KR20220078984A - Inorganic ceramic heat shielding floor coating material and heat shielding coating method using the same - Google Patents

Abstract

In the present invention, 1) methyltrimethoxysilane, 2) isopropyl alcohol, 3) tetraethoxysilane, 4) acetic acid is stirred in a stirrer to obtain a stirred substance A; A process of obtaining a stirred product B by stirring 5) colloidal silica and 6) distilled water in a separate stirrer; After the first addition of 1/n of the stirring material B to the stirring material A, the first stirring is performed from opaque to transparent, and 1/n of the remaining stirring material B is repeatedly added every time it becomes transparent in sequence, and when it reaches 60 degrees, the addition is finished, The process of obtaining a stirred material C by continuing only stirring and stopping when it reaches 80 degrees; 7) hydroxyppopylcellulose, 8) butoxyethanol part, and 9) glycidoxypropyltrimethoxysilane are sequentially stirred in the stirred water C, and then the aged stirred material D is prepared as a primer and a top coat as a primer and top coat; and mixing the inorganic material with the stirring material D to perform a homogenization process to prepare the inorganic stirring material E as a semi-finishing agent; A method for manufacturing and coating an inorganic ceramic heat-shielding waterproof floor coating agent for coating the top coat.

Description

Inorganic ceramic heat shielding waterproof floor coating manufacturing method and floor coating method using the prepared coating agent {Inorganic ceramic heat shielding floor coating material and heat shielding coating method using the same}

The present invention relates to a method for manufacturing an inorganic ceramic heat shielding waterproof floor coating agent and a floor coating method using the prepared coating agent.

A binder refers to a material that combines materials of different materials to provide required properties such as adhesion, coating film properties, or chemical resistance in the end use. Binders can be largely divided into organic binders and inorganic binders. Organic binders form a bond between materials by carbon bonding or ether bonding, and inorganic binders bind materials by Si-O bonding or Al-O bonding. The binder may be used for the manufacture of various materials such as paints, waterproofing agents, fibers or rubbers. On the other hand, ceramic is an inorganic non-metal that is hardened by sintering and mainly refers to a non-metal solid combined with oxygen.

A problem with organic binders widely used in various industrial fields is that they may generate volatile organic compounds (VOCs). Since volatile organic compounds can have a serious impact on the environment, regulations are being strengthened gradually. As an alternative to such organic binders, water-based binders or inorganic binders have been proposed.

As a prior art related to a method of manufacturing an inorganic binder, there is Patent Publication No. 2001-0027894 "Silica-based binder and method for manufacturing the same". The prior art relates to a silica (SiO2)-based coating material having excellent adhesion to form a thin film by being coated on the surface of glass, single crystal silicon, and metal, and a method for manufacturing the same. Si-CH3 group prepared by reacting silica sol made by decomposition with polysiloxane or R2Si(OR')2 (R is CH3 and R' is any one selected from H, CH3 and CH2CH3) Disclosed is a silica sol binder having low viscosity and excellent adhesion. As another prior art related to the method of manufacturing an inorganic binder, there is Patent Registration No. 0758286 “Method for Manufacturing Inorganic Polymer Binder”. In the prior art, 27 to 30 repeating units (n) of monosiloxane based on a bonding unit of -Si-O- and disiloxane having a -Si-O-Si- bonding unit as a basic unit ( disiloxane) is disclosed for an inorganic binder having 15 to 18 repeating units.

In general, in the field of materials that require heat resistance, such as kitchen appliances and food items, a method of preparing a coating agent by reacting silica sol and silane using a sol-gel reaction is widely used.

As such a method, two methods have been proposed in the prior art.

1). There is a method (hereinafter referred to as 'conventional method 1') of mixing and stirring silica sol, silane, alcohol, a base catalyst or an acid catalyst to form a coating agent.

2). Add a part of the catalyst to the silica sol to make 1 solution, mix the two with silane first, stir to react, and then mature for a certain period of time, then add alcohol as 3 solution, stir again, and mature to make a coating agent There is a method of making (hereinafter referred to as 'conventional method 2').

And in the case of manufacturing a colored coating agent, a coating agent is prepared by adding a pigment in the last process.

However, in the case of the conventional method 1, after 48 hours at room temperature, the coating agent gels due to a condensation reaction and can no longer work, so it is difficult to store the coating agent for a long time or transport it over a long distance. .

In addition, in the case of the conventional method 2, since the catalyst is added to the silica sol, it is difficult to store one liquid for a long time, and there is a problem that the working time, which is the use time after forming the coating agent, does not exceed 48 hours. Therefore, it has become a big obstacle in overseas exports that require long-term storage and transportation.

On the other hand, the coating agent produced by the conventional methods 1 and 2 has a problem in that both require preheating of the material before coating the coating agent, and a high temperature drying process of 200° C. or more is required during the coating process.

