KR102134598B1 - Epoxy urethane hybrid floor coating composition and manufacturing method thereof - Google Patents

Abstract

The present invention relates to an intermediate epoxy-urethane hybrid flooring composition for improving durability and a manufacturing method thereof, wherein the flooring composition comprises a main agent part and a curing agent part, the main agent part comprises: an epoxy resin; an isocyanate compound; polyol; phenylsilane; diphenylsilane; a silane coupling agent; and a solvent, and the curing agent part comprises: a curing agent; aminosilane; and a solvent.

Description

Epoxy urethane hybrid flooring composition for midway and its manufacturing method. {EPOXY URETHANE HYBRID FLOOR COATING COMPOSITION AND MANUFACTURING METHOD THEREOF}

The present invention relates to an epoxy urethane hybrid flooring composition for intermediates and a method for manufacturing the same, and more specifically, an epoxy urethane hybrid flooring composition for intermediates that can improve the heat resistance and weather resistance of the intermediate coating layer by containing an epoxy urethane hybrid resin and its preparation It's about how.

In general, the flooring material is constructed by a method of forming a coating film in order of primer, middle, and top. As such a flooring material, an organic flooring material mainly composed of a resin such as an epoxy resin, a urethane resin, a polyurea resin, and a FRP resin is widely used.

For example, in the case of a flooring composition containing urethane resin, it is used as a waterproofing material for topcoat before installation of the top coat, and it has excellent elongation rate of structure cracking resistance due to its high elongation, so it is vulnerable to continuous contraction and expansion due to its tensile strength drop, and has a minimum thickness of 2 mm or more. There is a problem that must be secured.

In addition, in the case of a flooring material containing an epoxy resin, it is applied when anticorrosive coating is performed without installing a top coat, but there is a problem in that the painting must be renewed every year because a problem arises in that the coating surface is lifted or peeled in winter.

In order to solve this problem, Korean Patent Publication No. 10-1625410 includes a modified hybrid resin obtained by modifying a polytetramethylene ether glycol-modified epoxy resin with an alkoxysilane to improve the chemical resistance and scratch resistance of the flooring. By using such a hybrid resin, it is possible to improve the properties of the flooring material, which is mainly suitable for improving the properties of the top coat layer, and when applied to the middle coat layer, there is a problem that the bonding strength between the primer and the top coat cannot be improved.

Applicants in the Republic of Korea Patent Publication No. 10-1967268 to improve the thermal stability of the flooring by containing a curing agent containing a curing agent, aminosilane, solvent and the main part including an epoxy resin, phenylsilane, alkoxy silane, silane coupling agent and solvent Thus, a composition suitable for application to a top coat layer has been disclosed.

The composition for the top coat is excellent in its coating properties, but when applied on a commercially available intermediate material, it has poor compatibility and shows a problem of peeling off of the coating film and deterioration in durability.

Republic of Korea Patent Registration No. 10-1625410 Republic of Korea Registered Patent Publication No. 10-1967268

The present invention has been devised in view of the prior art as described above, and an object thereof is to provide a flooring composition showing physical properties suitable for forming a midway in a flooring construction process.

In particular, it is an object of the present invention to provide a flooring composition capable of improving durability by improving heat resistance and weather resistance when forming a middle degree and having excellent compatibility with a top coat.

In addition, an object of the present invention is to provide a method for efficiently manufacturing the flooring composition.

The flooring composition of the present invention for achieving the above object is composed of a main part and a curing agent part, the main part comprises an epoxy resin, an isocyanate compound, polyol, phenylsilane, diphenylsilane, a silane coupling agent and a solvent, the The curing agent portion is characterized by comprising a curing agent, an aminosilane, and a solvent.

At this time, the phenylsilane and diphenylsilane are preferably contained in a weight ratio of 5:1 to 20:1.

In addition, in the manufacturing method of the flooring composition of the present invention, the main part is a mixture by mixing a first liquid containing an epoxy resin, an isocyanate compound, a polyol, a solvent, and a silane coupling agent and a second liquid containing phenylsilane and diphenylsilane Preparing a; The mixture may be prepared by mixing distilled water and a catalyst to react to prepare a main part.

The flooring composition of the present invention exhibits properties suitable for forming a middle in the flooring construction process.

In particular, when forming the middle, the heat resistance and weather resistance are improved, and the compatibility with the top coat is excellent, thereby improving the durability.

In addition, according to the method for manufacturing a flooring composition of the present invention, the flooring composition can be efficiently produced.

1 is a process diagram showing a method of manufacturing a coating composition for a flooring according to the present invention.
FIG. 2 is a view showing a state (c) in which a middle coating film is formed by mixing the main part (a), the curing agent part (b), and the main part and the curing agent part constituting the coating composition for a flooring according to the present invention.

