KR102258690B1 - Incombustible material having heat-resistant and non-flammable properties, method of fabricating of the same, building interior material, lagging material, sound absorbing material and insulation material including the same - Google Patents

Abstract

An incombustible material comprises a coating layer on the inside and the surface of a fiber base, wherein the coating layer includes an inorganic binder, ash, and clay powder. In the present invention, a manufacturing method of the incombustible material is simple, so that manufacturing time and manufacturing cost can be easily reduced, thereby being able to easily mass-produce the fiber-reinforced fiber.

Description

Incombustible material having heat-resistant and non-flammable properties, method of fabricating of the same, building interior material, lagging material , sound absorbing material and insulation material including the same}

The present invention relates to a non-combustible material having internal and non-combustible properties and a method of manufacturing the same, and more particularly, to a non-combustible material including a coating layer on the inside and the surface of a fibrous substrate, and a method of manufacturing the same.

The non-combustible material is a material that improves the physicochemical properties of the fiber base material by inserting or coating functional materials in or on the fiber base material. For non-combustible materials, technologies are being developed to improve low density compared to strength, corrosion resistance, fatigue resistance, and flame retardancy.

For example, fiber reinforced plastics are composite materials obtained by laminating a plurality of fibrous substrates provided with a plastic-based resin and thermocompression bonding. Fiber-reinforced plastics have fire resistance, heat resistance, flame resistance and sound absorption properties. Accordingly, the fiber-reinforced plastic can be used as a building interior material, a thermal insulation material, and an insulation material in petrochemical, oil refinery, power plants, shipbuilding ships, and the like.

As the field of application increases, fiber-reinforced plastics having various functions are being studied. For example, Korean Patent Registration No. 10-1947743 discloses, based on 100 parts by weight of a bisphenol-type vinyl ester resin having an unsaturated polyester group at the end of the epoxy group, 10 to 30 parts by weight of a chlorinated vinyl chloride resin, and a maleic anhydride kraft polyvinyl chloride copolymer couple. 5 to 10 parts by weight of a ring agent, 1 to 5 parts by weight of aramid fiber, 12 to 20 parts by weight of expanded graphite, 10 to 30 parts by weight of a suppressor selected from zinc borate or aluminum hydroxide or magnesium hydroxide, 10 to 20 parts by weight of a composite flame retardant, Multilayer by forming an inner corrosion-resistant layer and a surface non-combustible layer in which the thickness ratio of the corrosion-resistant outer layer and the corrosion-resistant reinforcing layer is 1:8-10 by impregnating glass fiber with a non-flammable matrix resin composed of 1 to 1.5 parts by weight of a hardener and 0.5 to 1 parts by weight of an accelerator. To prepare a non-combustible fiber-reinforced plastic (FRP) having a structure, wherein the inner corrosion-resistant layer is a corrosion-resistant outer layer impregnated with the non-flammable matrix resin in a space mat and the non-flammable matrix resin on a chopped strand mat. A first step of forming an impregnated corrosion-resistant reinforcing layer, and a second step of forming the surface non-combustible layer by laminating a glass roving and a chopped strand mat and impregnating the non-combustible matrix resin. Disclosed is a method of manufacturing a multi-layered non-flammable fiber-reinforced plastic (FRP) for exhaust gas ducts and piping in a semiconductor manufacturing plant, characterized in that.

One technical problem to be solved by the present invention is to provide a non-combustible material and a manufacturing method with improved heat resistance.

Another technical problem to be solved by the present invention is to provide a non-combustible material and a manufacturing method with improved non-combustibility.

Another technical problem to be solved by the present invention is to provide a non-combustible material and a manufacturing method with reduced manufacturing cost.

Another technical problem to be solved by the present invention is to provide a non-combustible material and a manufacturing method with reduced manufacturing time.

Another technical problem to be solved by the present invention is to provide a non-combustible material and a manufacturing method that are easy to mass-produce.

The technical problem to be solved by the present invention is not limited to the above.

In order to solve the above technical problem, the present invention provides a method of manufacturing a non-combustible material.

According to an embodiment, the method of manufacturing a non-combustible material includes preparing an inorganic binder, ash, and clay powder, providing a solvent to the inorganic binder and stirring to prepare a base solution, and the base solution Providing and stirring the ash and the clay powder to prepare a coating agent, and applying the coating agent to a fiber substrate.

According to an embodiment, the preparing of the ash includes a first purification step of filtering the ash with a first filter to remove foreign substances, and the ash using a second filter having a higher filtering level than the first filter. Further filtering may include a secondary purification step of separating unburned carbon.

According to an embodiment, the preparing of the clay powder includes: preparing a clay mineral, first drying the clay mineral, pulverizing the clay mineral, and first filtering the clay mineral , Secondary drying the clay mineral, and secondary filtering the clay mineral.

In order to solve the above technical problem, the present invention provides a non-combustible material.

According to an embodiment, the non-combustible material includes a fibrous substrate, a coating layer on the inside and on the surface of the fibrous substrate, and the coating layer may include an inorganic binder, ash, and clay powder.

According to an embodiment, the fiber substrate may include at least one of chemical fibers such as basalt fiber, glass fiber, carbon fiber, aramid fiber, silica fiber, cotton fiber, or nylon.

According to an embodiment, the inorganic binder includes silica, an alkali metal oxide, and water, and the alkali metal oxide may include at least one of sodium (Na), potassium (K), or lithium (Li) oxide. have.

According to an embodiment, the inorganic binder may include silicon dioxide (SiO ₂ ), sodium oxide (Na ₂ O), and a compound of silicon and sodium oxide.