To this end, a method for manufacturing an inorganic non-combustible ceramic binder capable of long-term preservation, a coating composition that extends the working time of the coating agent and has non-flammability by overcoming the limitations of working conditions such as preheating and high-temperature drying, is disclosed in Korean Patent Application Laid-Open No. 10-2019-0005924 As a result, 25 to 35% by weight of isopropyl alcohol (IPA) was added to 35 to 38% by weight of methoxysilane, and 1.5 to 5% by weight of tetraethoxysilane (TEOS) was gradually added with primary stirring for 5 to 10 minutes. The 1-1 step of preparing a 1-1 solution while dispersing by input;

A first step 1-2 of preparing a solution 1-2 by adding 1.5 to 2.5 wt% of an acid catalyst to solution 1-1 and stirring for 20 to 30 minutes;

A second step of preparing a second solution by mixing and stirring 8-15 wt% of distilled water to 10-15 wt% of colloidal silica (silica sol);

Drop the 2 liquids little by little repeatedly into the 1-2 liquids, but if it turns white at the time of initial drop-off, stir until it becomes transparent, and if it turns transparent, add some 2 liquids again until it becomes transparent for a total of 20~ A third step of reacting for 30 minutes;

Then, 0.5 to 1.5% by weight of epoxy silane is gradually added to perform the fourth step of improving adhesion. However, although this has the effect of extending the storage period, the amount of isopropyl alcohol added is small, so the dispersibility is lowered, so the stirring time is increased, so it takes a lot of time to prepare. Since the dispersibility is low, there is a problem in that the desired function is not uniformly implemented when the functional inorganic powder is added.

In addition, for floor waterproofing coatings, urethane waterproofing agents are mainly used as primers and intermediates, but urethane is an organic material, which causes fire. , There is a problem in that it takes at least one day to cure the topcoat after the coating operation, so that the waterproofing operation takes 2 to 3 days.

The present invention is to solve this problem, and the object of the present invention is to stir the colloidal silica diluted stirring material B to the stirring material A in which silane is diluted and stirred with acetic acid to prepare the stirring material C, the stirring material B is divided and stirred. When it becomes transparent in the initial opacity state, it is repeatedly stirred by additionally stirring another stirring material B, and when repeated stirring, the transparency is checked with a photograph, so that even beginners can accurately stir the inorganic ceramic heat shield waterproof floor coating manufacturing method and manufacturing An object of the present invention is to provide a heat-insulating waterproof floor coating method using a single coating agent.

Another object of the present invention is that the dispersing agent is well dissolved and dispersibility is maintained by dispersing the dispersing agent added in the heated state of the stirred material C in which the colloidal silica diluted stirring material B is stirred in the stirring material A in which silane is diluted and acetic acid is stirred. An object of the present invention is to provide a method for manufacturing an inorganic ceramic heat-blocking waterproof floor coating that provides a primer, and maintains a storage period of 6 months to 1 year, and a heat-insulating waterproof floor coating method using the prepared coating agent.

Another object of the present invention is to use agitated water D as a floor waterproofing primer and top coater and agitated water E as a floor heat-shielding waterproofing intermediate agent to realize a heat-shielding waterproof function and a matte function, and a method for manufacturing an inorganic ceramic heat-blocking waterproof floor coating and a coating agent It is intended to provide a heat-insulating waterproof floor coating method using

The present invention for this purpose is 1) 330 to 370 parts by weight of methyltrimethoxysilane;

2) stirring 330 to 370 parts by weight of isopropyl alcohol in a 1:1 ratio,

3) Mix and stir 30-40 parts by weight of tetraethoxysilane,

4) Stirring 20 parts by weight of acetic acid with a catalyst to obtain a stirred product A.

5) 258-300 parts by weight of colloidal silica;

6) 60 parts by weight of water (H2O) is stirred at a ratio of 4.3 to 5; to obtain a stirred product B.

Part of the stirred material B is divided by 1/n and added to the stirred material A one by one, but as the initial temperature of addition increases, it becomes opaque and then becomes transparent, then repeats adding 1/n of the stirring material B again, and the stirring temperature is 60 When the temperature is reached, the mixture C is obtained by stirring only until it reaches 80°C.

7) 7-15 parts by weight of hydroxypropyl cellulose,

8) 10-12 parts by weight of butoxyethanol;

9) a base coat preparation process in which 3-7 parts by weight of glycidoxy propyl trimethoxy silane is sequentially added and stirred to obtain a stirred product D as a primer and a top coat; and

10) 10-15 parts by weight of titanium oxide (powder),

11) 5-12 parts by weight of alumina (Al ₂ O ³ );

12) To provide a method for manufacturing an inorganic ceramic heat-shielding waterproof floor coating that performs an intermediate manufacturing process to obtain an inorganic stirring material E as an intermediate agent by sequentially adding and mixing 5-12 parts by weight of chromium (Cr) and a floor coating method using the prepared coating agent will be.

As described above, the present invention provides various effects as follows.

Effect 1. 5) Colloidal silica and 4) acetic acid are separated and stirred separately. (Registration of similar type No. 10-0732085 Conventional method 2 mixes the catalyst with colloidal silica first)---Prevents the promotion of the initial self-hydrolysis reaction .

Effect 2. In the process of obtaining the hydrolysis pyrogen C, it is added sequentially based on the transparent photo, so it is repeatedly added and stirred in real time without a delay time.

Effect 3. Since the hydrolysis exothermic stirring material C is self-heating to 60-80°C, the primer and top coater of the stirring material D prepared using the heated stirring material C increase the thickening property to achieve a uniform viscosity, so the stirring material D When coated on the floor by using as a primer or topcoat, it induces relatively rapid volatilization of the alcohol component, thereby shortening the contact time to about 1 hour.

Effect 4. It is sealed during the manufacturing process of the stirred substance D to prevent evaporation of alcohol components and maintain the viscosity state.

Effect 5. During the first 1-6 hours of the production process of stirred material D, the hydrolysis reaction of the binder is completed as an exothermic process, and the silane component is uniformly dispersed by cooling and aging from the exothermic temperature to room temperature for the next 2 to 6 hours. Therefore, the preservation of the primer or top coat itself is possible from 6 months to 1 year.

