KR20210073897A - Heat-resistant coating composition and method for manufacturing coated body using the same - Google Patents

Abstract

Disclosed are a heat-resistant coating composition and a method for manufacturing a coating body using the same. The heat-resistant coating composition comprises 20 to 40 parts by weight of a polysiloxane resin, 10 to 20 parts by weight of a pigment, and 45 to 50 parts by weight of a solvent. According to the present invention, since the coating composition is manufactured by using the polysiloxane resin manufactured by reacting different types of organic silanes, the content of inorganic substances contained in the heat-resistant coating composition is increased, so that heat resistance and flame retardancy are excellent.

Description

Heat-resistant coating composition and manufacturing method of a coating body using the same {HEAT-RESISTANT COATING COMPOSITION AND METHOD FOR MANUFACTURING COATED BODY USING THE SAME}

The present disclosure relates to a heat-resistant coating composition and a method for manufacturing a coating body using the same.

Recently, various types of fires are occurring, and government-level fire-related legal regulations are emerging as serious social problems, so the need for high heat-resistant coatings based on non-flammable or flame-retardant performance has been highlighted. In this regard, Korean Patent Publication No. 10-0432211 discloses a technology for a coating composition for coating the surface of an article requiring heat resistance (eg, an electric device, an automobile lamp, etc.).

Conventionally, a polymer composite coating agent or inorganic ceramic coating agent was manufactured by adding an inorganic filler to an organic binder. However, the polymer composite coating agent has poor heat resistance properties due to the high content of organic matter, and harmful gas is generated during the flame retardant test, and the inorganic ceramic coating agent has storage stability. Due to problems such as deterioration in compatibility and stability, the development of a heat-resistant coating agent having excellent stability and heat resistance and excellent compatibility is required.

The technical idea of the present disclosure is to solve the above problems, and it is an object of the present disclosure to provide a technology capable of improving heat resistance and coating film properties while reducing the content of organic matter and increasing the content of inorganic matter.

The problems to be solved by the present invention are not limited to the above problems, and other technical problems not mentioned will be clearly understood by those of ordinary skill in the art to which the present invention belongs from the following description.

In order to achieve this object, as an embodiment of the present invention, the heat-resistant coating composition comprises 20 to 40 parts by weight of a polysiloxane resin; 10 to 20 parts by weight of a pigment; and 45 to 50 parts by weight of a solvent.

In addition, the heat-resistant coating composition may contain 5 to 10 parts by weight of an additive; and 0.1 to 2 parts by weight of silica.

In addition, the polysiloxane resin may be prepared by reacting different types of organic silanes.

In addition, the organosilane is methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, n-propyltrimethoxysilane, n-propyltriethoxysilane, i-propyltrimethyl Toxysilane, i-propyltriethoxysilane, n-butyltrimethoxysilane, n-butyltriethoxysilane, n-pentyltrimethoxysilane, n-hexyltrimethoxysilane, n-heptyltrimethoxysilane , n-octyltrimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, cyclohexyltrimethoxysilane, cyclohexyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, 3-chloro Propyltrimethoxysilane, 3-chloropropyltriethoxysilane, 3,3,3-trifluoropropyltrimethoxysilane, 3,3,3-trifluoropropyltriethoxysilane, 3-aminopropyltri Methoxysilane, 3-aminopropyltriethoxysilane, 2-hydroxyethyltrimethoxysilane, 2-hydroxyethyltriethoxysilane, 2-hydroxypropyltrimethoxysilane, 2-hydroxypropyltrie Toxysilane, 3-hydroxypropyltrimethoxysilane, 3-hydroxypropyltriethoxysilane, 3-mercaptopropyltrimethoxysilane, 3-mercaptopropyltriethoxysilane, 3-isocyanatepropyltrimethoxy Silane, 3-isocyanatepropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltriethoxysilane, 3-(meth)acryloxypropyltrimethoxysilane, 3-(meth)acryloxypropyltriethoxysilane, 3-ureidopropyltrimethyl Toxysilane, 3-ureidopropyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, diethyldimethoxysilane, diethyldiethoxysilane, di-n-propyldimethoxysilane, di-n-propyldie Toxysilane, di-i-propyldimethoxysilane, di-i-propyldiethoxysilane, di-n-butyldimethoxysilane, di-n-butyldiethoxysilane, di-n-pentyldimethoxysilane, di- n-pentyldiethoxysilane, di-n-hexyldimethoxysilane, di-n-heptyldimethoxysilane, di-n-heptyldiethoxysilane, di-n-octyldimethoxysilane, di-n-octyldiethoxy Silane, di-n-cyclohexyldimethoxysilane, di-n-cyclohexyldiethoxysilane, di At least one selected from the group consisting of phenyldimethoxysilane and diphenyldiethoxysilane may be provided.

In addition, the polysiloxane resin is prepared by reacting 40 to 60 parts by weight of the methyltrimethoxysilane and 15 to 25 parts by weight of the n-propyltrimethoxysilane and 30 to 65 parts by weight of an organic solvent, and the organic solvent is xylene, At least one selected from the group consisting of butyl acetate, butyl cellosolve, ethyl alcohol, isopropyl alcohol, butyl alcohol, methyl ethyl ketone, methyl isobutyl ketone and propylene glycol monomethyl ether acetate may be provided.

On the other hand, the polysiloxane resin is 40 to 60 parts by weight of the methyltrimethoxysilane, 15 to 25 parts by weight of the n-propyltrimethoxysilane, and 0 to 6 parts by weight of the 3-(meth)acryloxypropyltrimethoxysilane and 30 to 65 parts by weight of an organic solvent, wherein the organic solvent is xylene, butyl acetate, butyl cellosolve, ethyl alcohol, isopropyl alcohol, butyl alcohol, methyl ethyl ketone, methyl isobutyl ketone and propylene glycol mono It may be provided with at least one selected from the group consisting of methyl ether acetate.