According to an embodiment, the clay powder is clay, kaolin, kaolinite, bentonite, zeolite, montmolinonite, nacrite, dicite ( dickite), haloysite, or gibbsite.

In order to solve the above technical problem, the present invention provides a building interior material, a thermal insulation material, a sound-absorbing material and a heat insulating material.

According to an embodiment, the building interior material, the insulating material, the sound absorbing material, and the heat insulating material include the non-combustible material according to the above-described embodiment, and have heat resistance and non-combustibility.

The method of manufacturing a non-combustible material according to an embodiment of the present invention includes preparing an inorganic binder, ash, and clay powder, providing a solvent to the inorganic binder and stirring to prepare a base solution, and the ash in the base solution And providing and stirring the clay powder to prepare a coating agent, and applying and drying the coating agent to a fiber substrate to form a coating layer. As described above, since the manufacturing method of the non-combustible material is simple, manufacturing time and manufacturing cost can be easily reduced, so that the fiber-reinforced fibers can be easily mass-produced.

The structure of the non-combustible material according to an embodiment of the present invention may be a structure including the coating layer inside and on the surface of the fibrous substrate. The coating layer may include the inorganic binder, the ash, and the clay powder. Specifically, the coating layer may be formed by volatilization of the solvent contained in the coating agent upon natural drying after the coating agent is applied to the fiber substrate. The ash in the coating layer may have heat resistance, non-flammability and flame retardancy at the same time. For example, the ash may include alumino silicate. In addition, the clay powder in the coating layer may have heat resistance and flame retardancy at the same time. For example, the clay powder may be kaolin powder. Therefore, the non-combustible material according to the embodiment of the present invention may have heat resistance and non-combustibility at the same time by the ash (eg, aluminosilicate) and the clay powder (eg, kaolin powder) in the coating layer. have. Accordingly, the non-combustible material may be used for a building interior material, a thermal insulation material, a sound absorbing material and a heat insulation material.

1 is a flow chart illustrating a method of manufacturing a non-combustible material according to an embodiment of the present invention.
2 is a view for explaining a step of preparing a base solution according to an embodiment of the present invention.
3 is a view for explaining a step of preparing an ash according to an embodiment of the present invention.
4 is a view for explaining a step of preparing a clay powder according to an embodiment of the present invention.
5 is a view for explaining a step of manufacturing a coating agent according to an embodiment of the present invention.
6 is a view for explaining a non-combustible material including a fibrous substrate and a coating layer according to an embodiment of the present invention.
7 is a photograph for explaining the manufacturing process of the coating agent and the non-combustible material according to Experimental Examples 1 to 6.
8 is a photograph for explaining a comparison between a non-combustible material and a ceramic fabric according to Experimental Example 2.
9 is a photograph showing the flame radiation test conditions of the non-combustible material according to Experimental Examples 1 to 6.
10 is a photograph for explaining a comparison before and after the flame radiation test of the non-combustible material according to Experimental Examples 1 to 6.
FIG. 11 is a photograph for comparing states of non-combustible materials and glass fabrics according to heat treatment conditions according to Experimental Example 2. FIG.
12 is a photograph comparing a torch flame test of a non-combustible material and a glass fabric according to Experimental Example 2.
13 is a photograph of a specimen of a non-combustible material according to Experimental Examples 1 to 6 after measuring a cone calorimeter.
14 is a photograph taken after measuring a cone calorimeter of a non-combustible material according to Experimental Example 2.
15 is a photograph taken after measuring the limiting oxygen index (LOI) of a non-combustible material specimen coated with the coating agent according to Experimental Example 2 on fiber reinforced plastics (FRP).

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, the technical idea of the present invention is not limited to the embodiments described herein and may be embodied in other forms. Rather, the embodiments introduced herein are provided so that the disclosed contents may be thorough and complete, and the spirit of the present invention may be sufficiently conveyed to those skilled in the art.

In the present specification, when a component is referred to as being on another component, it means that it may be formed directly on the other component or that a third component may be interposed therebetween. In addition, in the drawings, thicknesses of films and regions are exaggerated for effective description of technical content.

In addition, in various embodiments of the present specification, terms such as first, second, and third are used to describe various elements, but these elements should not be limited by these terms. These terms are only used to distinguish one element from another element. Accordingly, what is referred to as a first component in one embodiment may be referred to as a second component in another embodiment. Each embodiment described and illustrated herein also includes its complementary embodiment. In addition, in the present specification,'and/or' has been used to mean including at least one of the elements listed before and after.

In the specification, expressions in the singular include plural expressions unless the context clearly indicates otherwise. In addition, terms such as "comprise" or "have" are intended to designate the presence of features, numbers, steps, components, or a combination thereof described in the specification, and one or more other features, numbers, steps, or configurations. It is not to be understood as excluding the possibility of the presence or addition of elements or combinations thereof. In addition, in the present specification, "connection" is used to include both indirectly connecting a plurality of constituent elements and direct connecting.

In addition, in the following description of the present invention, if it is determined that a detailed description of a related known function or configuration may unnecessarily obscure the subject matter of the present invention, the detailed description will be omitted.

1 is a flow chart for explaining a method of manufacturing a non-combustible material according to an embodiment of the present invention, FIG. 2 is a view for explaining a step of preparing a base solution according to an embodiment of the present invention, and FIG. A view for explaining the step of preparing ash according to an embodiment, Figure 4 is a view for explaining the step of preparing clay powder according to an embodiment of the present invention, Figure 5 is a coating agent according to an embodiment of the present invention It is a view for explaining the step of manufacturing a, Figure 6 is a view for explaining a non-combustible material including a fiber substrate and a coating layer according to an embodiment of the present invention.