Effect 6. Since the stirring material D has good dispersibility, the intermediate agent of the stirring material E added with inorganic particles to the stirring material D stably provides heat shielding, corrosion resistance, and water resistance, and the contact time of the intermediate agent is also shortened to about 2 hours.

effect7; Since the intermediate agent, which is an inorganic agitated material E, has high viscosity and has water resistance, the coating adhesion is improved, and it is possible to continue coating the intermediate agent after only a touch time after coating with the primer. When the touch time has elapsed, the intermediate agent can be continuously coated, thereby shortening the coating time.

Effect 8. A primer and a topcoat are obtained by manufacturing agitated material D, and an inorganic additive is added to the obtained primer to separate and manufacture the intermediate agents, so the storage period of each primer (topcoat) and intermediate agent is extended, and the primer Since the contact time of the primer and the intermediate agent is less than 2 hours, it is possible to coat the primer in one day even after the touch time has passed and then the top coater is coated after the touch time has passed. It is mainly composed of a new concept of floor coating method that is not rotten and the duration of the effect is extended from 3 years to 10 years.

1 is a process diagram of the present invention;
2 is a block diagram of the stirrer of the present invention;
3 is a waveform diagram showing the time of addition of the stirred material to obtain the stirred material C of the present invention;
4 is a control configuration diagram of FIG. 2;
5 is an enlarged photograph of the main part of the confirmation plate of the present invention and a photograph thereof;
6 is a control flow diagram of the present invention;
7 is a photograph of a coating according to an embodiment of the present invention.

Hereinafter, the present invention will be described in detail.

Glossary of terms

＋2

◎Silane compound--

+2

(--R, R'가 알킬기[

－]이고, n=1~3이면 알킬알콕시실란(alkylalkoxysilane))◎Alkoxysilane (organoalkoxysilane)--

(--R, R' is an alkyl group [

-], and if n = 1 to 3, alkylalkoxysilane

=RO-, 메톡시(

), 에톡시(

)◎Alkoxy group

=RO-, methoxy (

), ethoxy (

)

－로 표시되며 약호는 R이다. 메테인(methane)의 수소 1개를 제외한 CH3-는 메틸(methyl), 에틸 C2H5-, 프로필 CH3CH2CH2-, 부틸 CH3CH2CH2CH2－이 있다.◎alkyl group It is the remaining atomic group except for one hydrogen in chain-shaped saturated hydrocarbons. general meal

It is marked with - and the abbreviation is R. Except for one hydrogen in methane, CH3- is methyl, ethyl C2H5-, propyl CH3CH2CH2-, butyl CH3CH2CH2CH2-.

◎TEOS

It is a compound of the formula Si (OC2H5)4, which is tetraethylorthosilicate, officially tetraethoxy silane, abbreviated as TEOS. TEOS is a colorless liquid that decomposes in water. TEOS is the ethyl ester of orthosilicic acid, Si(OH)4. It is the most common alkoxide of silicon.

TEOS is a tetrahedral molecule and is prepared by alcoholysis of silicon tetrachloride.

SiCl4 + 4 EtOH → Si (OEt) 4 + 4 HCl

Here, Et is an ethyl group, C2H5, so EtOH is ethanol.

TEOS is used in the production of airgels. These applications exploit the reactivity of Si-OR bonds.

◎Glycidoxy propyl trimethoxysilane-OFS-6040

XIAMETER™ OFS-6040 Silane is a bifunctional silane containing a glycidoxy reactive organic group and a trimethoxysilyl inorganic group. Represented by γ-glycidoxy propyl trimethoxy silane. This glycidoxy functional silane is reactive with many different types of organic polymers. OFS-6040 silane can be applied to inorganic surfaces as a diluted aqueous solution (0.1-0.5% silane concentration). It is recommended that the aqueous solution of OFS-6040 silane be used within 24 hours of preparation. The old solution will start to become cloudy. In the case of mineral fillers, minerals can be treated by mixing with silane at very low shear for several minutes without additional solvents. Silanes can be diluted with water or solvents.

Summary of ingredients and addition amount

1) 330 to 370 parts by weight of methyltrimethoxysilane

]-[OFS-6070](다우실리콘 코퍼레이션 사 제품)(분산제)[

]-[OFS-6070] (Dow Silicon Corporation) (dispersant)

(silane compound → alkoxysilane → methyltrimethoxysilane)

2) 330 to 370 parts by weight of isopropyl alcohol

,

]--용해 용[

,

]--For dissolving

[1);2)=1; stirring in a ratio of 1]

3) 30-40 parts by weight of tetraethoxysilane

]-[OFS-6697](다우실리콘 코퍼레이션 사 제품)(분산제)[TEOS; Tetraethoxysilane; Si

]-[OFS-6697] (Dow Silicon Corporation) (Dispersant)

1) Methyltrimethoxysilane + 2) isopropyl alcohol mixed with 3) tetraethoxysilane mixed and stirred to 1) improve dispersibility of methyltrimethoxysilane to give caking properties

COOH 촉매) 20중량부4) Acetic Acid (C)

COOH catalyst) 20 parts by weight

There is no catalytic reaction in the stirring of 1), 2), 3), and 4) [stirred material A] [3); 4) = 1.5 to 2; 1;

--4) Acetic acid catalyst promotes reaction only with 5) colloidal silica + 6) water stirring.

