test pieces used in the test are shown in FIG.

Referring to FIGS. 9 and 12, which are test results, the paint of Example 1 has a TVOC of 0.038, which is lower than the test reference value of 2.5, and toluene is 0.001 and formaldehyde value is also 0.001, so the result is lower than the reference value. gave.

As a result, the paint of Example 1 has low detection of TVOC (TOTAL Volatile Organic Compounds), toluene and formaldehyde, so it can be painted efficiently in parking lots and some enclosed spaces, and the degree of harm to workers was found to be very small.

As described above, it can be seen that the present invention is a basic technical idea of a floor moisture exhaust vent and a construction method using the vent, and within the scope of the basic idea of the present invention, common knowledge in the art Of course, many other variations are possible for those who have .

Claims (5)

Preparing a water-soluble hybrid resin by mixing 1 to 10 parts by weight of a fluororesin with 100 parts by weight of an aqueous polyamide resin by a dropwise method;
Resin stabilization step of mixing 20 to 40 parts by weight of the water-soluble hybrid resin, 10 to 20 parts by weight of water, and 0.1 to 1 part by weight of additives;
A composition dispersion step of mixing and dispersing 15 to 25 parts by weight of a colored pigment and 5 to 10 parts by weight of an extender pigment in the stabilized resin;
Preparing a main part by adding 1 to 10 parts by weight of a vegetable plasticizer, 1 to 10 parts by weight of a composite flame retardant, 0.5 to 7 parts by weight of a non-slip agent, 20 to 40 parts by weight of water, and 0.4 to 1 part by weight of an additive to the dispersed composition;
Preparing a curing agent part comprising 60 to 80 parts by weight of an epoxy resin, 20 to 30 parts by weight of a reactive diluent, 0.5 to 1.5 parts by weight of an additive, and 0.1 to 3 parts by weight of a non-slip agent in a separate container; and
Mixing the prepared main part and the curing agent part in a weight ratio of 3 to 5: 1; Method for producing a water-soluble epoxy composition containing nano-silica, characterized in that it comprises
According to claim 1,
The composite flame retardant comprises at least one of antimony oxide, magnesium hydroxide and aluminum hydroxide and nano-silica having a particle size of 10 to 900 nm. Method for producing a water-soluble epoxy composition containing nano-silica
A pretreatment step of removing foreign substances on the floor including the cracked portion;
An undercoating step of applying an epoxy undercoating composition to the pretreated floor surface; and
A top coat application step of applying a water-soluble epoxy paint composition containing nano-silica to the applied undercoat at least twice; including,
The water-soluble epoxy paint composition containing the nano-silica is
20 to 40 parts by weight of water-soluble hybrid resin, 30 to 60 parts by weight of water, 0.5 to 2 parts by weight of additives, 15 to 25 parts by weight of colored pigment, 5 to 10 parts by weight of extender pigment, 1 to 10 parts by weight of vegetable plasticizer, compound flame retardant 1 A main part comprising ~ 10 parts by weight and 0.5 to 7 parts by weight of a non-slip agent; and
60 to 80 parts by weight of an epoxy resin, 20 to 30 parts by weight of a reactive diluent, 0.5 to 1.5 parts by weight of a surfactant, and 0.1 to 3 parts by weight of a non-slip agent;
The main part and the curing agent part are mixed in a weight ratio of 3 to 5: 1,
The hybrid resin of the main part is a flooring construction method characterized by mixing 1 to 10 parts by weight of fluororesin with 100 parts by weight of water-based polyamide resin by a dropwise method
According to claim 3,
In the pre-processing step,
Further comprising a matrix strengthening step of applying a permeability enhancer to the bottom surface when a phenomenon including at least one of peeling, layer separation, and exfoliation occurs on the bottom surface,
The penetration enhancer comprises 10 to 20 parts by weight of distilled water, 40 to 50 parts by weight of a silicate binder, 15 to 20 parts by weight of an extender pigment, 1 to 5 parts by weight of a solvent, and 0.5 to 5 parts by weight of a silane coupling agent. method
According to claim 3,
In the pre-processing step,
The epoxy undercoating composition is
A main part comprising 50 to 75 parts by weight of an epoxy resin, 10 to 20 parts by weight of a non-reactive diluent, 15 to 20 parts by weight of an extender pigment, and 1 to 5 parts by weight of a colored pigment; and
A curing agent part containing 50 to 75 parts by weight of modified amine, 25 to 50 parts by weight of an extender pigment, and 1 to 5 parts by weight of a colored pigment;
Flooring construction method characterized in that the main part and the hardener part are mixed in a weight ratio of 1 to 5: 1

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