1 to 3, an inorganic binder 110, an ash 200, and a clay powder 300 are prepared (S110).

The inorganic binder 110 may include silica, an alkali metal oxide, and water. The alkali metal oxide may include at least one of sodium (Na), potassium (K), or lithium (Li) oxide. Specifically, the inorganic binder 110 may be sodium silicate including _{silicon dioxide (SiO 2} ) and sodium oxide (Na _{2 O).} Specifically, for example, the inorganic binder 110 may include sodium silicate as shown in [Table 1] below.

Sodium silicate type characteristics product name No.1-1 (1-1) No.2-1 (No. 2-1) No.2 (casting No. 2) No.3 (KS No. 3) No.4 (No. 4) Chemical formula Na ₂ O 2 SiO ₂ H ₂ O Na ₂ O 2.6 SiO ₂ H ₂ O Na ₂ O 2.6 SiO ₂ H ₂ O Na ₂ O 3.2 SiO ₂ H ₂ O Na ₂ O 4.0 SiO ₂ H ₂ O pH 12-13 12-13 12-13 12-13 12-13 Specific gravity (20±1℃) 1.570-1.590 1.550-1.570 1.490 1.380 or higher 1.260-1.270 Na ₂ O wt% 15-16 13-14 12-13 9-10 5-6 SiO ₂ wt% 31-33 33-35 31-33 28-30 21.5-23.5 Molar ratio 2.0-2.2 2.4-2.6 2.5-2.7 3.1-3.3 3.9-4.1 Viscosity
(20±1℃) cps 1,000-2,000 1,000-2,000 Min 500 Min 100 Max 100 25L standard won 20,000 20,000 15,000 13,000 20,000

Preparing the ash 200 includes a first purification step of filtering the ash 200 with a first filter 210 to remove foreign substances, and a second filter having a higher filtering level than the first filter 210. A second purification step of separating unburned carbon by additionally filtering the ash 200 using a filter 220 may be included. For example, the first filter 210 used in the first purification step may be 200 mesh. For example, the second filter 220 used in the second purification step may be 325 mesh. Accordingly, the second filter 220 may have a higher filtering level than the first filter 210.

Preparing the clay powder 300 includes preparing a clay mineral 310, first drying the clay mineral 310, pulverizing the clay mineral 310, the clay mineral It may include a step of primary filtering (310), secondary drying of the clay mineral 310, and secondary filtering of the clay mineral (310). For example, the first drying condition of the clay mineral 310 may be 3 hours at 110°C. For example, the clay mineral 310 may be provided in a pot mill and pulverized for 24 hours. For example, the secondary drying conditions of the clay mineral 310 may be the same as the primary drying conditions.

For example, the clay powder 300 is clay, kaolin, kaolinite, bentonite, zeolite, montmolinonite, nacrite, dick It may include at least one of kite (dickite), haloysite (holloysite), or gibbsite (gibbsite).

1 and 4, a base solution 100 is prepared by providing and stirring a solvent 120 to the inorganic binder 110 (S120).

The solvent 120 provided to the inorganic binder 110 may be water. As described above, the inorganic binder 110 may contain water. Accordingly, when water is provided as a diluted solution to the inorganic binder 110, and as described later, when the ash 200 and the clay powder 300 are provided to the base solution 100, the coating agent 410 The increase in viscosity of the can be prevented. Accordingly, as will be described later, the coating agent 410 can be easily applied to the fiber substrate 500 by a spray method.

For example, the temperature of the solvent 120 may be 25 to 35°C.

For example, the stirring time of the inorganic binder 110 and the organic solvent 120 may be 10 to 20 minutes.

1 and 5, the ash 200 and the clay powder 300 are provided to the base solution 100 and stirred to prepare a coating agent 410 (S130).

According to an embodiment, while the base solution 100 is stirred, the ash 200 may be slowly provided in a small amount. In contrast, when the ash 200 is provided in a large amount in the base solution 100, the inorganic binder 110 and the ash 200 may be solidified by a chemical reaction in the base solution 100. Therefore, the ash 200 is slowly provided in a small amount to the base solution 100, so that the chemical reaction of the inorganic binder 110 and the ash 200 is minimized, and thus, it can be prevented from being easily solidified. I can. Thereafter, the clay powder 300 may be further provided and stirred to prepare the coating agent 410. In this case, as will be described later, the coating agent 410 may be easily applied to the fiber substrate 500 by spraying 3 to 4 times by a spray method.

According to an embodiment, the stirring speed of the base solution 100 may be 400 rpm to 500 rpm. In contrast, when the stirring speed of the base solution 100 exceeds 500 rpm, bubbles may be generated in the mixture of the base solution 100 and the ash 200. In this case, as will be described later, the coating agent 410 may be difficult to be easily applied to the fiber substrate 500 by a spray method.

As described above, when it is difficult to easily apply by the spray method, spray application may be possible by adjusting the nozzle size and pressure of the spray gun included in the spray.

1 and 6, by applying the coating agent 410 to the fiber substrate 500, a non-combustible material 600 is manufactured (S140).

The method of applying the coating agent 410 to the fiber substrate 500 may include at least one of spray, impregnation, dipping, a conveyor, or a brush, and the coating agent 410 is the fiber substrate 500 ) Can be coated on one side or both sides.