5) 258-300 parts by weight of colloidal silica

Colloidal SiO2 particles, usually called silica, vary in size from several tens of nm to several μm, and colloidal silica is a material in which silica particles are dispersed in a dispersed phase of water or ethanol. Japanese Catalyst Cataloid SN]

6) 60 parts by weight of water (H2O)---[5);6)=4.3~5;1 stirring-stirred material B]

Divide the stirred material B into a certain amount and repeatedly add it to the stirred material A, but when the temperature changes from initially opaque to transparent as the temperature rises, the addition and stirring are repeated. .

to the stirrer C,

7-15중량부,7) Hydroxypropylcellulose

7-15 parts by weight,

[HPC; hydroxypropyl cellulose; Cellulose 2-hydroxypropyl ether]-Ceramic thickener-

8) 10-12 parts by weight of butoxyethanol;

]--바인더 건조지연, 증점제를 잘 녹여준다--[Butoxyethanol;

]--Binder drying delay, thickening agent well--

9) 3-7 parts by weight of glycidoxy propyl trimethoxy silane;

[Glycidoxy propyl tri methoxy silane] (XIAMETER ™ OFS-6040 Silane)

--Coupling agents and binders for various thermosetting resins and glass or minerals--

7) hydroxypropyl cellulose, 8) butoxyethanol, and 9) glycidoxy propyl trimethoxy silane are sequentially added and stirred to obtain a ceramic binder, stirred substance D, as a primer and a top coater.

Stirring D 100 parts by weight,

10) 10-15 parts by weight of titanium oxide (TiO ₂ ) powder;

11) 5-12 parts by weight of alumina (Al ₂ O ₃ );

12) 5-12 parts by weight of chromium (Cr);

are sequentially added and mixed to obtain a stirred substance E as a medium.

Manufacture process

I. Undercoating agent and topcoating agent manufacturing process (agitator; Agitator) --250~300rpm

The stirrer 1 shown in FIG. 2 is provided with a sensor 2 for detecting the internal temperature on the side wall, and the sensed value of the sensor 2 is converted into a digital value by an analog-to-digital converter built into the sensor 2, and the control unit ( 3) is provided in a recognizable state. The control unit 3 displays the recognized temperature value in characters on the display 4 so that a third party can check it from the outside. The output terminal O1 of the control unit 3 commands the rotation of the motor unit 5 (of course, the motor driving unit 5-1 shown in Fig. 4 is used for controlling the motor M rotation), and, if necessary, a feeder ( The supply is controlled by opening and closing the valve (V1) for supplying the raw material additive supplied in 6). The opening and closing of the valve V1 may be exemplified by, for example, driving a solenoid to operate the valve in forward or reverse rotation to open and close, but is not limited thereto. (7) is a stirring blade. After stirring and addition, the stirrer 1 of FIG. 2 is used, and the related symbols are not described one by one.

4 is an exemplary view showing the control configuration of FIG. 2 in a block diagram, the sensor for internal temperature recognition 2 is a sensor unit 2-1 for recognizing ultraviolet rays emitted by a change in temperature from a stirred object, and a sensor unit 2 It consists of an analog-to-digital converter 2-2 that converts the recognized value of -1) into a digital value and provides it to the input terminal I2 of the control unit 3 . The motor unit 5 includes a motor driving unit 5-1 connected to the output terminal O1 of the control unit 3 and a motor M rotating in association with the motor driving unit 5-1.

)분말[OFS-6070](다우실리콘 코퍼레이션 사 제품) 330-370중량부에,During stirring, the following materials 1), 2), 3), and 4) are supplied by opening the valve (V1) sequentially through a feeder (6) equipped with a feeder (6) for supplying additives to the stirrer (1), thereby stirring. That is, 1) methyltrimethoxysilane (

) powder [OFS-6070] (made by Dow Silicon Corporation) 330-370 parts by weight,

2) 330-370 parts by weight of isopropyl alcohol- 1) for dissolution of methyltrimethoxysilane in a 1:1 ratio, so that the viscosity due to alcohol is lowered, the control unit 3 moves from the stirrer 1 to the motor unit ( 5) After 10-20 minutes of stirring by rotating the stirring blade (7) linked to the motor (M) operation,

3) 30-40 parts by weight of tetraethoxysilane ([TEOS; Tetraethoxysilane]-[OFS-6697] (Dow Silicon Corporation) (dispersant)) is further supplied from the feeder 6, stirred for 10 to 15 minutes, 1 ), TEOS works to improve dispersibility and impart uniform caking properties in a state where the viscosity is lowered.

4) Then, in the feeder (6), 15-20 parts by weight of Acetic Acid [3); 4) 1.5 to 2; 1 ratio] , 1) methyltrimethoxysilane + 2) isopropyl alcohol + 3) The tetraethoxysilane is added dropwise to 690-780 parts by weight of a stirred substance to disperse acetic acid together to obtain 710-800 parts by weight of a stirred substance A.

In a separate stirrer (which has the same control configuration in FIGS. 2 and 4),

5) 260-300 parts by weight of colloidal silica (Cataloid SN of Illwhi Catalyst Hwaseong, Japan);

6) 60 parts by weight of water (H2O) is stirred and mixed to obtain 320-360 parts by weight of agitated water B.

Stirred water B (320-360 parts by weight) is divided several times in equal amounts, and slowly dropped and stirred into stirred material A (710-800 parts by weight), but after the initial stirring reaction, when the temperature changes from opaque to transparent, additional stirring Agitation for each process of repeating the process is stirred in the same manner as in FIG. 6 .

