KR20190023305A - Solvent-free epoxy coating composition - Google Patents

Abstract

The present invention relates to a solventless epoxy paint composition having excellent coating appearance and overall physical properties after curing. The solventless epoxy paint composition comprises: a main agent part containing 20 to 40 wt% of a solventless epoxy resin, 45 to 65 wt% of an extender pigment, 0.1 to 5 wt% of a reactive diluent, 2 to 10 wt% of a non-reactive diluent, 1 to 5 wt% of a color pigment, and 1 to 8 wt% of an additive; and a curing agent containing 20 to 40 wt% of an aliphatic amine resin, 10 to 20 wt% of an aromatic amine resin, 10 to 30 wt% of a curing accelerator, and 30 to 50 wt% of a non-reactive diluent.

Description

[0001] SOLVENT-FREE EPOXY COATING COMPOSITION [0002]

The present invention relates to a solvent-free epoxy floor coating composition having excellent low temperature curability.

The epoxy resin not only has excellent compression strength, hardness and workability, but also does not generate volatile substances or shrink in volume when cured, and has a large adhesive force on the surface of the resin. Accordingly, it can be widely used in various applications in combination with a suitable curing agent. Especially, epoxy resin has excellent adhesion to concrete and is less shrinkable than other types of paints for protecting concrete, and is suitable for use in high performance coating compositions because of its high mechanical and chemical resistance.

Currently, there are two types of epoxy flooring systems that are commercialized: thin film type (dry film thickness: about 300 ㎛) flooring type which is applied twice in middle and one time by roller coating using solvent type epoxy paint, There is a thick type (dry film thickness: 1,000 ㎛ or more) flooring type which applies a paint once and then applies the solvent type top coat one time.

In the case of the above solvent type (thin film type) epoxy paint, there is a problem that it is detrimental to environmental pollution and worker's health by using a large amount of volatile solvent in order to obtain a coating film having good roller workability and leveling. In addition, in order to form a coating film having a minimum thickness of 200 占 퐉, a solvent-type (thin film) epoxy paint has a function as a bottom material and a solvent-type paint having a low solids volume ratio should be applied at least twice. Generally, it takes about one day to dry at room temperature for repainting after one painting, so it is connected with a work period of at least 2 days and an increase in airflow.

In contrast, the conventional thick film epoxy flooring system is a type in which a solvent-based epoxy coating composition is applied on a thick film (dry film thickness: 1,000 μm or more) by using rake or troch, and then the solvent type coating is applied by a single roll coating . This thick film epoxy flooring system is environmentally friendly because it contains little volatile solvent. However, when the coating is applied at a low temperature of 5 DEG C or less, the coating thickness is close to 1.0-3.0 mm, so that the curing speed is slow and the appearance and physical properties of the coating film are significantly lowered.

The present invention uses an epoxy resin having a solid content of 96% or more as a solvent-free epoxy resin to improve workability and environmental friendliness, and has a combination of at least one amine curing agent and a curing accelerator excellent in low temperature curability, The present invention provides a solvent-free epoxy flooring coating composition which is improved in workability when coated at a low temperature of 5-10 캜 at a thickness of 1,000-3,000 탆 by controlling the blending ratio of the diluent to a specific blending ratio and excellent in appearance and overall coating film properties.

The present invention relates to a composition comprising 20-40% by weight of a solventless epoxy resin, 45-65% by weight extender pigment, 0.1-5% by weight reactive diluent, 2-10% by weight non-reactive diluent, 1-5% by weight color pigment, And a curing agent portion containing 20 to 40% by weight of an aliphatic amine resin, 10 to 20% by weight of an aromatic amine resin, 10 to 30% by weight of a curing accelerator, and 30 to 50% by weight of an unreactive diluent, The mixing ratio (weight ratio) of the main portion and the curing agent may be 70-80: 20-30 based on 100 parts by weight of the total composition in which the main portion and the curing agent are mixed.

The coating composition for a solvent-free epoxy flooring of the present invention is excellent in low-temperature curing property and can exhibit excellent physical properties of a coating film after curing, good appearance and good gloss even when it is coated with a thick film at a low temperature.