According to an embodiment, the coating agent 410 is sprayed 3-4 times by a spray method, applied to the fiber substrate 500, and dried naturally, so that the coating layer 400 is formed on the inside and the surface of the fiber substrate 500 Can be formed. In this case, the film quality of the coating layer 400 varies depending on the weight ratio of the inorganic binder 110, the solvent 120, the ash 200, and the clay powder 300 in the coating agent 410. I can.

Specifically, the ratio of the inorganic binder 100 is 20wt%, the ratio of the solvent 120 is more than 30wt% to less than 50wt%, the ratio of the ash 200 is more than 30wt% to less than 50wt%, the clay powder The coating agent 410 consisting of 3 wt% of 300 is spray-coated on the fiber substrate 500 and dried, so that the coating layer 400 can be easily formed with a uniform thickness. In this case, the coating layer 400 may be conformal and have excellent film quality.

When the ratio of the solvent 120 is 30 wt% or less or the ash 200 is 50 wt% or more, the viscosity of the coating agent 410 increases, and the fiber substrate 500 by spraying the coating agent 410 ) May be impossible to apply.

In contrast, when the ratio of the solvent 120 is 50 wt% or more or the ash 200 is 30 wt% or less, the viscosity of the coating agent 410 is lowered, and the coating agent 410 is sprayed. It may be possible to apply to the fibrous substrate 500. However, since the viscosity of the coating agent 410 is low, the applied coating agent 410 flows down on the fibrous substrate 500, and the film quality of the coating layer 400 may be deteriorated.

According to a modified example, before applying the coating agent 410 to the fibrous substrate 500, a pretreatment source may be first applied to the fibrous substrate 500. By the source for pretreatment, the coating agent 410 can be easily adsorbed on the fiber substrate 500, and thus, the coating layer 400 can have a uniform thickness. For example, the pretreatment source may be alcohol or water. In addition, the providing of the pretreatment source to the fiber substrate 500 may include spraying the pretreatment source in a droplet state using an ultrasonic vibrator, and the pretreatment source in the sprayed droplet state to the fiber substrate It may include the step of providing to 500. Accordingly, the source for pretreatment may be uniformly provided throughout the fiber substrate 500.

According to a modified example, heat-resistant particles are manufactured by using the ash 200 and the clay powder 300, and the coating agent 410 may further include the heat-resistant particles. Specifically, in the step of preparing the heat-resistant particles, the clay powder 300 is provided to a pot mill, and then the pot mill is rotated while spraying a primary solvent to prepare primary particles. The step of, spraying the ash 200 and a secondary solvent onto the primary particles to prepare the heat-resistant particles, and heat-treating and drying the heat-resistant particles. For example, the primary solvent may be water and the secondary solvent may be the inorganic binder 110. Accordingly, the heat-resistant particles may have the clay powder 300 core and the ash 200 shell, and the heat-resistant particles may be easily and uniformly dispersed in the coating agent 410. Due to this, the heat-resistant particles are uniformly dispersed in the coating layer 400, so that heat resistance and non-combustibility of the non-combustible material 600 may be improved.

In addition, according to a modified example, according to the above-described embodiment, only the first coating agent (the coating agent 410) and the base solution 100 and the heat-resistant particles having the ash 200 and the clay powder 300 A second coating agent may be prepared, and the second coating agent and the first coating agent may be sequentially applied to the fiber substrate 500. Accordingly, the heat-resistant particles may not be exposed on the surface of the non-combustible material 600, thereby providing the non-combustible material 600 having a smooth surface and excellent aesthetics. In other words, by applying the second coating agent first, a relatively large amount of the heat-resistant particles may be provided in the fibrous substrate 500 and a relatively small amount of the heat-resistant particles may be provided on the surface of the fibrous substrate 500.

The manufacturing method of the non-combustible material 600 according to an embodiment of the present invention, as described above, the step of preparing the inorganic binder 110, the ash 200, and the clay powder 300, the inorganic Preparing the base solution 100 by providing and stirring the solvent 120 to the binder 110, providing the ash 200 and the clay powder 300 to the base solution 100 and stirring Preparing the coating agent 410, and applying the coating agent 410 to the fibrous substrate 500 and drying to form the coating layer 400 may be included. As described above, since the manufacturing method of the non-combustible material 600 is simple, manufacturing time and manufacturing cost can be easily reduced, so that the fiber-reinforced fiber 600 can be easily mass-produced.

The structure of the non-combustible material 600 according to an embodiment of the present invention may be a structure including a coating layer 400 inside and on the surface of the fibrous substrate 500. The coating layer 400 may include the inorganic binder 100, the ash 200, and the clay powder 300. Specifically, the coating layer 400 may be formed by volatilization of the solvent 120 contained in the coating agent 410 upon natural drying after the coating agent 410 is applied to the fiber substrate 500. have. The ash 200 in the coating layer 400 may have heat resistance, non-flammability and flame retardancy at the same time. For example, the ash 200 may include alumino silicate. In addition, the clay powder 300 in the coating layer 400 may have heat resistance and flame retardancy at the same time. For example, the clay powder 300 may be kaolin powder. Therefore, the non-combustible material 600 according to an embodiment of the present invention is the ash 200 (for example, alumino silicate) and the clay powder 300 (for example, kaolin powder) in the coating layer 400 Thereby, it can have heat resistance and non-flammability at the same time. Accordingly, the non-combustible material 600 may be used for a building interior material, a thermal insulation material, a sound absorbing material, and a heat insulation material.

Hereinafter, specific experimental examples and characteristic evaluation of a non-combustible material according to an embodiment of the present invention will be described.

Manufacturing method of non-combustible material according to Experimental Example 1

Sodium silicate was prepared as an inorganic binder, ash containing alumino silicate was prepared, and kaolin powder was prepared as clay powder.