In order to achieve this object, as another embodiment of the present invention, a method for manufacturing a coating body using a heat-resistant coating composition includes a coating step of applying the aforementioned heat-resistant coating composition to an object to be coated; and a curing step of curing the coating layer formed in the coating step.

Means for solving the above problems are merely exemplary, and should not be construed as limiting the present invention. In addition to the exemplary embodiments described above, there may be additional embodiments described in the drawings and detailed description.

As described above, according to various embodiments of the present invention, since the coating composition is prepared using a polysiloxane resin prepared by reacting different types of organic silanes, the content of inorganic substances contained in the heat-resistant coating composition is increased, so that heat resistance and flame retardancy are improved. It has an excellent effect.

In addition, according to various embodiments of the present invention, propyltrimethoxysilane (or propyltrimethoxysilane and methacryloxypropyltrimethoxysilane) is added in a certain amount to methyltrimethoxysilane during the preparation of the polysiloxane resin, and together By reacting the polysiloxane resin to synthesize it, there is an advantage in that the coating film properties such as flame retardancy, curability, adhesion, hardness, and solvent resistance are excellent while maintaining the high inorganic content of the heat-resistant coating composition.

Effects of the present invention are not limited to the effects mentioned above, and other effects not mentioned will be clearly understood by those skilled in the art from the description of the claims.

1 is a flowchart illustrating a method for manufacturing a coating body according to an embodiment of the present invention.

A preferred embodiment of the present invention will be described in more detail with reference to the accompanying drawings, but already known technical parts will be omitted or compressed for the sake of brevity of description.

It should be noted that references herein to “one” or “an” embodiment of the invention are not necessarily to the same embodiment, and they mean at least one.

In the following examples, the singular expression includes the plural expression unless the context clearly dictates otherwise.

In the following embodiments, terms such as include or have means that the features or components described in the specification are present, and the possibility that one or more other features or components may be added is not excluded in advance.

In the following embodiments, when it is said that a part such as a film, region, or component is on or on another part, it is not only when it is directly on the other part, but also another film, region, component, etc. is interposed therebetween. Including cases where there is

Where certain embodiments are otherwise feasible, a specific process sequence may be performed different from the described sequence. For example, two processes described in succession may be performed substantially simultaneously, or may be performed in an order opposite to the order described. That is, each step of the method described herein may be appropriately performed in any order unless otherwise stated in the specification or clearly contradicted by context.

The term "about" used in front of a numerical value throughout this specification is used in or close to the numerical value when manufacturing and material tolerances inherent in the stated meaning are presented, and is intended to be accurate or accurate to aid understanding of the present application. Absolute figures are used to prevent unreasonable exploitation of the stated disclosure by unscrupulous infringers.

<Description of the heat-resistant coating composition>

The heat-resistant coating composition according to an embodiment of the present invention may include a polysiloxane resin, a pigment, and a solvent. In one embodiment, the polysiloxane resin may be prepared by reacting different types of organic silanes. Here, the organosilane is methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, n-propyltrimethoxysilane, n-propyltriethoxysilane, i-propyltrimethyl Toxysilane, i-propyltriethoxysilane, n-butyltrimethoxysilane, n-butyltriethoxysilane, n-pentyltrimethoxysilane, n-hexyltrimethoxysilane, n-heptyltrimethoxysilane , n-octyltrimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, cyclohexyltrimethoxysilane, cyclohexyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, 3-chloro Propyltrimethoxysilane, 3-chloropropyltriethoxysilane, 3,3,3-trifluoropropyltrimethoxysilane, 3,3,3-trifluoropropyltriethoxysilane, 3-aminopropyltri Methoxysilane, 3-aminopropyltriethoxysilane, 2-hydroxyethyltrimethoxysilane, 2-hydroxyethyltriethoxysilane, 2-hydroxypropyltrimethoxysilane, 2-hydroxypropyltrie Toxysilane, 3-hydroxypropyltrimethoxysilane, 3-hydroxypropyltriethoxysilane, 3-mercaptopropyltrimethoxysilane, 3-mercaptopropyltriethoxysilane, 3-isocyanatepropyltrimethoxy Silane, 3-isocyanatepropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltriethoxysilane, 3-(meth)acryloxypropyltrimethoxysilane, 3-(meth)acryloxypropyltriethoxysilane, 3-ureidopropyltrimethyl Toxysilane, 3-ureidopropyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, diethyldimethoxysilane, diethyldiethoxysilane, di-n-propyldimethoxysilane, di-n-propyldie Toxysilane, di-i-propyldimethoxysilane, di-i-propyldiethoxysilane, di-n-butyldimethoxysilane, di-n-butyldiethoxysilane, di-n-pentyldimethoxysilane, di- n-pentyldiethoxysilane, di-n-hexyldimethoxysilane, di-n-heptyldimethoxysilane, di-n-heptyldiethoxysilane, di-n-octyldimethoxysilane, di-n-octyldiethoxy silane, di-n-cyclohexyldimethoxysilane, di-n-cyclohexyldiethoxysilane, At least one selected from the group consisting of diphenyldimethoxysilane and diphenyldiethoxysilane may be provided.

The polysiloxane resin according to an embodiment may be prepared through hydrolysis and condensation reactions. That is, the polysiloxane resin can be obtained through a hydrocondensation reaction by adding various kinds of organic silanes, organic solvents, catalysts, and water under constant temperature conditions.

In one embodiment, an organic solvent and a catalyst are added to a mixture of two or more organic silanes, and the polysiloxane resin is synthesized by stirring at a temperature of room temperature (for example, 25° C.) to 150° C. for 1 hour to 24 hours. have. In addition, distillation and removal of hydrolysis by-products or condensation by-products may be performed during stirring. In addition, the reaction temperature and stirring time during the preparation of the polysiloxane resin may be appropriately changed according to the experimental conditions.