Further, the coating composition for a solvent-free epoxy flooring of the present invention can increase the solid content of the coating material to ensure excellent physical properties of the coating film and excellent appearance characteristics, reduce environmental pollution caused by solvent volatilization, improve workability, The indoor air quality control law and the atmospheric environment special law in the standard consultation can all be satisfied, so that the use and management cost of the conventional environmental facilities can be minimized.

Hereinafter, the present invention will be described in detail. However, it should be understood that the present invention is not limited by the following description, and that various elements may be variously modified or selectively mixed according to need. Accordingly, it is to be understood that the invention includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.

The coating composition for a floor coating material of the present invention comprises a base part comprising a solvent-free epoxy resin and a curing agent part containing an amine curing agent, wherein the base part and the curing agent part have a specific ratio (for example, 70-80: -30 weight ratio). Hereinafter, the composition of the low temperature curing type non-solvent epoxy floor coating composition will be described in detail.

<Topic section>

In the solventless epoxy floor coating composition according to the present invention, the main part includes a solventless epoxy resin, an extender pigment, a reactive diluent, a non-reactive diluent, a color pigment and an additive.

Dance Formulation  Epoxy resin

The non-solvent type epoxy resin contained in the main part of the present invention combines with the amine type curing agent contained in the curing agent to form a coating film, to impart gloss, and to secure basic properties of the coating film.

As the above-mentioned epoxy resin, a conventional solvent-free epoxy resin known in the art may be used without limitation. For example, an epoxy resin having a solid content ratio of 96% or more and a volatile solvent content of not more than 96% can be used. Non-limiting examples of available solventless epoxy resins include bisphenol-A diglycidyl ether (DGEBA), bisphenol-F, or a mixture thereof. This bisphenol-A diglycidyl ether is a diglycidyl ether of bisphenol A produced by reacting diphenyl, referred to as bisphenol-A, with epichlorohydrin.

According to one embodiment of the present invention, the solventless epoxy resin has an epoxy equivalent (EEW) of 180-200 g / eq, in other words 182-192 g / eq, a viscosity of 11,000-14,000 cps (25 ° C) A diglycidyl ether having a solids content of 96% or more.

In the present invention, the content of the solventless epoxy resin is not particularly limited, and may be 20 to 40% by weight based on the total weight of the subject part (100% by weight). If the content of the epoxy resin is less than 20% by weight, the outer appearance of the coating film is poor and the physical properties of the coating film such as chemical resistance deteriorate. When the content of the epoxy resin exceeds 40% by weight, the pot life is shortened, and mechanical properties such as workability and hardness Can be degraded.

Extender pigment

The extender pigment contained in the main part of the present invention functions to fill pores in the coating film, to complement hardness and chemical properties, and to control gloss. In particular, since the epoxy-free composition of the present invention is applied to a floor material, it is required to select a pigment having excellent abrasion resistance and hardness in consideration of abrasion resistance of the coating film, which greatly affects the storage stability and workability of the paint.

The extender pigment may be selected from the group consisting of silica, barite (natural barium sulfate), blanch (synthetic barium sulfate), talc, calcium carbonate, calcium carbonate and the like. The above-mentioned components may be used alone or in combination of two or more.

In the present invention, the content of the extender pigment is not particularly limited, and may be, for example, 45 to 65% by weight based on the total weight of the subject part. When the content of the extender pigment is less than 45% by weight, the mechanical properties of the coating film are deteriorated. When the content of the extender pigment is more than 65% by weight, physical properties of the coating film and poor workability are caused.

diluent

The diluent contained in the main part of the present invention plays a role of overcoming the limitation of pigment application due to the high viscosity of the epoxy resin of the solventless type and adjusting the viscosity so that the self-leveling (1,000-3,000 mu m) work can be performed.

The diluent may be classified into a reactive diluent that participates in the reaction together with a curing agent, and a non-reactive diluent that does not participate in the reaction but remains in the coating film and affects physical properties. In the present invention, the reactive diluent and the non-reactive diluent are mixed, and the use ratio thereof is adjusted to a specific range.

In the present invention, as the reactive diluent, a conventional diluent known in the art having an epoxide group can be used without limitation. For example, monoepoxide such as cresyl glycidyl ether and alkyl glycidyl ether, glycidyl ester, phenylglycidyl ether, 2-ethylhexylglycidyl ether, and para-tertiary butylphenylglycidyl Diepoxide such as versatile acid such as ether, neopentyldiglycidyl ether, 1,4-butane diglycidyl ether, cyclohexanedimethanol diglycidyl ether and resorcinol diglycidyl ether, etc. have. The above-mentioned components may be used alone or in combination of two or more.