Hereinafter, the present invention will be described in more detail. The terms or words used in the present specification and claims should not be interpreted as being limited to ordinary or dictionary meanings, and the inventor can appropriately define the concept of terms in order to explain his or her invention in the best way. Based on the principle of being present, it should be interpreted as meanings and concepts consistent with the technical spirit of the present invention.

The flooring composition of the present invention according to the present invention comprises a main part and a curing agent part, and the main part includes an epoxy resin, an isocyanate compound, a polyol, phenylsilane, diphenylsilane, a silane coupling agent, and a solvent, and the curing part comprises a curing agent, It is characterized by containing an aminosilane and a solvent.

The flooring composition is to form a coating film by mixing the subject portion and the curing agent portion in the flooring construction process and then applying it, and is particularly used as a flooring composition for intermediate use. That is, in the state where the top coat is applied to the floor, the top coat is applied to improve the compatibility and adhesion between the top coat and the top coat before the top coat is applied, and the top coat is a coating composition of Korea Patent Registration No. 10-1967268, which is the applicant's development technology. It can be formed, it is possible to construct a conventional flooring material for the primer.

The main part improves the physical properties of the flooring material when the epoxy urethane hybrid resin is applied by containing phenylsilane and diphenylsilane, thereby obtaining suitable properties as a composition for forming a medium.

The physical properties required for the commonly used epoxy-based intermediate flooring materials should be within 60 minutes of dry contact and less than 6 hours of dry drying according to KS M 5000-2512, and have an adhesion performance of 1.20 N/㎟ or more according to KS F 4937. , In the evaluation of the lubricating load resistance performance, the surface condition must satisfy the properties such as no cracks, cracks, or flakes, and the underlying layer is not exposed. In addition, it is necessary to prevent the waterproofness of the coating film from being deteriorated by exhibiting excellent adhesion by being installed between the top and bottom coats along with these general physical properties.

In Korean Patent Registration No. 10-1967268, phenylsilane is used as a component of the coating material, and such phenylsilane is phenyltrimethoxysilane, phenyltriethoxysilane, dimethylphenylsilane, 1,1,1-trimethyl-2,2,2-triphenyldisilane (1,1,1-trimethyl-2,2,2-triphenyldisilane), one phenyl group is attached to any one silicon atom Compounds.

It was found that the composition containing the phenylsilane exhibits an effect of improving the physical properties of the coating material through modification of the epoxy resin.

In the present invention, diphenylsilane is mixed with the phenylsilane. Examples of the diphenylsilane include diethoxydiphenylsilane, diphenyl(3-methoxypentyloxy)pentyloxysilane, and diphenyl(3-methoxypentyloxy)propoxy. Any one of silane (diphenyl(3-methylpentyloxy)propoxysilane) may be mentioned. Unlike phenylsilane, diphenylsilane having a relatively low hydrolysis rate is included, so that it not only satisfies the properties of the middle coating film but also has compatibility with top coat. It was found that the adhesion of the coating film was improved by increasing.

The phenylsilane and diphenylsilane are preferably contained in a weight ratio of 5:1 to 20:1. When phenylsilane and diphenylsilane are simultaneously contained, the phenylsilane group is partially bonded to the epoxy urethane hybrid resin, and some reaction of urethane It is understood that it inhibits the formation of some unreacted product of the isocyanate compound and the polyol, and the unreacted product is cured after the coating film is formed, making the connection of the polymer chain more complicated and thereby improving the durability of the middle coating film.

In particular, when applying the composition disclosed in the Republic of Korea Patent Publication No. 10-1967268 as a composition constituting the top coat, it was found that the compatibility between the top and the middle is improved.

In addition, the epoxy urethane hybrid resin forming the main part can be hybridized when mixed with a curing agent part and applied by mixing an epoxy resin and an isocyanate compound capable of forming a urethane resin and a polyol. When the epoxy urethane hybrid resin was used, it was found that, unlike the epoxy resin or the urethane resin, the adhesion, durability, and waterproofness of the middle coat film could be improved, and the compatibility with the primer and top coat was also improved.

As the epoxy resin, it is preferable to use any one of bisphenol A type epoxy resin, bisphenol F type epoxy resin, bisphenol AD type epoxy resin, and urethane-modified epoxy resin.

In addition, the isocyanate compounds include diphenylmethane diisocyanate (MDI) or homopolymer thereof, toluene diisocyanate (TDI) or homopolymer thereof, hexamethylene diisocyanate (HDI) or homopolymer thereof, and isophorone diisocyanate. (IPDI) or a homopolymer thereof may be used, and the polyol may be polyethylene glycol, polypropylene glycol, polybutylene glycol, or polyisoprene glycol.