The polysiloxane resin according to an embodiment may be prepared by reacting 40 to 60 parts by weight of methyltrimethoxysilane and 15 to 25 parts by weight of propyltrimethoxysilane. As a specific example, the content of methyltrimethoxysilane is about 40 parts by weight, about 41 parts by weight, about 42 parts by weight, about 43 parts by weight, about 44 parts by weight, about 45 parts by weight, about 46 parts by weight, about 47 parts by weight. parts, about 48 parts by weight, about 49 parts by weight, about 50 parts by weight, about 51 parts by weight, about 52 parts by weight, about 53 parts by weight, about 54 parts by weight, about 55 parts by weight, about 56 parts by weight, about 57 parts by weight parts, about 58 parts by weight, about 59 parts by weight, or about 60 parts by weight. Also, the content of methyltrimethoxysilane may be in the range of at least one of the above values and less than or equal to one of the above values.

For example, the content range of methyltrimethoxysilane is about 40 parts by weight to about 50 parts by weight, about 50 parts by weight to about 60 parts by weight, about 45 parts by weight to about 55 parts by weight, about 45 parts by weight to about 60 parts by weight. It may be provided in an amount of from about 40 parts by weight to about 60 parts by weight or by weight. Methyltrimethoxysilane according to an embodiment may maintain the physical properties and flame retardancy of the coating film at an excellent level within the above range.

If the amount of methyltrimethoxysilane is less than 40 parts by weight, the content of inorganic substances in the polysiloxane resin is reduced, and as a result, the content of inorganic substances contained in the heat-resistant coating composition decreases, so that heat resistance and heat resistance may be reduced, and if it exceeds 60 parts by weight, Since the inorganic content in the heat-resistant coating composition is too high, there is a risk that the coating film may be cracked or the coating film properties may be deteriorated. Therefore, the amount of methyltrimethoxysilane added during the synthesis of the polysiloxane resin is preferably applied within the above-described range.

On the other hand, in an embodiment, the content of propyltrimethoxysilane may be applied in an amount of 15 to 25 parts by weight when synthesizing the polysiloxane resin. As a specific example, the content of propyltrimethoxysilane is about 15 parts by weight, about 16 parts by weight, about 17 parts by weight, about 18 parts by weight, about 19 parts by weight, about 20 parts by weight, about 21 parts by weight, about 22 parts by weight. parts, about 23 parts by weight, about 24 parts by weight, or about 25 parts by weight. In addition, the content of propyltrimethoxysilane may be in the range of at least one of the above values and less than or equal to one of the above values.

For example, the content range of propyltrimethoxysilane may be about 15 parts by weight to about 20 parts by weight, 20 parts by weight to about 25 parts by weight, or about 15 parts by weight to about 25 parts by weight. Propyltrimethoxysilane according to an embodiment may prevent cracks in the coating film and maintain the stability of the coating film within the above range.

If the amount of propyltrimethoxysilane is less than 15 parts by weight, the content of methyltrimethoxysilane is relatively high and the content of inorganic substances increases, so that the coating film stability is deteriorated and cracks may occur in the coating film, and the propyltrimethoxysilane content is 25 When it exceeds parts by weight, the content of propyltrimethoxysilane is preferably applied within the above-described range because there is a risk that heat resistance and flame retardancy may be deteriorated as the content of organic matter in the polysiloxane resin increases.

Meanwhile, in another embodiment, the polysiloxane resin is 40 to 60 parts by weight of methyltrimethoxysilane, 15 to 25 parts by weight of propyltrimethoxysilane, and 0 to 6 parts by weight of 3-(meth)acryloxypropyltrimethoxysilane. can be manufactured by When methacryloxypropyltrimethoxysilane is added together with methyltrimethoxysilane and propyltrimethoxysilane to make a polysiloxane resin, other components included in the heat-resistant coating composition due to organic matter contained in methacryloxypropyltrimethoxysilane Compatibility with other materials may be improved, and crosslinking density and curability may be further improved upon curing of the heat-resistant coating composition.

As a specific example, the content of methacryloxypropyltrimethoxysilane is about 0.1 parts by weight, about 0.5 parts by weight, about 1 part by weight, about 2 parts by weight, about 3 parts by weight, about 4 parts by weight, about 5 parts by weight or It may be provided in about 6 parts by weight. In addition, the content of methacryloxypropyltrimethoxysilane may be in the range of at least one of the above values and less than or equal to one of the above values.

For example, the content range of methacryloxypropyltrimethoxysilane is about 0.1 parts by weight to about 6 parts by weight, about 0.5 parts by weight to about 6 parts by weight, about 1 part by weight to about 6 parts by weight, about 2 parts by weight. to about 6 parts by weight, about 3 parts by weight to about 6 parts by weight, about 4 parts by weight to about 6 parts by weight, about 5 parts by weight to about 6 parts by weight, or about 2 parts by weight to about 5 parts by weight. have. Methacryloxypropyltrimethoxysilane according to an embodiment can be easily cured within the above range and maintain the physical properties of the coating film at an excellent level. If the amount of methacryloxypropyltrimethoxysilane exceeds 6 parts by weight, the organic content in the heat-resistant coating composition is excessively increased, so that the hardness of the coating film decreases and there is a risk of yellowing. Therefore, when synthesizing the polysiloxane resin, methacryloxypropyltri When methoxysilane is added, it is preferably applied in an amount of 6 parts by weight or less.