According to one embodiment of the present invention, the reactive diluent has an epoxy equivalent weight (EEW) of 4,000-4,500 g / eq, and in another example 4,100-4,250 g / eq.

The content of the reactive diluent is not particularly limited, and may be, for example, 0.1 to 5% by weight based on the total weight of the subject part. If the content of the reactive diluent is less than 0.1% by weight, the workability is poor and the appearance characteristics of the coating film are deteriorated. When the content is more than 5% by weight, the hardening of the coating film is deteriorated.

The non-reactive diluent used in combination with the above-described reactive diluent can be used without limitation in a conventional non-reactive diluent known in the art. Examples thereof include dodecylphenol, styrene phenol, benzyl alcohol, or a mixture of two or more thereof.

In the present invention, the content of the non-reactive diluent is not particularly limited, and may be, for example, 2 to 10% by weight based on the total weight of the subject part. If the content of the non-reactive diluent is less than 2% by weight, the workability is poor and the appearance properties of the coating film are deteriorated. If the content is more than 10% by weight, the mechanical properties of the coating film are deteriorated.

Color pigment

The color pigments contained in the main part of the present invention are included for the purpose of expressing a desired color (colored) in a paint by mixing with an epoxy resin.

The pigment may be an organic pigment, an inorganic pigment, a metallic pigment, an Al-paste, a pearl, and the like, which are conventionally used in the art and may be used alone or in combination of two or more thereof . For example, one or a mixture of two or more selected from the group consisting of titanium dioxide, bismuth vanadate, cyanine green, carbon black, iron oxide red, iron oxide yellow, navy blue and cyanine blue can be used.

In the present invention, the content of the color pigment may be 1 to 5% by weight based on the total weight of the subject part. When the content of the color pigment is out of the above range, the color expression of the coating film to which the floor coating composition of the present invention is applied may be insignificant.

additive

The topical part constituting the solventless epoxy floor coating composition of the present invention may contain conventional additives known in the art, so long as the inherent characteristics of the composition are not impaired.

Non-limiting examples of usable additives include dispersants, defoaming agents, defoaming agents, leveling agents, weathering additives, drying agents, appearance control agents, anti-settling agents, coupling agents or a mixture of two or more thereof. For example, two or more additives selected from the group consisting of an anti-settling agent, a dispersant, a defoaming agent, a defoaming agent and a leveling agent may be mixed. In the present invention, the content of the additive may be appropriately controlled within the range of contents known in the art, for example, 1 to 8% by weight based on the total weight of the subject portion.

The anti-settling agent plays a role of preventing the settling of the materials and forming the coating film into a uniform property, and any of those known in the art can be used without limitation. For example, a clay type anti-settling agent. The content of the anti-settling agent is not particularly limited, and may be, for example, 0.1 to 0.7% by weight. When the content of the sedimentation inhibitor is less than 0.1% by weight, the leveling of the coating film is excellent, but the storage stability of the coating material becomes poor. When the content of the sedimentation inhibitor is more than 0.7% by weight, the storage stability of the coating material is excellent.

In the case of epoxy flooring, defoamer and defoamer can be mixed so that the air bubbles on the surface of the film can be quickly floated to the surface. If the internal bubbles do not float and remain in the coating, poor adhesion to the substrate and / or deterioration of the physical properties may be caused. Even if the internal bubbles rise, the flowability of the coating film deteriorates , Bubble marks may remain on the surface of the coating. In addition, when various color pigments are used, the pigments may have different fluidity depending on the color, resulting in color separation before and after curing. When the subject part contains at least one additive such as the above-mentioned dispersant, antifoaming agent, defoaming agent and leveling agent, it is possible to improve occurrence of coating film defects such as defective defoaming, cretering occurrence and color separation.

The dispersing agent serves to disperse each material constituting the composition and to prevent the re-agglomeration through maintaining the distance, thereby exhibiting uniform physical properties of the coating film. As the dispersing agent, those conventionally known in the art can be used, and for example, a dispersant of a high molecular weight block copolymer type and the like are available.