1) When the amount (for example, 80 parts by weight) divided by the same number of times (for example, 4 times) of the stirring material B is added to the stirring material A, colloidal silica and alkoxysilane (methyltrimethoxysilane, tetraethoxysilane) ) changes to an opaque state due to the onset of exothermicity while generating bubbles due to the hydrolysis reaction, and then turns from opaque to transparent after 3 to 5 minutes of stirring. It is difficult to check the exact timing due to the delay time of recognizing this, etc., so in the present invention, the confirmation plate 8-1 shown in FIGS. After taking a photo of the confirmation plate 8-1 through ), the photo taken is enlarged as shown in FIG. 1(S1)].

The transparency recognition process is the identification table (8-1) picture as in Fig. 5 (a) (numbers in the picture indicate that the control unit 3 arbitrarily adds to the location like a grid, and is not a number in the photographed picture) The enlargement process of magnifying the horizontal bar and vertical bar of the identification tag photo twice as shown in FIG. 5(b) to recognize the transparency by whether the vertical bar is longer than this horizontal bar,

Transparency is obtained by comparing the enlarged pixel part (the control unit 3 is randomly marked like a grid to recognize the position with a cross-digit number, which is not in the actual photo) to determine whether the line at the border of the edge of the enlarged vertical bar and horizontal bar is straight. to carry out the verification process,

In the verification process, the control unit 3 confirmed that it was transparent when the border line of the identification table 8-1 of the original shooting size and the line straightness of the enlarged part were within the error range of 10 to 15%, and exceeded 15%. If it is, it is a case that the transparency is still less, and if it is less than 10%, there is no difference in the transparency.

2) Following step 1 (S1), a part of the remaining stirring material B (80 parts by weight) is dropped again, bubbles are generated due to hydrolysis, an exothermic reaction occurs, and after 3 to 5 minutes of stirring, the reaction is completed in opacity according to the reaction The process 2 (S2) of judging whether or not to be made transparent with a photo taken of the confirmation plate 8-1 through the camera 8 is repeated several times [Process 4 (S3, when the stirring material B is exhausted) S4)], stirring conditions are 250 to 350 rpm, when less than 250 rpm, the stirring time increases, and when it exceeds 350 rpm, the viscosity becomes too high due to gelation. In process 1 (S1), if the initial (starting at 20 ° C.) exothermic temperature is 30 ° C, process 2 (S2) is 40 ° C, process 3 (S3) is 50 ° C, and process 4 (S4) is 60 ° C. is considered to rise, but based on the transparency, the present invention functions to accurately determine this time point without a delay time. When the temperature rises to 60°C, only stirring is performed thereafter, and when the temperature reaches 80°C, stirring is terminated. In the present invention, by quickly determining the delay time determined based on the temperature based on the transparency and performing the stirring, accurate and rapid stirring is possible.

3) When the stirred material reaches 60°C in the stirrer, additional stirring (until it reaches 80°C) is performed to obtain a sol state, stirred material C [Step (S5)].

7) Slowly dropping 7-15 parts by weight of hydroxypropylcellulose powder (thickener) to the stirring water C, increasing the viscosity by adding a thickener, 8) butoxyethanol 10-12 parts by weight is added dropwise, delaying drying of the stirring material C, and dissolving the thickener (HPC) well to induce uniform dispersion, 9) Glycidoxy propyl trimethoxy silane (XIAMETER ™ OFS-6040 Silane) It maintains the dispersed state by adding 3 to 7 parts by weight.

In a sealed state, an exothermic reaction occurs when the first is stirred for 2 to 6 hours, and the second is aged (stopped heat, cooled to room temperature) during stirring for 2 to 6 hours to obtain agitated material D, a ceramic binder, which is a heat-shielding waterproof floor coating agent. Used as a primer and top coat.

II. Inorganic powder mixing process (Homo Mixer)

In the stirring material D, leave the primer and top coat, and put 100 parts by weight of the stirring material in the homomixer at 800 to 900 rpm, while rotating the mixer rotor.

10) Titanium oxide (TiO ₂ )] 10-15 parts by weight (heat-shielding agent, melting point 1843 ℃)

11) Alumina (Al ₂ O ₃ ) 5-12 parts by weight (heat-shielding agent, melting point 2050 ℃),

12) Mixing and aging process in which 5-12 parts by weight of chromium (Cr) (heat shielding agent and colorant, melting point 1907℃) are mixed sequentially and mixing is performed for 3 to 4 hours so that the inorganic particles are uniformly dispersed and maintained Obtain an intermediate agent for Inorganic Stirring E. Inorganic stirrer E has a high melting point of added inorganic substances and is an inorganic powder, so when used as an intermediate agent, it takes on an opaque green color (chromium pigment). In the case, it acts as a firewall to prevent fire by blocking heat conduction from the inside to the outside of the floor and from the outside to the inside of the floor.

Hereinafter, Examples and Comparative Examples of the present invention will be described.

<Comparative Example 1>

1. 1) Dow Silicon Corporation, which is methyltrimethoxysilane, is mixed with 420 grams of OFS-6070, 2) 300 grams of isopropyl alcohol is mixed and stirred for 15 minutes, 3) tetraethoxysilane, brand name of Dow Silicon Corporation, OFS-6697 20 grams more were mixed and stirred for 15 minutes, and 20 grams of acid catalyst 4) acetic acid was mixed to make a stirred product (1 solution),

2. 5) Mix 140 grams of Cataloid SN, a trade name of Japan Ilhwi Catalyst, which is a silica sol, 6) in 120 ml of water to make a stirred mixture 2 (2 liquids),

3. A coating composition is prepared by mixing and stirring the two liquids with one liquid to function as a separate coagulant.