When preparing the polysiloxane resin according to an embodiment, at least one of xylene, butyl acetate, and butyl cellosolve may be applied as a usable organic solvent. The organic solvent content is 30 to 65 parts by weight (eg, 30 parts by weight, 35 parts by weight, 40 parts by weight, 45 parts by weight, 50 parts by weight, 55 parts by weight, 56 parts by weight, 57 parts by weight, 58 parts by weight, 59 parts by weight, 60 parts by weight, 61 parts by weight, 62 parts by weight, 63 parts by weight, 64 parts by weight or 65 parts by weight).

As a specific example, the content of the organic solvent added during the preparation of the polysiloxane resin may be about 30 parts by weight, about 40 parts by weight, about 55 parts by weight, about 60 parts by weight, or about 65 parts by weight. In addition, the content of the organic solvent may be in the range of at least one of the above values and less than or equal to one of the above values. For example, the content range of the organic solvent may be provided in a range of about 30 parts by weight to about 60 parts by weight or about 62 parts by weight to about 65 parts by weight.

In one embodiment, the organic solvent may be applied in 60 parts by weight of xylene alone. When polysiloxane resin is synthesized using xylene, moisture content can be reduced and resistance value can be lowered, so electrostatic coating of paints is also possible. In another embodiment, 40 parts by weight of xylene and 20 parts by weight of butyl cellosolve may be mixed and applied as an organic solvent for coatability, compatibility, and stability of the coating film.

And, in the preparation of the polysiloxane resin according to an embodiment, the usable catalyst is an acid or basic catalyst, and at least one of acetic acid, formic acid, hydrochloric acid, nitric acid, phosphoric acid, aqueous ammonia and sodium hydroxide may be applied. . For example, when synthesizing the polysiloxane resin, 0.1 to 0.15N HCl may be used as a catalyst consisting of water and an acid.

In addition, in one embodiment, the content of the catalyst for the hydrolysis and condensation reaction is 10 to 20 parts by weight (eg, 10 parts by weight, 11 parts by weight, 12 parts by weight, 13 parts by weight, 14 parts by weight, 15 parts by weight) , 16 parts by weight, 17 parts by weight, 18 parts by weight, 19 parts by weight, 20 parts by weight). As a specific example, the amount of the catalyst for hydrolysis and condensation added during the preparation of the polysiloxane resin may be about 10 parts by weight, about 15 parts by weight, or about 20 parts by weight. And, the content of the catalyst for the hydrolysis and condensation reaction may be in the range of at least one of the above values and less than or equal to one of the above values. For example, the content range of the catalyst for the hydrolysis and condensation reaction may be provided in the range of about 10 parts by weight to about 15 parts by weight or about 16 parts by weight to about 20 parts by weight. Of course, the content range of the catalyst is not limited to the above-described range, and may be flexibly changed according to the content of the organosilane input during the synthesis of the polysiloxane resin. In addition, in one embodiment, the concentration of the catalyst for the hydrolysis and condensation reaction may be applied in a variety of ranges from 0.01N to 10N concentration.

In one embodiment, the polysiloxane resin may be provided in an amount of 20 to 40 parts by weight. As a specific example, the content of the polysiloxane resin is about 20 parts by weight, about 21 parts by weight, about 22 parts by weight, about 23 parts by weight, about 24 parts by weight, about 25 parts by weight, about 26 parts by weight, about 27 parts by weight, about 28 parts by weight. parts by weight, about 29 parts by weight, about 30 parts by weight, about 31 parts by weight, about 32 parts by weight, about 33 parts by weight, about 34 parts by weight, about 35 parts by weight, about 36 parts by weight, about 37 parts by weight, about 38 parts by weight It may be provided in parts by weight, about 39 parts by weight, or about 40 parts by weight. In addition, the content range of the polysiloxane resin may be in the range of at least one of the above numerical values and less than or equal to one of the above numerical values.

For example, the content range of the polysiloxane resin is about 20 parts by weight to about 25 parts by weight, about 20 parts by weight to about 30 parts by weight, about 20 parts by weight to about 35 parts by weight, about 20 parts by weight to about 40 parts by weight; It may be provided in the range of about 20 parts by weight to about 34 parts by weight, about 22 parts by weight to about 36 parts by weight, about 24 parts by weight to about 38 parts by weight, or about 20 parts by weight to about 40 parts by weight. The polysiloxane resin according to an embodiment may maintain heat resistance and flame retardancy at an excellent level within the above range.

If the amount of the polysiloxane resin is less than 20 parts by weight, the content of inorganic substances in the total heat-resistant coating composition decreases, heat resistance and flame retardancy may decrease and hardness may be lowered. If it exceeds 40 parts by weight, the coating film hardness becomes too high to cause cracks or the substrate Since there is a risk of lowering adhesion with the polysiloxane resin, the content of the polysiloxane resin is preferably applied within the above-described range.

In one embodiment, the content of the pigment may be applied in an amount of 10 to 20 parts by weight. As a specific example, the content of the pigment is about 10 parts by weight, about 11 parts by weight, about 12 parts by weight, about 13 parts by weight, about 14 parts by weight, about 15 parts by weight, about 16 parts by weight, about 17 parts by weight, about 18 parts by weight. parts, about 19 parts by weight, or about 20 parts by weight. Further, the content of the pigment may be in the range of at least one of the above values and less than or equal to one of the above values.

For example, the content range of the pigment is in the range of about 10 parts by weight to about 15 parts by weight, about 12 parts by weight to about 17 parts by weight, about 15 parts by weight to about 20 parts by weight, or about 10 parts by weight to about 20 parts by weight. can be provided. The pigment according to an embodiment may maintain the coating film properties at an excellent level within the above range. If the amount of the pigment is less than 10 parts by weight, it may be difficult to realize the color of the paint due to a decrease in hiding power, and if it exceeds 20 parts by weight, aggregation of the pigment particles occurs due to an increase in the content of the pigment, resulting in reduced dispersibility and increased viscosity As a result, the paint workability may be deteriorated.