The flooring composition of the present invention is to prepare a coating film by coating the surface of the substrate after mixing the main portion and the curing agent portion prior to coating on the substrate, respectively, as shown in FIG.

The main part and the curing agent part are mixed in a weight ratio of 1:1 to 5:1, preferably 2:1 to 3:1, and appropriately selected and mixed within the above range in consideration of the type of substrate or the thickness of the coating film. Can.

Referring to FIG. 1, a method for manufacturing the main part will be described, and a first liquid phase is prepared by mixing an epoxy resin, an isocyanate compound, a polyol, a silane coupling agent, a solvent, and a catalyst, and separately, phenylsilane, diphenylsilane, and silane After mixing the coupling agent, distilled water, and a catalyst to prepare a second liquid, the main liquid is prepared by mixing the first liquid and the second liquid with distilled water containing a catalyst.

Since the order of the manufacturing process is for the purpose of modifying the epoxy urethane hybrid resin by the phenylsilane and diphenylsilane, if the order or conditions of the process change, such as mixing phenylsilane and diphenylsilane with the resin solution at the same time, the present invention It was found that the properties of the desired coating material composition could not be obtained.

Further, the curing agent portion may be prepared by mixing a curing agent, aminosilane, and solvent.

In one embodiment, the first liquid was prepared as follows. Bisphenol A type epoxy resin (YD-115CA, Kukdo Chemical) 20 to 40 parts by weight, 3 to 5 parts by weight of methyl cellosolve as a solvent, and 2 to 5 parts by weight of 3-glycidoxypropyl trimethoxysilane as a silane coupling agent And stirred to prepare stirring solution A. In addition, 20 to 40 parts by weight of hexamethylene-1,6-diisocyanate homopolymer (Demodur N3900, Bayer), 5 to 10 parts by weight of polyethylene glycol (PP-1000, KPX), and 0.1 to 0.5 parts by weight of catalyst DBTDL are sequentially The mixture was added and stirred at 80° C. for 3 hours to prepare stirring solution B. A first liquid was prepared by dropping and stirring the stirring solution B in stirring solution A.

In order to prepare the second liquid, 60 to 80 parts by weight of a mixture of phenyl trimethoxysilane and diphenyl (3-methoxypentyloxy) pentyloxysilane in 10:1 parts by weight, and 3-glycine as a silane coupling agent 10 to 20 parts by weight of doxypropyltrimethoxysilane was introduced into the reactor and stirred. In addition, a mixture of 3 to 8 parts by weight of distilled water and 0.1 to 0.5 parts by weight of sulfuric acid as a catalyst was slowly added dropwise to the reactor and mixed, followed by stirring at 30°C for 6 hours to prepare a second liquid.

65 to 85 parts by weight of the first liquid and 15 to 35 parts by weight of the second liquid were sequentially added to the reactor and stirred, and a mixture of 1 to 5 parts by weight of distilled water and 0.1 to 0.3 parts by weight of sulfuric acid as a catalyst was added dropwise thereto. And stirred at 30 ℃ for 12 hours to prepare the main part.

In addition, 40 to 60 parts by weight of aspartic amine (NH-1420, Bayer), 5 to 10 parts by weight of 3-glycidoxypropyl trimethoxysilane, imine curing agent (KH-816, Kukdo Chemical) 20 To 30 parts by weight, 5 to 10 parts by weight of aminosilane (OFS-6020, Dow Corning), 1 to 5 parts by weight of BYK-182 as a dispersing agent, 0.5 to 2 parts by weight of BYK-333 as a leveling agent, BYK-066N 2 to 2 as an antifoaming agent After adding 5 parts by weight to the reactor sequentially and stirring, 15-25 parts by weight of calcium carbonate as a filler and 3-8 parts by weight of pigment were added thereto and stirred. After stirring, it was put into a basket mill, milled for 1 hour, and crushed to have an average particle size of less than 30 μm.

The main part and the curing agent part manufactured as described above constitute a main part having a low viscosity and a high-viscosity curing agent part as shown in FIG. 2, and forming a middle coating film by combining them can form a cured film as shown in FIG. 2(c). .

Further, for comparison, a main part and a curing agent part were prepared as described above, but phenylsilane and diphenylsilane were not mixed, and phenyltrimethoxysilane was mixed in an amount of 60 to 80 parts by weight to prepare a main part to prepare a composition of a comparative example.

After mixing the coating material composition according to the present invention with the coating material composition according to the comparative example and the commercially available coating material composition so that the main part and the curing agent part are in a weight ratio of 2:1, 1, 4, under conditions of 20°C and 60% humidity. After 8 hours, the emission amount of formaldehyde, toluene, and xylene was measured through a gas detector using gas chromatography.