4. 1100 g of the coating composition was mixed with 60 g of fluoride, 50 g of zinc phosphate, and 60 g of green carbite and coated on the floor.

During painting, the sand blast (sand blast) treated floor was preheated and then painted and dried at a temperature between 130 and 150°C.

As a result, the dried floor had an excellent appearance and had a good gloss of 65. In addition, the adhesion was good because it did not peel off from the bottom, and the pencil hardness was also good at 8H. The flexibility was moderate, the storage stability was 1 year, and the port life of the coating was 168 hours. The heat resistance temperature was 900℃

<Comparative Example 2>

In Comparative Example 2, 300 grams of isopropyl alcohol (IPA) was added to 380 grams of Dow Corning's trade name OFS-6060, which is methoxysilane, and stirred at 300 rpm for 7 minutes first, while tetraethoxysilane (TEOS), a trade name of Dow Corning's trade name OFS, was added. -Step 1-1 to prepare a 1-1 solution while slowly adding and dispersing 20 grams of -6697;

A first 1-2 step of preparing a 1-2 solution by dropping 20 grams of acetic acid as an acid catalyst to the 1-1 solution and stirring at 300 rpm for 20 to 30 minutes;

A second step of mixing and stirring 120 g of distilled water to 140 g of colloidal silica (silica sol) at 300 rpm to prepare a second solution;

The 2 liquids are repeatedly dropped into the 1-2 liquids little by little, but when the initial drop turns white, the mixture is stirred at 300 rpm and stirred until it becomes transparent. a third step of reacting for a total of 30 minutes in a manner of stirring at 300 rpm until the

Then, 10 grams of Dow Corning's OFS-6040, which is ethoxysilane, is slowly added to perform the fourth step of improving adhesion to prepare a coating composition,

The floor was coated by mixing and stirring 80 g of fluoride, 80 g of zinc phosphate, and 80 g of green carbite to 1100 g of the coating composition.

After preheating on the sand blast-treated floor, it was painted and dried at a temperature between 60 and 100 °C.

As a result, the dried floor had an excellent appearance and had a good glossiness of 57. And the adhesion was good because it did not peel off, and the pencil hardness was also good at 8H. Flexibility was mediocre. The storage stability was 1 year, and the port life of the coating was 168 hours. The heat resistance temperature was 900°C.

Example 1

I. Undercoat and top coat manufacturing process (agitator)

Agitated material A manufacturing process

on agitator 1,

1) Methyltrimethoxysilane [OFS-6070] (manufactured by Dow Silicon Corporation) powder in 330g

2) After stirring 330 g of isopropyl alcohol------------ with a stirrer for 10 to 20 minutes,

3) Add 30 g of tetraethoxysilane ([OFS-6697] (manufactured by Dow Silicon Corporation)) and stir for 10 to 15 minutes,

4) 20 g of acetic acid was added dropwise to obtain 710 g of a stirred substance A.

Agitated material B manufacturing process in another stirrer 2

5) To 260 g of colloidal silica (Cataloid SN, Cataloid SN, Inc., Ihwi Catalyst, Japan)

6) 60 g of water (H 2 O) was stirred and mixed to obtain 320 g of a stirred product B.

Stirred material C manufacturing process

3. Stirred water B (320g) is evenly divided (1/4), and 80g of stirred material B is slowly dropped and stirred into stirred water A (710g), and the stirring condition is from opaque to transparent. -1) Judging by recognition, it is added. The addition process may illustrate the state of FIG. 3 .

1) 80 g of a part (1/4) of the stirred material B is dropped on the stirring material A and stirred with a stirrer, colloidal silica forming the stirred material B and alkoxysilane forming the stirring material A (methyltrimethoxysilane, tetraethoxysilane ), it changes to an opaque state as bubbles are generated by the hydrolysis reaction, and heat is started. Stirring is 3-5 minutes, and the time from starting to exotherm at room temperature (20 ° C) and turning from opaque to transparent coincides with the time the temperature rises by 10 ° C. The confirmation plate 8-1 is taken as shown in Fig. 5 (a), and the photographed picture is recognized through the input terminal I1 of the control unit 3 through the input/output interface 9 in the memory shown in Fig. 4, In order to determine whether the recognized photo has the desired transparency, enlarge the photo as shown in FIG. (33,41) (34,42) (51,42) (53,44) was determined whether the dividing line is flat or not. When the control unit 3 recognizes that it is transparent, the control unit 3 controls the output terminal O1. Stop the output to the furnace, and at this time, it is the T1 time of FIG. 3 when the stirring material is 30 ℃ ( process 1),

2) The control unit 3 stops the output to the output terminal O1, opens the valve V1 (apply a level signal under the valve driving to open it), and then drops 80 g of the stirring material B again, and then the camera again When the picture of the confirmation plate (8-1) through (8) becomes transparent, the control unit (3) regards it as the T2 time of FIG. 3, which is raised to 40 °C by hydrolysis, and stops stirring ( process 2), and then the stirred material Until the time (T3, T4 in FIG. 3) to add 80 g of B again Repeat (up to process 4 in which the agitated material B is consumed), stirring conditions are 250-350 rpm, when less than 250 rpm, the stirring time increases, and when it exceeds 350 rpm, the viscosity becomes too high due to gelation.

