KR102516574B1 - Inorganic ceramic heat shielding floor coating material and heat shielding coating method using the same - Google Patents

Abstract

The present invention is a process of obtaining a stirred material A by stirring 1) methyltrimethoxysilane 2) isopropyl alcohol, 3) tetraethoxysilane, 4) acetic acid in a stirrer; 5) colloidal silica and 6) distilled water are stirred in a separate stirrer to obtain an agitated material B; After the first addition of 1/n of the stirred material B to the stirred material A, the first stirring was performed from opaque to transparent, and 1/n of the remaining stirred material B was added repeatedly at each transparent time in turn, and the addition was completed when it reached 60 ° C. , the process of continuing only stirring and stopping when it reaches 80 ° C to obtain the stirred material C; 7) hydroxypropyl cellulose, 8) butoxyethanol part, and 9) glycidoxypropyltrimethoxysilane are sequentially stirred in the stirred material C, and the undercoat and topcoat manufacturing step to obtain the aged stirred material D as a primer and a top coat; And performing a homogenization process by mixing the inorganic material with the stirring material D to perform an intermediate manufacturing process of preparing the inorganic stirring material E as an intermediate agent, removing dust from the floor of the building and coating the primer, It is a manufacturing method and coating method of an inorganic ceramic heat-shielding waterproof floor coating that coats the top coat when the lower surface is dry to the touch.

Description

Inorganic ceramic heat shielding floor coating material and heat shielding coating method using the same}

The present invention relates to a method for preparing an inorganic ceramic heat-insulating and waterproof floor coating and a method for coating a floor using the prepared coating.

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

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

Prior art related to the manufacturing method of the inorganic binder includes Patent Publication No. 2001 - 0027894 "Silica Binder and Manufacturing Method Thereof". The prior art relates to a silica (SiO2)-based coating material with excellent adhesion capable of forming a thin film by being coated on a surface of glass, single crystal silicon, or metal, and a manufacturing method thereof, wherein Si(OC ₂ H5) ₄ or ethyl silicate is mixed with an acid aqueous solution Silica sol made by hydrolysis and polysiloxane or R ₂ Si(OR') ₂ (R is CH ₃ and R' is any one selected from H, CH ₃ and CH ₂ CH ₃ ) reacted Disclosed is a silica sol binder having a Si-CH ₃ group prepared by a method having low viscosity and excellent adhesive strength. Another prior art related to the manufacturing method of an inorganic binder is Patent Registration No. 0758286 entitled “Method for Manufacturing Inorganic Polymer Binder”. The prior art has 27 to 30 repeating units (n) of monosiloxane based on -Si-O- bonding units and disiloxane based on -Si-O-Si- bonding units ( An inorganic binder having 15 to 18 repeating units of disiloxane) is disclosed.

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

As such a method, two methods have been conventionally proposed.

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

2). Partially added catalyst to silica sol to make 1 liquid, silane as 2 liquid, mixing and stirring to react, and aging for a certain time, then adding alcohol as 3 liquid, stirring again, and aging to obtain a coating agent There is a method for making (hereinafter referred to as 'conventional method 2').

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

However, in the case of conventional method 1, after 48 hours at room temperature, the coating agent gels due to a condensation reaction, and it is impossible to work anymore, 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 preserve the liquid for a long time, and the working time, which is the use time after forming the coating agent, does not exceed 48 hours. Therefore, it has been a major obstacle in overseas exports that require long-term storage and transportation.

On the other hand, the coating agents prepared by conventional methods 1 and 2 both require preheating of the corresponding material before coating the coating agent, and there is also a problem that a high temperature drying process of 200 ° C. or more is required during the painting process.

To this end, a method for manufacturing an inorganic non-combustible ceramic binder capable of long-term preservation, which is a coating composition that extends the working time of the coating agent and overcomes the limitations of working conditions such as preheating and high-temperature drying, is disclosed in Korean Patent Publication 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 stirred while first stirring for 5 to 10 minutes. A 1-1 step of preparing a 1-1 liquid while dispersing by inputting;

Step 1-2 of preparing liquid 1-2 by adding 1.5 to 2.5% by weight of acid catalyst dropwise to liquid 1-1 and stirring for 20 to 30 minutes;

A second step of preparing a second liquid by mixing and stirring 8 to 15% by weight of distilled water with 10 to 15% by weight of colloidal silica (silica sol);

The 2 liquids are repeatedly dropped into the 1-2 liquids little by little, but if they change to white at the time of initial drop, they are stirred until they become transparent, and when they become transparent, some of the 2 liquids are dropped again and a total of 20~ A third step of reacting for 30 minutes;

Next, it is an inorganic nonflammable ceramic binder manufacturing method in which a fourth step of improving adhesion by gradually adding 0.5 to 1.5% by weight of epoxysilane is performed. However, this has the effect of extending the storage period, but the addition of isopropyl alcohol is small, so the dispersibility is low, and the stirring time is increased, which takes a lot of manufacturing time. Since the dispersibility is low, there is a problem in that the implementation of the desired function is not constant when the functional inorganic powder is added.