The sodium silicate was prepared with _{a weight ratio of NaO 2} of 9 wt% to 10 wt%, and a Molar ratio of 3.1 to 3.3, and the ash was filtered with a first filter (200 mesh), and then filtered with a second filter (325 mesh). The kaolin powder was first dried (110° C., 3 hours) of kaolin minerals, and then finely pulverized for 24 hours by providing the kaolin mineral to a pot mill, and then using the second filter (325 mesh). After secondary filtering, secondary drying (110° C., 3 hours) was performed, and secondary filtering was performed with the secondary filter (325 mesh).

Then, water (30wt%, 25°C to 35°C) was provided as a solvent to the sodium silicate (20wt%) and stirred for 10 to 20 minutes to prepare a base solution.

And, while stirring the base solution at 400 rpm to 500 rpm, the ash (50wt%) was slowly provided in a small amount, and then, the kaolin powder (3wt%) was provided and stirred to prepare a coating agent.

In addition, the coating agent was spray-coated on a ceramic fabric, which is a fibrous substrate, and dried naturally, to form a coating layer on the inside and on the surface of the fibrous substrate to prepare a non-combustible material.

Manufacturing method of non-combustible material according to Experimental Example 2

A non-combustible material was prepared by performing the same process as in Experimental Example 1, except that ash (40wt%) and water (40wt%) were used.

Manufacturing method of non-combustible material according to Experimental Example 3

A non-combustible material was manufactured by performing the same process as in Experimental Example 1, except that ash (30 wt%) and water (50 wt%) were used.

Manufacturing method of non-combustible material according to Experimental Example 4

Except for using sodium silicate (30wt%), water (30wt%), and ash (40wt%), a non-combustible material was manufactured by performing the same process as in Experimental Example 1.

Manufacturing method of non-combustible material according to Experimental Example 5

Except for using sodium silicate (30wt%), water (40wt%), and ash (30wt%), a non-combustible material was manufactured by performing the same process as in Experimental Example 1.

Manufacturing method of non-combustible material according to Experimental Example 6

Except for using sodium silicate (40wt%), water (30wt%), and ash (30wt%), a non-combustible material was prepared by performing the same process as in Experimental Example 1.

division Inorganic binder Solvent ash
(wt%) Clay powder Sodium silicate
(wt%) water
(wt%) Kaolin powder
(wt%) Experimental Example 1 20 30 50 3 Experiment Example 2 20 40 40 3 Experiment Example 3 20 50 30 3 Experiment Example 4 30 30 40 3 Experimental Example 5 30 40 30 3 Experimental Example 6 40 30 30 3

※ The ratio of kaolin powder is fixed at 3wt% based on the total weight of sodium silicate, water, and ash.

7 is a photograph for explaining the manufacturing process of the coating agent and the non-combustible material according to Experimental Examples 1 to 6.

Referring to Figure 7 (a), water was provided to sodium silicate and stirred to prepare a base solution, and then the base solution was stirred at 400 rpm to 500 rpm while slowly providing ash in small portions to prepare the coating agent.

Referring to (b) of FIG. 7, the coating agent was spray-coated on ceramic fabrics at a pressure of 2 bar to 4 bar, 3 to 4 times, and naturally dried to prepare the non-combustible material.

As can be seen in Figure 7, the coating agent of Experimental Examples 1 to 6, as described above, while stirring the base solution at 400rpm to 500rpm, the ash was slowly provided in small portions to prepare the coating agent.

In contrast, when a large amount of the ash is provided while stirring the base solution at 400 rpm to 500 rpm, the sodium silicate and the ash in the base solution may be solidified by a chemical reaction. Therefore, as described above, while stirring the base solution at 400rpm to 500rpm, it can be seen that slowly providing the ash in small portions is a method of easily preparing the coating agent.

Thereafter, the coating agent was spray-applied on the ceramic fabric to form a coating layer on the inside and the surface of the ceramic fabric, so that the non-combustible material was manufactured.

8 is a photograph for explaining a comparison between a non-combustible material and a ceramic fabric according to Experimental Example 2.

Referring to FIG. 8A, it can be seen that the ceramic fabric has a structure formed by intersecting ceramic fibers having a plurality of horizontal directions (180°) and ceramic fibers having a plurality of diagonal directions (45°). .

Referring to (b) of Figure 8, the non-combustible material according to Experimental Example 2, the ceramic fabric, the coating agent is uniformly applied and dried, it can be seen that it has a conformal (comformal) and excellent film quality coating layer. have.

division Inorganic binder Solvent ash Clay powder Film quality of the coating layer Sodium silicate
(wt%) water
(wt%) Alumino silicate
(wt%) Kaolin powder
(wt%) Experimental Example 1 20 30 50 3 wt% Spray application is not possible Experiment Example 2 20 40 40 3 wt% Great Experiment Example 3 20 50 30 3 wt% Bad Experiment Example 4 30 30 40 3 wt% Spray application is not possible Experimental Example 5 30 40 30 3 wt% Spray application is not possible Experimental Example 6 40 30 30 3 wt% Spray application is not possible

As can be seen from Figure 8 and [Table 3], it can be seen that the film quality of the coating layer according to Experimental Example 2 is the best. The most excellent factor of the film quality of the coating layer can be interpreted as having the most suitable viscosity in the spray coating method than the coating agent according to Experimental Example 2, Experimental Example 1, and Experimental Examples 3 to 5. Therefore, it can be seen that the coating agent is uniformly spray-applied on the ceramic fabric and dried to form the coating layer having a conformal and excellent film quality.