The antifoaming agent is a mixture of a hydrophilic and a polysiloxane. The antifoaming agent acts to increase the appearance of a coating film by suppressing bubbles generated during coating, and conventional antifoaming agents known in the art can be used without limitation. As an example, a defoamer of polysiloxane type may be used.

The defoaming agent prevents and removes bubbles during coating and improves the manufacturing process. For example, non-silicone type polymer defoaming agents can be used.

The leveling agent is intended to improve the appearance characteristics of the coating film while improving the adhesion in the composition by leveling the composition so as to be flat and smoothly coated. The leveling agent may be any of those known in the art without limitation. Examples of the leveling agent include an acrylic type, a silicone type, a polyester type, and an amine type leveling agent.

<Curing agent part>

In the solventless epoxy floor coating composition according to the present invention, the curing agent part includes an amine curing agent, a curing accelerator and a non-reactive diluent.

Amine system  Hardener

The amine-based curing agent included in the curing agent of the present invention combines with the epoxy resin of the non-use type contained in the main part to form a coating film and secure the basic physical properties of the coating film.

As the amine-based curing agent, conventional resins for amine curing agents known in the art may be used without limitation. For example, an aliphatic amine base, an aromatic amine base, or a mixture thereof.

According to one embodiment of the present invention, the aliphatic amine resin has an amine value of 400-500 mgKOH / g, a viscosity of 100-1,000 cps (25 ° C), an aromatic amine resin of 350-400 mgKOH / g, May be 500-2,000 cps (25 &lt; 0 &gt; C). Here, the ratio of the aliphatic amine resin to the aromatic amine resin is, for example, 1 to 3: 1 by weight, and may be 1-2.5: 1 by weight.

The content of the amine-based curing agent is not particularly limited, and may be, for example, 30 to 60% by weight based on the total weight of the curing agent portion. For example, the content of the aliphatic amine resin may be 20 to 40 wt% based on the total weight of the curing agent part, and the content of the aromatic amine resin may be 10 to 20 wt%, based on the total weight of the curing agent part, Lt; / RTI &gt; When the content of the amine curing agent is less than the above range, there is a problem that the appearance of the coated film after curing is poor and the hardness is lowered. When the content exceeds the above range, the workability is deteriorated and the drying time is delayed Lt; / RTI &gt;

Hardening accelerator

The curing accelerator included in the curing agent of the present invention is a substance that promotes the reaction between the epoxy resin and the amine curing agent, and any conventional materials known in the art can be used without limitation.

Non-limiting examples of usable curing accelerators may be at least one selected from the group consisting of tridimethylaminomethylphenol, triphenylphosphite and aminoethylpiperazine.

The content of the curing accelerator is not particularly limited, and may be, for example, 10 to 30% by weight based on the total weight of the curing agent portion. If the content of the curing accelerator is out of the range, physical properties such as chemical resistance and water resistance of the coating film may be deteriorated and the appearance of the coating film may be poor.

According to one embodiment of the present invention, the amine curing agent and the curing accelerator may be 50-95: 5-50 by weight based on 100 parts by weight of the total amount of the amine curing agent and the curing accelerator. Outside the ranges described above, the chemical resistance, water resistance and the like are deteriorated and the appearance of the coating film is poor.

Non-reactive  diluent

In addition to the curing agents and curing accelerators described above, the curing agent portion of the present invention includes conventional non-reactive diluents known in the art.

The non-reactive diluent may be the same as or different from the non-reactive diluent component of the above-mentioned subject, and examples thereof include dodecylphenol, styrene phenol, benzyl alcohol, or a mixture of two or more thereof.

In the present invention, the content of the non-reactive diluent is not particularly limited. For example, the content of the non-reactive diluent may be 100% by weight of the curing agent portion, and may be 30 to 50% have. If the content of the non-reactive diluent is less than 30 wt%, the workability is poor and the appearance characteristics of the coating film deteriorate. If the content of the non-reactive diluent is more than 50 wt%, the mechanical properties of the coating film deteriorate.

The mixing ratio (weight ratio) of the aromatic amine resin to the non-reactive diluent in the curing agent may be 1: 1.5-5. If the mixing ratio of the aromatic amine resin and the non-reactive diluent is less than 1: 1.5, the workability is poor and the appearance characteristics of the coating film are deteriorated. If the mixing ratio exceeds 1: 5, the mechanical properties of the coating film are deteriorated.