3) Process 4 is stopped when it is transparent corresponding to the time point when the temperature becomes 60°C (time T4 in FIG. 3), and after process 4, additional stirring for 10-20 minutes (stop stirring when it reaches 80°C) Agitation C is obtained. Of course, temperature measurement is to recognize a value recognized by the sensor 2 in the control unit 3 .

Stirred material D manufacturing process

to the stirrer C,

7) Slowly drop 7g of hydroxypropylcellulose powder (thickener) and stir for 3-5 minutes

8) 10 g of butoxyethanol is added dropwise,

9) After adding 7 g of glycidoxy propyl trimethoxy silane (XIAMETER ™ OFS-6040 Silane), seal and exothermic reaction during the first 6 hours of stirring, and aging (cooling to room temperature) during the second 6 hours of stirring, stirring material D, a ceramic binder is obtained for use as top coats and base coats.

When agitated material D is used as a primer, the primer of the present invention hardens while penetrating between the pores of the concrete forming the floor, so it blocks pores and has excellent waterproofness. reduced to 1 hour.

II. Inorganic powder mixing process (Homo Mixer)

Leave the amount of primer and top coat in the stirred material D, and put 100 g of the remaining stirring material D into a homomixer at 800 to 900 rpm while rotating the mixer rotor,

10) Titanium oxide (TiO ₂ ) 10g (heat-shielding agent, melting point 1843℃),

11) Alumina (Al ₂ O ₃ ) 5g (heat-shielding agent, melting point 2050℃),

12) Inorganic stirrer E in the mixing and aging process in which 5g of chromium (heat shielding agent and pigment, melting point 1907℃) is mixed sequentially and mixing is performed for 3 to 4 hours so that the inorganic particles are uniformly dispersed and maintained. After coating with the primer, it was coated on the floor after drying to the touch.

As a result, the dried coating film had an excellent appearance and the floor became green and opaque. And the adhesion was good because it did not peel off, and the pencil hardness was also good at 8H. Flexibility was mediocre. The storage stability was 1 year, and the port life of the coating was 240 hours. The heat shielding temperature was 1100 °C.

Example 2

Same as Example 1, except that 1) methyl methoxysilane 340 g, 2) a primer was obtained including 340 g of isopropyl alcohol, and 10) titanium oxide powder 13 g, 11) alumina powder 8 g, 12) chromium powder 8 g was added. Except for the above, it was prepared in the same manner and coated with a primer when drying to the touch after 1 hour had passed on the floor coated with the primer.

As a result, the dried coating film had an excellent appearance and was a matte green color. And the adhesion was good because it did not peel off, and the pencil hardness was also good at 8H. Flexibility was mediocre. The storage stability was 1 year, and the port life of the coating was 240 hours. The heat shielding temperature was 1100 °C.

Example 3

Same as Example 1 except that 1) 350 g of methylmethoxysilane, 2) 350 g of isopropyl alcohol, 3) 40 g of tetraethoxysilane to obtain a primer, 10) 15 g of titanium oxide powder, 11) 12 g of alumina powder , 12) Except for adding 12 g of chromium powder, it was prepared in the same manner and coated with a primer when 1 hour had elapsed on the undercoat-coated floor to dry to the touch.

As a result, the dried coating film had an excellent appearance and was opaque and green. And the adhesion was good because it did not peel off, and the pencil hardness was also good at 8H. Flexibility was mediocre. The storage stability was 1 year, and the port life of the coating was 240 hours. The heat shielding temperature was 1150 °C.

In Examples 1 to 3, compared to Comparative Examples 1 and 2, the usage time was extended, and the heat shielding temperature was increased. This is because the dispersibility of the silane is increased by adjusting the content ratio, and inorganic powder that improves the heat resistance temperature in a homogenized state in which the viscosity is increased by adding HPC, butoxyethanol and glycidoxypropyltrimethoxysilane is added. considered to be improved.

In Examples 1 to 3, a primer and a primer are coated, and if necessary, after the intermediate agent is dry to the touch and then the primer is coated with a topcoat, it is coated with three layers of a primer, an intermediate agent and a topcoat. When the intermediate agent is coated after drying the surface of the transparent primer coating layer shown in the left side of FIG. 7, an opaque green layer is formed as shown in the center of FIG. The surface becomes transparent like the picture on the right of Figure 7.

According to the present invention, the primer provides a waterproof function by blocking the pores of the concrete floor, and the intermediate agent provides opacity and heat shielding properties by adding inorganic substances. If you want to make the surface transparent, you can use the primer remaining on the middle coat to coat it again with the top coat. Since it can be done in 2 hours, the coating process can be completed in one day with the coating process of the primer, intermediate agent and top coater, thereby reducing the coating time. Of course, 65 hours must pass after coating with an intermediate or top coat until the complete curing time, which is due to the curing time of silane. Of course, waterproofness can be confirmed by maintaining the surface tension state on the surface without water droplets penetrating as shown in the lower middle photo of FIG. 7 .