In contrast, in Experimental Example 1, Experimental Example 4, and Experimental Example 5, it can be seen that the viscosity of the coating agent was higher than that of Experimental Example 2, so that spray application was not possible.

In addition, the viscosity of the coating agent according to Experimental Example 3 may have the lowest viscosity because the water ratio (50wt%) is higher than that of other experimental examples. Therefore, when the coating agent is applied to the ceramic fabric, it can be seen that the coating agent flows down on the ceramic fabric to form the coating layer having a poor film quality.

9 is a photograph showing the flame radiation test conditions of non-combustible materials according to Experimental Examples 1 to 6, and FIG. 10 is a comparative description of the conditions before and after the flame radiation test of the non-combustible materials according to Experimental Examples 1 to 6 This is a photo for.

Referring to FIG. 9, it can be seen that the flame propagation test can be performed under at least one temperature condition of 649°C, 1,022°C, or 1,270°C.

Referring to (a) of FIG. 10, the non-combustible materials according to Experimental Examples 1 to 6 were each prepared by applying and drying the coating agents according to Experimental Examples 1 to 6 on a glass fabric. 10A is a photograph of a non-combustible material according to Experimental Examples 1 to 6 before the flame propagation test.

Referring to (b) of FIG. 10, (b) of FIG. 10 is a photograph of the non-combustible material according to Experimental Examples 1 to 6 after a flame propagation test.

division Torch flame propagation test result (1,270℃) Propagation distance: 1cm Propagation distance: 2cm Propagation distance: 3cm Propagation distance: 4cm Experimental Example 1 No radio waves No radio waves No radio waves No radio waves Experiment Example 2 No radio waves No radio waves No radio waves No radio waves Experiment Example 3 No radio waves No radio waves No radio waves No radio waves Experiment Example 4 No radio waves No radio waves No radio waves No radio waves Experimental Example 5 No radio waves No radio waves No radio waves No radio waves Experimental Example 6 No radio waves No radio waves No radio waves No radio waves

9, 10, and [Table 4], the non-combustible materials according to Experimental Examples 1 to 6 were subjected to a torch flame propagation test at 1,270°C.

As can be seen in FIGS. 9, 10, and [Table 4], it can be seen that the coating layer of the non-combustible material according to Experimental Examples 1 to 6 was substantially unchanged in shape before/after the torch flame propagation test. have. In addition, in the flame propagation test, it can be seen that the torch flame propagation distances of Experimental Examples 1 to 6 were all less than 1 cm. Therefore, it can be seen that the non-combustible material according to Experimental Examples 1 to 6 is a material having excellent flame retardancy, heat resistance, non-combustibility, and fire resistance.

FIG. 11 is a photograph for comparing states of non-combustible materials and glass fabrics according to heat treatment conditions according to Experimental Example 2. FIG.

Referring to FIG. 11, the non-combustible material according to Experimental Example 2 was prepared by spray coating and drying a coating agent on the glass fabric. In addition, the non-combustible material and the glass fabric were heat-treated at 600° C. for 2 hours, 700° C. for 2 hours, and 800° C. for 2 hours according to heat treatment conditions in an electric furnace.

As can be seen from FIG. 11, it can be seen that the non-combustible material and the glass fabric have substantially no change in shape after heat treatment at 600°C and 700°C.

However, the glass fabric, after heat treatment at 800 ℃, it can be confirmed that the shape shrinks. In contrast, it can be seen that the non-combustible material does not substantially shrink in shape after heat treatment at 800°C. Therefore, it can be seen that the non-combustible material is stable up to 800°C. Accordingly, accordingly, it can be seen that the non-combustible material according to Experimental Examples 1 to 6 is a material having excellent flame retardancy, heat resistance, non-flammability, and fire resistance up to 800°C.

12 is a photograph comparing a torch flame test of a non-combustible material and a glass fabric according to Experimental Example 2.

Referring to FIG. 12, the torch flame test was performed up to 1,100°C.

As can be seen in FIG. 12, it can be seen that the glass fabric is melted at 870° C. in 5 seconds, and the shape is changed. In contrast, it can be seen that the non-combustible material is not substantially melted at 1,100° C. for 37 seconds, so that the shape does not change. Therefore, the non-combustible material has excellent heat resistance and non-combustibility, and can be used as a non-combustible material for building materials.

13 is a photograph of a specimen of a non-combustible material according to Experimental Examples 1 to 6 after measuring a cone calorimeter.

Referring to Figure 13, the cone calorimeter equipment is an equipment that evaluates the fire resistance and flame retardancy of a material, when exposed to a specific heat flux condition, the maximum heat release rate (PHRR, peak heat release rate), the total heat release amount ( Total heat release (THR), smoke production (SPR), and total smoke release rate (TSP) can be measured.

In addition, the non-combustible materials according to Experimental Examples 1 to 6 were manufactured by being coated on both sides on a basalt fabric of 100mm (width) x 100mm (height) and 50mm (thickness) or less according to ISO 5660-1.

In addition, the non-combustible materials according to Experimental Examples 1 to 6 were measured for 5 minutes at 750°C temperature condition in a cone calorimeter device.

division PHRR(kW/m ² ) THR(MJ/m ² ) SPR(m ² /s) TSP(m ² ) Experimental Example 1 9.59 1.7 0 0 Experiment Example 2 8.09 1.7 0.0002 0.8 Experiment Example 3 7.47 1.6 0 0 Experiment Example 4 7.02 1.3 0 0 Experimental Example 5 8.29 1.8 0 0.1 Experimental Example 6 7.66 1.7 0 0.1

division Flame retardant performance standard Semi-incombustible material
(Level 2) KS F ISO 5660-1
(Corn calorie metric) -The total amount of heat radiated for 10 minutes after starting heating is 8mJ/m ² or less,
The maximum heat dissipation rate for 10 minutes is 200KW/m continuously for 10 seconds or more
Does not exceed.