The heat-resistant coating composition according to an embodiment may include 45 to 50 parts by weight of a solvent (eg, 45 parts by weight, 46 parts by weight, 47 parts by weight, 48 parts by weight, 49 parts by weight, 50 parts by weight) for coating properties and painting workability. ) may be included. Here, the solvent may be applied to ethyl alcohol, isopropyl alcohol, butyl alcohol, butyl cellusolve, xylene, methyl ethyl ketone, methyl isobutyl ketone or propylene glycol monomethyl ether acetate, but is not limited to the above-described examples and is known Other types may be used as solvents. In addition, the content of the solvent may be appropriately adjusted in consideration of the content of other components added to the heat-resistant coating composition.

The heat-resistant coating composition according to an embodiment may further include 5 to 10 parts by weight of an additive (eg, 5 parts by weight, 6 parts by weight, 7 parts by weight, 8 parts by weight, 9 parts by weight, or 10 parts by weight). . In one embodiment, as the additive, at least one may be selected from the group consisting of a general dispersing agent, an antifoaming agent, a leveling agent, and a viscosity stabilizer, and two or more additives may be mixed in an appropriate amount to exhibit optimal coating film performance. .

And, the heat-resistant coating composition according to an embodiment may further include 0.1 to 2 parts by weight of silica (eg, 0.1 parts by weight, 0.5 parts by weight, 1 part by weight, or 2 parts by weight). In an embodiment, the silica may be prepared as fumed silica.

<Description of the manufacturing method of the coating body using the heat-resistant coating composition>

A method of manufacturing a coating body according to an embodiment of the present invention will be described according to the flowchart shown in FIG. 1, but for convenience, the order will be attached. As used herein, the coating means an interior or exterior material in which a heat-resistant coating composition is coated on the surface of an object to be coated and cured to form a coating layer. For example, the coating body may be applied as an automobile interior material or subway interior material in which a coating layer of a heat-resistant coating composition is formed on the surface. However, the article on which the heat-resistant coating composition can be coated is not limited to the above-described example, and may be applied to other articles such as interior materials or exterior materials for construction requiring heat resistance and flame retardancy.

1. Coating step <S101>

In this step, the above-described heat-resistant coating composition may be applied to the object to form a coating layer on the surface of the object to be coated. In this step, a coating layer may be formed on the surface of the object to be coated with a coating film thickness of 15 to 30 μm. As a specific example, the thickness of the coating film coated on the surface of the object to be coated is about 15 μm, about 16 μm, about 17 μm, about 18 μm, about 19 μm, about 20 μm, about 21 μm, about 22 μm, about 23 μm, about 24 μm, about 25 μm, about 26 μm, about 27 μm, about 28 μm, about 29 μm, or about 30 μm. In addition, the thickness of the coating film may be applied in a range of at least one of the above values and less than or equal to one of the above values. For example, the range of the thickness of the coating film coated on the object to be coated is about 15 μm to about 16 μm, about 16 μm to about 17 μm, about 17 μm to about 18 μm, about 18 μm to about 19 μm, about 19 μm. to about 20 μm or about 15 μm to about 30 μm may be provided.

The coating method performed in this step is not limited to any specific method as long as it is a method of forming a coating layer by coating a paint on the substrate, which is the object to be coated, bar coating, slit coating, dip coating, roll coating, spin coating, spray coating, needle coating A person skilled in the art can arbitrarily select and apply it from among known coating methods such as a paper method, an impregnation method, and a gravure coating.

2. Curing step <S102>

In this step, the coating layer formed in step S101 may be cured. In one embodiment, heat treatment may be performed on the coating layer. As a specific example, in this step, the coating layer may be thermally cured at a temperature of 50 to 250° C. for 10 to 60 minutes. The heat treatment temperature and time performed in this step may be adjusted within an appropriate range so that the coating layer can be sufficiently cured.

Hereinafter, the present invention will be described in more detail through specific examples and experimental examples. Since the following Examples and Experimental Examples are merely examples to help the understanding of the present invention, the scope of the present invention is not limited or limited thereto.

1. Synthesis of polysiloxane resin

Table 1 shows methyltrimethoxysilane, n-propyltrimethoxysilane, and 3-(meth)acryloxypropyltrimethoxysilane in a 4-neck glass flask reactor equipped with a reflux condenser, nitrogen inlet, stirrer and heating device. It was added to the indicated content (unit: g), and 60 g of xylene and 15 g of 0.1N HCl were added, and the mixture was stirred at 60° C. for 8 hours under a nitrogen stream. After stirring, the reaction product was put into a vacuum distiller under reduced pressure, and the reaction product was vacuum distilled at 40° C. for 30 minutes to remove unreacted substances, reaction by-products and moisture, and filtered through a 1 μm bag filter to obtain a polysiloxane resin.

ingredient Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 ¹ methyltrimethoxysilane 40 50 60 39 61 ² n-propyltrimethoxysilane 25 20 15 26 14 ³ 3-(meth)acryloxypropyltrimethoxysilane 4 6 2 7 8
week)
1: Methyltrimethoxysilane - Manufacturer DOW, Product Name OFS-6060
2: n-propyltrimethoxysilane - manufacturer HUBEI BLUESKY, product name D-2401
3: 3-(meth)acryloxypropyltrimethoxysilane - Manufacturer QUFU chenguang chemical, Product name CG-0174

2. Preparation of a heat-resistant coating composition using the polysiloxane resin of Example 1

Mix in the same composition as in Table 2 below, but blend each polysiloxane resin, pigment, solvent, additive (dispersant, defoaming agent, leveling agent) and silica at the content (unit: g) shown in Table 2 below in a 1L container, After stirring for 1 hour, the heat-resistant coating composition was completed.