1; Agitator 2; Sensor 2-1; Sensor unit 2-2; Analog-to-digital converter 3; Control unit 4; Display 5; Motor unit M; Motor 5-1; Motor drive unit 6; Feeder 7; Stirring blade 8; Camera 8- 1; Identification table 9; I/O interface V1; Supply valve

Claims (5)

on agitator 1,
1) 330-370 parts by weight of methyltrimethoxysilane,
2) 330-370 parts by weight of isopropyl alcohol,
was first stirred at the same weight ratio (1; 1),
3) 30-40 parts by weight of tetraethoxysilane,
4) the process of obtaining a stirred product A by second stirring 20 parts by weight of acetic acid in a ratio of 1.5 to 2;
5) 260-300 parts by weight of colloidal silica,
6) a process of obtaining a stirred product B by stirring 60 parts by weight of distilled water;
The stirred material B is equally divided by 1/n, 1/n of the stirred material B is added to the stirred material A, and the first stirring is performed (the point of time from being opaque to transparent after stirring), and 1/ which is a part of the remaining stirring material B n is repeatedly added at each transparent time in turn, and for transparent time identification, an identification tag is added to the bottom of the stirrer, an identification camera is installed on the top of the stirrer, and the transparency is identified by whether the identification tag border line comes out straight from the camera photograph, and the transparency becomes 60 degrees The process of obtaining a stirred material C by completing the addition at this point, and by continuing only stirring and stopping when it reaches 80 degrees;
7) 7-13 parts by weight of hydroxyppophyll cellulose in stirred water C,
8) 10-12 parts by weight of butoxyethanol;
9) 3-7 parts by weight of glycidoxypropyltrimethoxysilane
A base coat manufacturing process in which stirring is performed in a sealed state for an exothermic reaction for the initial 2 to 6 hours and aging at room temperature for an additional 6 hours after the exothermic reaction to obtain a stirred material D, which is a ceramic binder, as a primer and a top coat; and
Put 100 parts by weight of the stirring material D left behind as the primer and top coater in a homomixer, 10) 10-15 parts by weight of titanium oxide, 11) 5-12 parts by weight of alumina, and 12) 5-12 parts by weight of chromium A method for manufacturing an inorganic ceramic heat shield waterproofing floor coating, characterized in that the intermediate manufacturing process is performed to produce an inorganic agitator E as a middle agent by performing a homogenization process for heat resistance and moisture resistance by aging in a mixed state for 3-4 hours.
The transparency of claim 1, wherein the identification tag installed on the bottom of the stirrer in the process of obtaining the stirring material C is a cross, and the identification tag is made so that the vertical bar length is longer than the horizontal bar. A method for manufacturing an inorganic ceramic heat-shielding waterproof floor coating, characterized in that recognition is performed by performing a recognition process.
According to claim 2, wherein the transparency recognition process is an enlargement process of enlarging the horizontal bar and the vertical bar of the identification tag photo twice to recognize the transparency based on whether the vertical bar is longer than the horizontal bar of the identification tag photo;
A confirmation process is performed to check the transparency by whether the line at the boundary of the edge of the enlarged vertical bar and horizontal bar is straight,
The verification process is a method of manufacturing an inorganic ceramic heat shielding waterproof floor coating, characterized in that it is confirmed as transparent when the straightness of the line of the original size and the line straightness of the enlarged part is within an error range of 10 to 15%.
Undercoat coating process of removing dust from the floor of the building and coating the base coat, which is an inorganic binder;
Undercoat drying process to touch and dry in the air for 1-2 hours after coating with a primer;
An intermediate coating process of coating a matte intermediate agent on the surface of the primer after drying to the touch; and
It includes a middle-to-touch drying process of drying to the touch for 2-3 hours in the atmosphere after coating with a middle agent;
The primer is in agitator 1,
1) 330-370 parts by weight of methyltrimethoxysilane,
2) 330-370 parts by weight of isopropyl alcohol,
3) 30-40 parts by weight of tetraethoxysilane,
4) A process of obtaining a stirred product A by stirring 20 parts by weight of acetic acid;
5) 260-300 parts by weight of colloidal silica,
6) a process of obtaining a stirred product B by stirring 60 parts by weight of distilled water;
The stirred material B is equally divided by 1/n, 1/n of the stirred material B is added to the stirred material A, and the first stirring is performed (the point of time from being opaque to transparent after stirring), and 1/ which is a part of the remaining stirring material B The process of obtaining a stirred material C by repeatedly adding n in sequence at each transparent time, completing the addition at the transparent time point of 60 degrees, and stopping only when stirring is reached at 80 degrees;
7) 7-13 parts by weight of hydroxyppophyll cellulose in stirred water C,
8) 10-12 parts by weight of butoxyethanol;
9) Stir 3-7 parts by weight of glycidoxypropyltrimethoxysilane in sequence, but in a sealed state, stirring was performed to cause an exothermic reaction for the initial 2 to 6 hours and aging at room temperature for an additional 6 hours after the exothermic reaction to obtain the stirred substance D obtained as a primer;
The intermediate agent is put in a homomixer with 100 parts by weight of the stirred substance D, 10) 10-15 parts by weight of titanium oxide, 11) 5-12 parts by weight of alumina, 12) 5-12 parts by weight of chromium inorganic powder is sequentially added to 3- Inorganic ceramic heat-shielding waterproof floor coating method, characterized in that it is obtained by performing an intermediate manufacturing process of preparing an inorganic agitated material E aged in a mixing state for 4 hours as a medium.
5. The method according to claim 4, further performing a top coat coating process of coating the primer surface with a top coat agent on the surface of the intermediate agent again after the middle touch drying process,
Topcoat drying process to touch, in which the topcoat is dried to the touch for 1-2 hours after the topcoat coating process;
Inorganic ceramic heat-shielding waterproof floor coating method, characterized in that the curing process is further performed within 65 hours after the topcoat touch drying process.

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