Hazardous chemicals time Commercial product (ppm) Comparative Example (ppm) Example (ppm) Formaldehyde 1 hours 800 520 510 4 hours 380 250 240 8 hours 180 120 130 toluene 1 hours 1,600 1,000 1,000 4 hours 1,100 490 500 8 hours 800 400 400 Xylene 1 hours 800 400 400 4 hours 600 320 300 8 hours 200 100 100

Looking at the results of Table 1, both commercial products, examples, and compositions of Comparative Examples showed a result that the emission amount of formaldehyde, toluene, and xylene decreased over time, but the commercial products were relatively compared to the coating composition of the present invention. As a result, it was found to contain large amounts of hazardous chemicals. In the case of the coating composition of the present invention, the process does not contain the harmful chemicals, but it was found that formaldehyde, toluene, and xylene are detected by the traces of harmful chemicals contained in the raw materials used. However, the content was found to be significantly reduced compared to commercial products.

In addition, a pencil hardness test was performed on the coating film to which the compositions of Examples and Comparative Examples were applied. The pencil hardness test is measured in accordance with KS M ISO 15184 and is a resistance test against the occurrence of marks or defects on the surface of the coating film when the surface is pressed with a pencil core having the specified specimen size, shape, and prescribed hardness. The marks produced by the defects appear on the surface of the coating film. To this end, a pencil hardness tester and a pencil specified in KS M ISO 15184 were used to test the paint surface with a load of 750±10 g. The test plate was selected as a commercially available aluminum plate of 200×300 mm, and hardness was measured with a commercially available epoxy product for comparison. As a result, the coating film formed of a commercially available coating composition formed a mark in the pencil core 2H, and in the case of a coating film in which the composition of Examples and Comparative Examples was applied, the coating composition of the present invention had better hardness performance than that of the conventional coating composition. It was shown. However, there was no difference in pencil hardness of the coating film to which the compositions of Examples and Comparative Examples were applied.

Next, in order to confirm the effect of using the composition of the present invention for forming a middle coat film, a commercially available waterproof urethane coating agent was applied to a concrete surface area of 1 m 2 to form a primer film, and then the composition of Examples and Comparative Examples was 4±. The coating was applied in an amount of 2 g/m 2 to form a middle coating film, and after the middle coating was cured, the composition according to Korean Patent Publication No. 10-1967268 was applied in an amount of 5±2 g/m 2 to form a top coating film.

An adhesive strength test based on KS F 4937 was performed on the prepared coating film, and the same test was performed after leaving the coating film on the roof for 6 months to evaluate whether the adhesive force was changed. In the adhesion test, after applying the adhesive to the surface of the specimen after curing, attach 1 kg of weight, leave it for 24 hours, remove the weight, and apply the tensile force in the vertical direction to the sample surface using the lower tension jig to obtain the maximum tension. The load is obtained and the adhesion strength is calculated from Eru. Table 2 shows the results. In Table 2, the unit is N/㎟, and the reference value of the adhesion performance according to KS F 4937 is 1.2 N/㎟.

0 days 1 month 3 months 6 months Example 1.32 1.30 1.31 1.29 Comparative example 1.34 1.29 1.20 1.12

Looking at the results of Table 2, when forming the intermediate coating film using the composition of the example, the adhesion strength of the sample surface does not change even after 6 months, which suggests that the adhesion of the top, middle and bottom is maintained to be. On the other hand, the composition of the comparative example was excellent in initial adhesion strength, but it was found that the adhesion strength between coatings was lowered because the adhesion strength tended to decrease over time. From these results, it can be seen that the epoxy urethane hybrid flooring material containing phenylsilane and diphenylsilane exhibits physical properties suitable for forming a middle coating film.

The present invention has been described with reference to preferred embodiments as described above, but is not limited to the above embodiments and various modifications by those skilled in the art to which the present invention pertains without departing from the spirit of the present invention. And change is possible. Such modifications and variations are to be regarded as falling within the scope of the invention and appended claims.

Claims (3)

A flooring composition consisting of a main part and a curing agent part,
The main part includes epoxy resin, isocyanate compound, polyol, phenylsilane, diphenylsilane, silane coupling agent and solvent,
The curing agent portion includes a curing agent, aminosilane, and a solvent,
The phenylsilane and diphenylsilane is a flooring composition characterized in that it is contained in a weight ratio of 5:1 to 20:1.
delete As a method for manufacturing a flooring composition according to claim 1,
The main part comprises preparing a mixture by mixing a first liquid containing an epoxy resin, an isocyanate compound, a polyol, a solvent, and a silane coupling agent and a second liquid containing phenylsilane and diphenylsilane;
Preparing a main part by reacting the mixture by mixing distilled water and a catalyst;
Method for producing a flooring composition, characterized in that it is prepared, including.

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