ingredient manufacturing example
One manufacturing example
2 manufacturing example
3 Comparative Preparation Example 1 Comparative Preparation Example 2 ¹ Polysiloxane resin 20 30 40 19 41 ² pigment 20 15 10 21 9 ³ solvent 50 47 45 51 44 ⁴ dispersant 2 2 2 2 2 ⁵ Antifoam 2 2 2 2 2 ⁶ Silica 2 2 2 2 2
week)
1: Polysiloxane resin - Example 1
2: Pigment - manufacturer Cristal, product name Tiona RCl 575
3: Solvent - A solvent in which xylene (manufacturer GS Caltex, product name Xylene) and butyl cellosolve (manufacturer Yeocheon NCC, product name Butyl cellosolve) are mixed in a weight ratio of 2:1
4: Dispersant - manufacturer BYK, product name Disperbyk 182
5: Defoamer - manufacturer BYK, product name BYK-054
6: Silica - manufacturer Evonik, product name Aerosil R 972

3. Preparation of heat-resistant coating composition using polysiloxane resin of Example 2

Mix in the same composition as in Table 3 below, but blend each polysiloxane resin, pigment, solvent, additive (dispersant, defoaming agent, leveling agent) and silica at the content (unit: g) shown in Table 3 below in a 1L container, After stirring for 1 hour, the heat-resistant coating composition was completed.

ingredient manufacturing example
4 manufacturing example
5 manufacturing example
6 Comparative Preparation Example 3 Comparative Preparation Example 4 ¹ Polysiloxane resin 20 30 40 19 41 ² pigment 20 15 10 21 9 ³ solvent 50 47 45 51 44 ⁴ dispersant 2 2 2 2 2 ⁵ Antifoam 2 2 2 2 2 ⁶ Silica 2 2 2 2 2
week)
1: Polysiloxane resin - Example 2
2: Pigment - manufacturer Cristal, product name Tiona RCl 575
3: Solvent - A solvent in which xylene (manufacturer GS Caltex, product name Xylene) and butyl cellosolve (manufacturer Yeocheon NCC, product name Butyl cellosolve) are mixed in a weight ratio of 2:1
4: Dispersant - manufacturer BYK, product name Disperbyk 182
5: Defoamer - manufacturer BYK, product name BYK-054
6: Silica - manufacturer Evonik, product name Aerosil R 972

4. Preparation of heat-resistant coating composition using polysiloxane resin of Example 3

Mix in the same composition as in Table 4 below, but blend each polysiloxane resin, pigment, solvent, additive (dispersant, defoaming agent, leveling agent) and silica at the content (unit: g) shown in Table 4 below in a 1L container, After stirring for 1 hour, the heat-resistant coating composition was completed.

ingredient manufacturing example
7 manufacturing example
8 manufacturing example
9 Comparative Preparation Example 5 Comparative Preparation Example 6 ¹ Polysiloxane resin 20 30 40 19 41 ² pigment 20 15 10 21 9 ³ solvent 50 47 45 51 44 ⁴ dispersant 2 2 2 2 2 ⁵ Antifoam 2 2 2 2 2 ⁶ Silica 2 2 2 2 2
week)
1: Polysiloxane resin - Example 3
2: Pigment - manufacturer Cristal, product name Tiona RCl 575
3: Solvent - A solvent in which xylene (manufacturer GS Caltex, product name Xylene) and butyl cellosolve (manufacturer Yeocheon NCC, product name Butyl cellosolve) are mixed in a weight ratio of 2:1
4: Dispersant - manufacturer BYK, product name Disperbyk 182
5: Defoamer - manufacturer BYK, product name BYK-054
6: Silica - manufacturer Evonik, product name Aerosil R 972

5. Preparation of a heat-resistant coating composition using the polysiloxane resin of Comparative Example 1

Mix in the same composition as in Table 5 below, but blend each polysiloxane resin, pigment, solvent, additive (dispersant, defoaming agent, leveling agent) and silica at the content (unit: g) shown in Table 5 below in a 1L container, After stirring for 1 hour, the heat-resistant coating composition was completed.

ingredient Comparative Preparation Example 7 Comparative Preparation Example 8 Comparative Preparation Example 9 ¹ Polysiloxane resin 20 30 40 ² pigment 20 15 10 ³ solvent 50 47 45 ⁴ dispersant 2 2 2 ⁵ Antifoam 2 2 2 ⁶ Silica 2 2 2
week)
1: Polysiloxane resin - Comparative Example 1
2: Pigment - manufacturer Cristal, product name Tiona RCl 575
3: Solvent - A solvent in which xylene (manufacturer GS Caltex, product name Xylene) and butyl cellosolve (manufacturer Yeocheon NCC, product name Butyl cellosolve) are mixed in a weight ratio of 2:1
4: Dispersant - manufacturer BYK, product name Disperbyk 182
5: Defoamer - manufacturer BYK, product name BYK-054
6: Silica - manufacturer Evonik, product name Aerosil R 972

6. Preparation of heat-resistant coating composition using polysiloxane resin of Comparative Example 2

Mix in the same composition as in Table 6 below, but blend each polysiloxane resin, pigment, solvent, additive (dispersant, defoaming agent, leveling agent) and silica at the content (unit: g) shown in Table 6 below in a 1L container, After stirring for 1 hour, the heat-resistant coating composition was completed.

ingredient Comparative Preparation Example 10 Comparative Preparation Example 11 Comparative Preparation Example 12 ¹ Polysiloxane resin 20 30 40 ² pigment 20 15 10 ³ solvent 50 47 45 ⁴ dispersant 2 2 2 ⁵ Antifoam 2 2 2 ⁶ Silica 2 2 2
week)
1: Polysiloxane resin - Comparative Example 2
2: Pigment - manufacturer Cristal, product name Tiona RCl 575
3: Solvent - A solvent in which xylene (manufacturer GS Caltex, product name Xylene) and butyl cellosolve (manufacturer Yeocheon NCC, product name Butyl cellosolve) are mixed in a weight ratio of 2:1
4: Dispersant - manufacturer BYK, product name Disperbyk 182
5: Defoamer - manufacturer BYK, product name BYK-054
6: Silica - manufacturer Evonik, product name Aerosil R 972

7. Preparation of test specimens

Each heat-resistant coating composition was applied to a steel sheet having a size of 7 cm X 15 cm by spraying so that the thickness of the coating film was 25 μm. Thereafter, the coating layer was cured at 230° C. for 10 minutes to prepare a test specimen.