According to one embodiment of the present invention, the coating composition for a solventless epoxy flooring material comprises 20 to 40% by weight of an epoxy resin without a solvent, 45 to 65% by weight of an extender pigment, 0.1 to 5% by weight of a reactive diluent, From 20 to 40% by weight of an aliphatic amine resin, from 10 to 20% by weight of an aromatic amine resin, from 10 to 30% by weight of a curing accelerator, and from 10 to 30% Wherein the mixing ratio (weight ratio) of the main portion to the curing agent is 70 to 80: 1, and the mixing ratio of the main portion and the curing agent is 100: 20-30. If the mixing ratio of the main portion and the curing agent portion is out of the above range, the solvent resistance and hardness may be lowered and the appearance of the coating film may become poor.

In the present invention, a non-reactive diluent is contained in the main portion together with a reactive diluent, and at the same time, a non-reactive diluent is contained as a component of the hardener portion. As a result, the content of the non-reactive diluent increases compared to the conventional epoxy floor coating, and the workability is improved due to the plasticity of the non-reactive diluent. Particularly, when a phenol-based plasticizer is used, physical properties excellent in low-temperature curing performance can be exhibited.

According to an embodiment of the present invention, the content of the non-reactive diluent may be 5-25% by weight based on the total weight of the total composition in which the main portion and the curing agent are mixed.

In addition, the coating composition for a solventless epoxy flooring material may have a viscosity of 900-1,200 cps (25 캜) and a solid content of 93-98% by weight.

The epoxy-free floor coating composition of the present invention can be produced by a conventional method known in the art. For example, the epoxy-based floor coating composition of the present invention can be prepared by constituting a subject portion and a hardening agent portion of the above- .

In one embodiment of the above manufacturing method, a reaction solution is prepared by adding a solventless epoxy resin, a reactive diluent, a non-reactive diluent and additives (for example, a dispersant, a defoaming agent, a sedimentation inhibitor, a defoaming agent, a leveling agent, A second step of adding a squeeze pigment and a color pigment to the reaction solution and preparing a main part by stirring; a third step of adding a curing accelerator, a curing accelerator, and a non-reactive diluent to prepare a curing agent; (Weight ratio) of the main portion and the curing agent is 70 to 80: 20-30 based on 100 parts by weight of the total composition in which the main portion and the curing agent are mixed, thereby preparing a solventless epoxy floor coating composition It can be composed of four steps.

For example, in the second step, the extender pigment is slowly added to the reaction solution and stirred. Thereafter, the reaction solution is dispersed in a high speed disperser until a specific particle size (for example, 40-50 μm) After dispersing, the coloring agent to which the color pigment is added may be gradually added and stirred to prepare the subject portion.

As described above, the epoxy-based floor coating composition of the present invention is safe to use because it hardly uses solvents harmful to human and environment, and it can finish a thick film having a dry film thickness of 1,000 to 3,000 탆 with a single coating, Even after curing at a temperature of -10 DEG C, the appearance and physical properties of the coating film are good. Accordingly, the epoxy-based floor coating composition of the present invention can be applied to various flooring materials, but is not limited thereto, and can be applied to various processing steps and applications.

Hereinafter, the present invention will be described more specifically by way of examples. However, the following examples are provided to aid understanding of the present invention, and the scope of the present invention is not limited to the examples in any sense.

[ Example  And Comparative Example ]

Epoxy resin, reactive diluent, non-reactive diluent, color pigment, additive and extender pigment were added in the amounts shown in Table 1, followed by Bead Mill dispersion to uniformly prepare the subject portions of Examples 1-2 and Comparative Examples 1-7 . An aliphatic amine resin, an aromatic amine resin, a curing accelerator, and a non-reactive diluent in the contents shown in Table 1 were added and mixed at low speed stirring to uniformly prepare the curing agent portion of Example 1-2 and Comparative Example 1-7. Detailed specifications of the components used in Examples and Comparative Examples are shown in Table 2 below.

 [ Experimental Example ] Evaluation of Physical Properties of Coating Film

The physical properties of the coating compositions of Examples 1-2 and 1-7 were measured as described below, and the results are shown in Tables 3 and 4.