-Cracks, holes and melting through the test strip after heating for 10 minutes
(In the case of composite materials, all core materials are melted or destroyed)
There should be no back. KS F 2271
(Gas hazard test) -The average stop time of the experimental rats should be 9 minutes or longer. Flame retardant material
(Level 3) KS F ISO 5660-1
(Corn calorie metric) -The total amount of heat radiated for 5 minutes after starting heating is 8mJ/m ² or less,
The maximum heat dissipation rate for 5 minutes is ^{200 KW/m 2 for 10 seconds or more continuously}
Does not exceed.

-Cracks, holes and melting through the test strip after heating for 5 minutes
(In the case of composite materials, all core materials are melted or destroyed)
There should be no back. KS F 2271
(Gas hazard test) -The average stopping time of the experimental rats should be 9 minutes or longer. Non-combustible material (Class 1) KS F ISO 5660-1
(Corn calorie metric) -The maximum temperature in the furnace is finalized for 20 minutes after the start of heating.
Do not increase the temperature by more than 20K (however, for 20 minutes
If equilibrium is not reached, the average temperature for the last minute is finalized.
It is called temperature.)

-The mass reduction rate should be less than 30% KS F 2271
(Gas hazard test) -The average stopping time of the experimental rats should be 9 minutes or longer.

※ 2.3.2 Ministry of Construction and Transportation Ordinance No. 476, flame retardant performance standard for interior materials of buildings

As can be seen from Figure 13, [Table 5], and [Table 6], it can be seen that the shape of the non-combustible material according to Experimental Examples 1 to 6 has substantially no change in shape after measuring a cone calorimeter. In addition, the non-combustible materials according to Experimental Examples 1 to 6 include a maximum heat release rate (PHRR, peak heat release rate), total heat release (THR), smoke generation rate (SPR, smoke production), and total smoke. It can be seen that the values of the emission rate (PHRR(kW/m ² ) are almost the same.) Therefore, it can be seen that the fire resistance and flame retardancy of the non-combustible materials according to Experimental Examples 1 to 6. In addition, the [Table] 5], the non-combustible materials of Experimental Examples 1 to 6, after heating at 750°C for 5 minutes, had a total heat dissipation of 8mJ/m ² or less, and a maximum heat dissipation rate of 10 seconds or more continuously for 5 minutes. It does not exceed 200KW/m ² , it can be confirmed that the flame retardant material is the third grade.

14 is a photograph taken after measuring a cone calorimeter of a non-combustible material according to Experimental Example 2.

Figure 14 (a) is, one-sided and double-sided coating of the coating agent according to Experimental Example 2 on a glass fabric to prepare the non-combustible material according to ISO 5660-1 standard in Figure 13, and a cone calorimeter for 10 minutes at 750 ℃ temperature It was measured.

14 (b) is a single-sided and double-sided coating of the coating agent according to Experimental Example 2 on a basalt fabric to prepare the non-combustible material according to ISO 5660-1 standard in FIG. 13, and cone calorie for 10 minutes at 750°C. The meter was measured.

division PHRR(kW/m ² ) THR(MJ/m ² ) SPR(m ² /s) TSP(m ² ) Glass fabric
(section) 4.003 1.406 0 0 Glass fabric (both sides) 1.814 0.2354 0 0 Basalt fabric (cross section) 1.953 0.417 0 0 Basalt fabric (both sides) 4.475 1.5736 0 0

14, [Table 6], and [Table 7], in the case of the non-combustible material coated on one side and both sides on the glass fabric and the non-combustible material coated on one side and both sides on the basalt fabric, the maximum heat release rate ( It can be seen that the values of PHRR, peak heat release rate), and total heat release (THR) are different.

Specifically, in the case of the non-combustible material coated on one side of the glass fabric, PHRR: 4.003 kW/m ² , THR: 1.814 MJ/m ² , and in the case of the non-combustible material coated on both sides of the glass fabric, PHRR: 1.1814 kW/m ² , THR: 0.2354 MJ/m ² , in the case of the non-combustible material coated on one side on the basalt fabric, PHRR: 1.953 kW/m ² , THR: ^{0.417 MJ/m 2} , and the non-combustible material coated on both sides on the basalt fabric In the case of, it can be seen that PHRR: 4.475 kW/m ² , THR: 1.5736 MJ/m ^2. Accordingly, it can be seen that the non-combustible material coated on both sides of the glass fabric has the lowest PHRR and THR values and has the best flame retardancy.

And, when comparing the maximum heat dissipation rate and total heat dissipation amount of the non-combustible material coated on one side of the glass fabric and the non-combustible material coated on both sides of the glass fabric, the case of double-sided coating on the glass fabric, than the case of single-sided coating, It can be seen that the maximum heat release rate and the total heat release amount are low. Accordingly, it can be seen that the non-combustible material coated on both sides of the glass fabric has more improved flame retardancy than the non-combustible material coated on one side.

In contrast, when comparing the maximum heat release rate and total heat release amount of the non-combustible material coated on one side of the basalt fabric and the non-combustible material coated on both sides of the basalt fabric, the case of single-sided coating on the basalt fabric is compared to the case of double-sided coating. , It can be seen that the maximum heat release rate and the total heat release amount are low. Accordingly, it can be seen that the non-combustible material coated on one side on the basalt fabric has improved flame retardancy more than the non-combustible material coated on both sides.