8. Test and Evaluation Methods

For the test specimens prepared as described above, the curability, adhesion, hardness, solvent resistance and flame retardancy of the coating film were evaluated through the method described below, and the results are shown in Table 7.

Experimental environment conditions

The test environment, that is, the place where the test is conducted, should be in a place where there is no direct sunlight and very little gas, steam, dust and ventilation at a temperature of 23±2℃ and humidity of 50±5% (hereinafter referred to as ‘room temperature’), and the test specimen In principle, those left for more than 48 hours after painting were used for the experiment.

Hardenability evaluation

It was checked whether a nail scratch occurred by scraping the coating film of the cured test specimen with a nail. When a nail scratch occurred, hardenability was evaluated as poor, and when it did not occur, it was evaluated as good.

Adhesion evaluation

A cross-cutting test method was performed on the cured coating film of the test specimen, and a glass tape was used at this time. That is, the film or layer formed on the specimen is cut into 100 checkered slices with a size of 1 mm * 1 mm, and a glass tape is attached to the slice. gender was evaluated.

Hardness evaluation

For hardness evaluation, a 45° inclination using a Mitsubishi pencil and a 1 kg load were applied to evaluate whether the coating film was abnormal when moving 2 cm. In 5 evaluations, the maximum pencil hardness value was recorded when there were no scratches in all 5 times.

Solvent resistance evaluation

After methyl ethyl ketone was applied to the gauze, the gauze was rubbed with a certain force on the specimen on which the coating film was formed, and the number of times the gauze was rubbed until the coating film was peeled off to reveal the substrate was measured.

Flame-retardant evaluation

When measured by the non-combustible test method (KS F ISO 1182), the mass reduction rate is 30% or less, and when measured by the gas toxicity test method (KS F 2271), the gas toxicity (average behavior of mice due to the combustion gas of the specimen when 8 mice are observed If the stopping time) is 11 minutes or more, the flame retardancy is evaluated as excellent, and if all of the above conditions are not satisfied, the flame retardancy is evaluated as poor.

division hardenability adherence Hardness solvent resistance flame retardant Preparation Example 1 bad 100/100 4H 40 episodes bad Preparation 2 Good 100/100 4H 50 episodes Great Preparation 3 Good 100/100 3-4H 50 episodes Great Preparation 4 Good 100/100 5H 50 episodes Great Preparation 5 Good 100/100 4~5H 50 episodes Great Preparation 6 Good 95/100 4~5H 50 episodes Great Preparation 7 Good 95/100 5H 50 episodes Great Preparation 8 Good 90/100 5H 50 episodes Great Preparation 9 Good 85/100 5H 50 episodes Great Comparative Preparation Example 1 bad 90/100 4H 40 episodes bad Comparative Preparation Example 2 Good 90/100 4H 50 episodes Great Comparative Preparation Example 3 bad 90/100 4~5H Episode 45 bad Comparative Preparation Example 4 Good 95/100 5H 50 episodes Great Comparative Preparation Example 5 bad 95/100 5H 50 episodes bad Comparative Preparation Example 6 Good 85/100 5H 50 episodes Great Comparative Preparation Example 7 bad 100/100 4H 40 episodes bad Comparative Preparation Example 8 Good 100/100 4H Episode 45 bad Comparative Preparation Example 9 Good 100/100 3H 50 episodes bad Comparative Preparation Example 10 Good 85/100 5H 50 episodes Great Comparative Preparation Example 11 Good 85/100 5H 50 episodes Great Comparative Preparation Example 12 Good 80/100 5H 50 episodes Great

As shown in Table 7, it can be seen that Preparation Examples 1 to 9 of the present invention are at an overall excellent level in surface properties such as curing, adhesion, hardness, solvent resistance and flame retardancy of the coating film. And, through the experimental results of Comparative Preparation Examples 1 to 6, when the content of each component included in the coating composition exceeds or is less than the input amount range for each component, it can be confirmed that the surface properties of the coating film are relatively lowered compared to those of Preparation Examples. can In addition, looking at the results of Comparative Preparation Examples 7 to 12, even if the content of the polysiloxane resin is set to be the same as in Preparation Examples, when the content of each organosilane constituting the polysiloxane resin is outside a specific range, the coating film properties are lowered. Able to know.

9. Additional Fabrication of Test Specimens and Determination of Inorganic Content

The polysiloxane resins of Examples 1 to 3 were spray-coated on a steel sheet having a size of 7 cm X 15 cm so that the thickness of the coating film was 25 μm. Thereafter, the coating layer was cured at 230° C. for 10 minutes to prepare a test specimen. The prepared specimen was put into a thermogravimetric analysis, and the inorganic material content was measured at a high temperature of 750° C. or higher. Table 8 shows the results of the measured mineral content.

division Example 1 Example 2 Example 3 mineral content 68% by weight 70% by weight 72% by weight

As can be seen from the measurement results in Table 8, the polysiloxane resins of Examples 1 to 3 had an inorganic material content of 68 wt% or more that remained even at a high temperature of 750 ° C. or higher, indicating that the polysiloxane resin contained an inorganic material in a high proportion. .