&Lt; Method for measuring physical properties &

1. Hardness

SHORE-D hardness: The coating film painted at 2,000 탆 was measured using a SHORE-D hardness meter.

2. Low temperature amine blushing

The coating composition was coated on a concrete plate, and after 7 days, the occurrence of amine blushing on the coating film was measured using a polisher.

3. Appearance

The coating composition was coated on a glass plate, and visually observed for defoaming, crimping, and leveling defects.

4. Polish

The coating composition was coated on a glass plate and cured at low temperature (5 ° C) for 10 days, and then the gloss (60 °) of the coating film was observed.

5. Workability

The paint composition was painted using a rake in the night light, and the ease of operation, leveling, defoaming and the like were observed.

6. Gel-Time

After 80% by volume of each coating composition was filled in the tin cans, the stick test was conducted under constant temperature and humidity conditions, and the time when the sticks were not moving was measured.

7. Smoothness

Sag Meter was used to measure the smoothness of the coating after horizontal coating.

?: Very excellent,?: Excellent,?: Fair, X: poor

As shown in Tables 3 and 4, the non-solvent type epoxy coating composition according to the present invention is characterized in that the blending ratio of a specific subject portion and a curing agent portion, a mixing ratio of an aliphatic amine and an aromatic amine, a mixing ratio of a reactive diluent and a non- As a result, it was confirmed that excellent effects were obtained in all of the physical property evaluation items and that the quality of the solvent-free epoxy coating material at low temperatures can be optimized. On the other hand, when the mixing ratio of the main portion and the hardener portion is out of the range of the present invention (Comparative Example 1-2), the mixing ratio of the aliphatic amine and the aromatic amine is out of the range of the present invention, or the mixing ratio of the reactive diluent and non- (Comparative Example 3-7), one or more of the evaluation items showed a poor effect.

Claims (10)

20 to 40% by weight of an epoxy resin without a solvent, 45 to 65% by weight of an extender pigment, 0.1 to 5% by weight of a reactive diluent, 2 to 10% by weight of an unreactive diluent, 1 to 5% And
A curing agent portion containing 20-40 wt% of an aliphatic amine resin, 10-20 wt% of an aromatic amine resin, 10-30 wt% of a curing accelerator, and 30-50 wt% of a non-reactive diluent,
Wherein the mixing ratio (weight ratio) of the main portion and the curing agent portion is 70-80: 20-30 based on 100 parts by weight of the total composition in which the main portion and the curing agent are mixed. The epoxy coating composition according to claim 1, wherein the mixing ratio (weight ratio) of the aromatic amine resin to the non-reactive diluent in the curing agent part is 1: 1.5-5. 2. The epoxy coating composition of claim 1, wherein the content of the non-reactive diluent is 5-25% by weight based on the total weight of the total composition of the mixture of the main part and the curing agent. The epoxy coating composition of claim 1, wherein the epoxy-free epoxy resin has an epoxy equivalent weight (EEW) of 180-200 g / eq, a viscosity of 11,000-14,000 cps at 25 ° C, and a solids content of 96% or more. The epoxy coating composition of claim 1, wherein the non-reactive diluent is at least one selected from the group consisting of dodecyl phenol, styrene phenol, and benzyl alcohol. The method of claim 1, wherein the aliphatic amine resin has an amine value of 400-500 mgKOH / g, a viscosity of 100-1,000 cps (25 ° C), an amine value of 350-400 mgKOH / g, 2,000 cps (25 占 폚). 2. The epoxy coating composition of claim 1, wherein the ratio of the aliphatic amine resin to the aromatic amine resin is 1-3: 1 by weight. The epoxy coating composition according to claim 1, wherein the curing accelerator is at least one selected from the group consisting of tridimethylaminomethylphenol, triphenylphosphide, and aminoethylpiperazine. The epoxy coating composition according to claim 1, wherein the additive is at least one selected from the group consisting of a dispersing agent, a defoaming agent, a defoaming agent, a leveling agent, a weathering additive, a drying agent, an external conditioner, an anti-settling agent and a coupling agent. 2. The epoxy coating composition of claim 1, wherein the composition is capable of floor construction with a film thickness of 1.0-3.0 mm at a low temperature of 5-10 &lt; 0 &gt; C.