And, according to [Table 6], the non-combustible material coated on one side and both sides on the glass fabric and the non-combustible material coated on one side and both sides on the basalt fabric, after heating at 750° C. for 10 minutes, the total amount of heat emission It is 8mJ/m ² or less, and the maximum heat release rate for 10 minutes ^{does not exceed 200KW/m 2} continuously for 10 seconds or more, so it can be seen that all are semi-non-combustible materials grade 2.

Accordingly, the non-combustible material coated on one side and both sides on the glass fabric and the non-combustible material coated on one side and both sides on the basalt fabric may be used as a heat insulating material. In particular, in the case of the non-combustible material coated on one side of the glass fabric, it has the best flame retardancy and lower cost than the basalt fabric, so it can be easily commercialized.

15 is a photograph taken after measuring the limiting oxygen index (LOI) of a non-combustible material specimen coated with the coating agent according to Experimental Example 2 on fiber reinforced plastics (FRP).

Referring to FIG. 15, the limiting oxygen index (LOI) measurement is an experiment in which the oxygen concentration in the air required to burn for 3 minutes without extinguishing the fire after the specimen containing the polymer is ignited.

Referring to Figure 15 (a), the shape of the FRP before and after the measurement of the limiting oxygen index was compared.

Referring to (b) of FIG. 15, the coating agent according to Experimental Example 2 was applied to the FRP by spraying and dried to prepare the non-combustible material, and the conditions before and after the measurement of the limiting oxygen index of the non-combustible material were compared. .

Based on the Ministry of Construction and Transportation of Korea European Integration (EU) UK (BS) United States (ASTM) Germany Remark Notice No. 476 Notice No. 438 rank
LOI
standard rank
LOI
standard rank
LOI
standard rank
LOI
standard - rank LOI
standard rank LOI
standard Flame Retardant
1st grade Incombustible Separately applied A1 Incombustible Separate standard Separate standard B1 35%
More than - Flame Retardant
Level 2 Semi-incombustible A2 Semi-incombustible Flame Retardant
Level 3 42~
47% B 40%
More than Class
0 40%
More than - Risk
4 35%
More than C 32%
More than Class
One 32%
More than Class
A 32%
More than - - International architectural interior materials
Fire flame retardant grade 1 Risk
3 32%
More than Risk
2 28%
More than D 28%
More than Class
2 28%
More than Class
B 28%
More than Flame retardant grade 2 Risk 1 24%
More than E 24%
More than Class
3 24%
More than Class
C 24%
More than Self-extinguishing

As can be seen from Fig. 15 and [Table 8], as a result of measuring the limiting oxygen index of the FRP, flame reaction did not occur up to 27.4% of oxygen concentration, but it can be seen that flame reaction occurs when the oxygen concentration is 27.5% or more.

In contrast, when the coating agent according to Experimental Example 2 was spray-coated on the FRP and dried to prepare the non-combustible material, flame reactions occurred up to 25%, 30% to 40%, 50%, and 60% oxygen concentration. You can see that it was not. Therefore, it can be seen that the non-combustible material according to Experimental Example 2 has excellent flame retardancy.

As described above, the present invention has been described in detail using preferred embodiments, but the scope of the present invention is not limited to specific embodiments, and should be interpreted by the appended claims. In addition, those who have acquired ordinary knowledge in this technical field should understand that many modifications and variations are possible without departing from the scope of the present invention.

100: base solution
110: inorganic binder
120: solvent
200: ash
210: first filter
220: second filter
300: clay powder
310: clay mineral
400: coating layer
410: coating agent
500: fiber base
600: non-combustible material

Claims (9)

Preparing sodium silicate, ash, and kaolin;
Providing a solvent to the sodium silicate and stirring to prepare a base solution;
Preparing a coating agent by providing and stirring the ash and kaolin to the base solution; And
Including the step of preparing a non-combustible material by applying the coating agent to the fiber substrate,
The method of manufacturing a non-combustible material in which the content of the ash in the coating agent is more than 30 wt% and less than 50 wt%.
The method of claim 1,
Preparing the ash,
A first purification step of filtering the ash with a first filter to remove foreign substances; And
And a second purification step of separating unburned carbon by additionally filtering the ash using a second filter having a higher filtering level than the first filter.
The method of claim 1,
The step of preparing the kaolin,
Preparing kaolin minerals;
First drying the kaolin mineral;
Pulverizing the kaolin mineral;
First filtering the kaolin mineral;
Secondary drying the kaolin mineral; And
Method for producing a non-combustible material comprising the step of secondary filtering the kaolin mineral.
Fiber base;
Including a coating layer on the inside and the surface of the fiber substrate,
The coating layer includes sodium silicate, ash and kaolin,
A non-combustible material in which the content of the ash in the coating layer is more than 30 wt% and less than 50 wt%.
The method of claim 4,
The fiber substrate is a non-combustible material comprising at least one of basalt fiber, glass fiber, carbon fiber, aramid fiber, silica fiber, cotton fiber, or nylon fiber.
A building interior material comprising the non-combustible material according to claim 4, and having heat resistance and non-combustibility.
Insulating material comprising the non-combustible material according to claim 4, and having heat resistance and non-combustibility.
A sound absorbing material comprising the non-combustible material according to claim 4 and having heat resistance and non-combustibility.
Insulation material comprising the non-combustible material according to claim 4, and having heat resistance and non-combustibility.

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