As described above, according to various embodiments of the present invention, since the coating composition is prepared using a polysiloxane resin prepared by reacting different types of organic silanes, the content of inorganic substances contained in the heat-resistant coating composition is increased, so that heat resistance and flame retardancy are improved. It has an excellent effect.

In addition, according to various embodiments of the present invention, propyltrimethoxysilane (or propyltrimethoxysilane and methacryloxypropyltrimethoxysilane) is added in a certain amount to methyltrimethoxysilane during the preparation of the polysiloxane resin and together By reacting polysiloxane resin to synthesize polysiloxane resin, it is possible to increase the stability and compatibility of the paint while maintaining a high content of inorganic substances in the heat-resistant coating composition, and to further improve heat resistance properties. It has excellent advantages.

In addition, according to various embodiments of the present invention, since the inorganic content is relatively higher than the organic content, the amount of carbonization during combustion is small and the amount of harmful gas generated is excellent in flame retardancy. Therefore, when a heat-resistant coating composition is coated on an article requiring heat resistance to prepare a coating body, high flame retardancy properties can be secured while maintaining the aesthetics of the coating body.

As described above, the specific description of the present invention has been made by way of examples, but since the above-described exemplary embodiments have been described only with preferred examples of the present invention, it should not be understood that the present invention is limited only to the above examples. No, the scope of the present invention should be understood as the following claims and their equivalents.

Claims (7)

20 to 40 parts by weight of polysiloxane resin;
10 to 20 parts by weight of a pigment; and
45 to 50 parts by weight of a solvent; characterized in that it contains
Heat-resistant coating composition. According to claim 1,
The heat-resistant coating composition is
Additives 5 to 10 parts by weight; and
Silica 0.1 to 2 parts by weight; characterized in that it further comprises
Heat-resistant coating composition. According to claim 1,
The polysiloxane resin is characterized in that it is prepared by reacting different types of organic silanes.
Heat-resistant coating composition. 4. The method of claim 3,
The organic silane is methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, n-propyltrimethoxysilane, n-propyltriethoxysilane, i-propyltrimethoxysilane Silane, i-propyltriethoxysilane, n-butyltrimethoxysilane, n-butyltriethoxysilane, n-pentyltrimethoxysilane, n-hexyltrimethoxysilane, n-heptyltrimethoxysilane, n-octyltrimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, cyclohexyltrimethoxysilane, cyclohexyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, 3-chloropropyl Trimethoxysilane, 3-chloropropyltriethoxysilane, 3,3,3-trifluoropropyltrimethoxysilane, 3,3,3-trifluoropropyltriethoxysilane, 3-aminopropyltrimethyl Toxysilane, 3-aminopropyltriethoxysilane, 2-hydroxyethyltrimethoxysilane, 2-hydroxyethyltriethoxysilane, 2-hydroxypropyltrimethoxysilane, 2-hydroxypropyltriethoxy Silane, 3-hydroxypropyltrimethoxysilane, 3-hydroxypropyltriethoxysilane, 3-mercaptopropyltrimethoxysilane, 3-mercaptopropyltriethoxysilane, 3-isocyanatepropyltrimethoxysilane , 3-isocyanatepropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 2- (3,4-epoxycyclohexyl) ethyltrimethoxysilane, 2 -(3,4-epoxycyclohexyl)ethyltriethoxysilane, 3-(meth)acryloxypropyltrimethoxysilane, 3-(meth)acryloxypropyltriethoxysilane, 3-ureidopropyltrimethoxy Silane, 3-ureidopropyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, diethyldimethoxysilane, diethyldiethoxysilane, di-n-propyldimethoxysilane, di-n-propyldiethoxy Silane, di-i-propyldimethoxysilane, di-i-propyldiethoxysilane, di-n-butyldimethoxysilane, di-n-butyldiethoxysilane, di-n-pentyldimethoxysilane, di-n -pentyldiethoxysilane, di-n-hexyldimethoxysilane, di-n-heptyldimethoxysilane, di-n-heptyldiethoxysilane, di-n-octyldimethoxysilane, di-n-octyldiethoxysilane , di-n-cyclohexyldimethoxysilane, di-n-cyclohexyldiethoxysilane, diphene characterized in that at least one selected from the group consisting of nyldimethoxysilane and diphenyldiethoxysilane
Heat-resistant coating composition. 5. The method of claim 4,
The polysiloxane resin is prepared by reacting 40 to 60 parts by weight of the methyltrimethoxysilane, 15 to 25 parts by weight of the n-propyltrimethoxysilane, and 30 to 65 parts by weight of an organic solvent,
The organic solvent is at least one selected from the group consisting of xylene, butyl acetate, butyl cellosolve, ethyl alcohol, isopropyl alcohol, butyl alcohol, methyl ethyl ketone, methyl isobutyl ketone and propylene glycol monomethyl ether acetate. characterized by
Heat-resistant coating composition. 5. The method of claim 4,
The polysiloxane resin comprises 40 to 60 parts by weight of the methyltrimethoxysilane, 15 to 25 parts by weight of the n-propyltrimethoxysilane, and 0 to 6 parts by weight of the 3-(meth)acryloxypropyltrimethoxysilane and It is prepared by reacting 30 to 65 parts by weight of an organic solvent,
The organic solvent is at least one selected from the group consisting of xylene, butyl acetate, butyl cellosolve, ethyl alcohol, isopropyl alcohol, butyl alcohol, methyl ethyl ketone, methyl isobutyl ketone and propylene glycol monomethyl ether acetate. characterized by
Heat-resistant coating composition. A coating step of applying the heat-resistant coating composition according to any one of claims 1 to 6 to an object to be coated; and
A curing step of curing the coating layer formed in the coating step; characterized in that it comprises
A method for producing a coating body using a heat resistant coating composition.

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