In addition, the floor waterproofing coating mainly uses urethane waterproofing agent as a primer and an intermediate agent, but since urethane is an organic material, it causes a fire, and after 3 years, it deteriorates and the coating layer floats and loses its waterproof function. There is a problem in that it takes at least one day to cure after coating the first and top coats, so that waterproofing takes 2 to 3 days.

The present invention is to solve this problem, and the object of the present invention is to dilute silane and stir acetic acid to stir the colloidal silica diluted stirring material B to stir the stirring material C, divide the stirring material B by stirring When it becomes transparent from the initial opaque state, it is stirred repeatedly to additionally stir another agitation material B, and the transparency is confirmed with a photograph during repeated stirring, so that even beginners can accurately stir. Manufacturing method and manufacturing of inorganic ceramic heat-shielding waterproof floor coating It is intended to provide a heat shield waterproof floor coating method using a coating agent.

Another 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 acetic acid is stirred, and the stirring material C is heated. It is intended to provide a method for manufacturing an inorganic ceramic heat-insulating waterproof floor coating that provides a primer and maintains a storage period of 6 months to 1 year, and a heat-resistant waterproof floor coating method using the prepared coating agent.

Another object of the present invention is a method for manufacturing an inorganic ceramic heat-resistant waterproof floor coating agent capable of realizing a heat-shielding waterproof function and a matte function by using the agitated water D as a floor waterproofing primer and top coater, and the agitated water E as a floor heat-shielding waterproof intermediate agent, and a coating agent prepared It is intended to provide a heat shield waterproof floor coating method using a.

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

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

3) mixing and stirring 30-40 parts by weight of tetraethoxysilane;

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

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

6) 60 parts by weight of water (H ₂ O) is stirred at a ratio of 4.3 to 5:1 to obtain a stirred substance B.

Part of the agitated substance B was divided by 1/n and added to the stirred substance A in turn, but when the initial temperature of the addition increased and became opaque and then transparent, then 1/n of the stirred substance B was added again, and the stirring temperature was 60 When it reaches ℃, only stirring is performed until it reaches 80 ℃ to obtain the stirred material C.

7) 7-15 parts by weight of hydroxypropyl cellulose to the stirred material C;

8) 10-12 parts by weight of butoxyethanol,

9) 3 to 7 parts by weight of glycidoxy propyl trimethoxy silane are sequentially added and stirred to obtain an agitation material D as a primer and a top coat; and

100 parts by weight of stirring material D as a primer and a top coat 10) 10-15 parts by weight of titanium oxide (powder),

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

12) In order to provide a method for manufacturing an inorganic ceramic heat-insulating waterproof floor coating and a floor coating method using the prepared coating agent, which performs an intermediate manufacturing process in which 5-12 parts by weight of chromium (Cr) are sequentially added and mixed to obtain inorganic agitator E as an intermediate agent. will be.

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

Effect1. 5) Separate colloidal silica and 4) acetic acid and stir separately. (Registration No. 10-0732085, conventional method 2 mixes colloidal silica with catalyst first) ---Prevents the promotion of initial self-hydrolysis reaction .

effect 2. In the process of obtaining the hydrolysis pyrogen C, since it is added sequentially based on the transparent picture, it is repeatedly added and stirred in real time without delay, so the stirring time is shortened and there is no error in the process, so even unskilled people can manufacture it.

effect 3. Since the hydrolysis exothermic stirring material C self-heats to 60-80 ℃, the thickening agent and the top coat of the stirring material D prepared using the stirring material C in the heated state increase in viscosity to form a uniform viscosity, so the stirring material D is used as a primer or top coat to induce relatively rapid volatilization of alcohol components when coating on the floor, shortening the contact time to about 1 hour.

Effect 4. In the process of manufacturing the agitated water D, it is sealed to prevent evaporation of the alcohol component and maintain the viscous state.

Effect 5. In the process of manufacturing the agitated material D, the hydrolysis reaction of the binder is completed by an exothermic process for the first 1-6 hours, and the silane component is maintained in a uniformly dispersed state by cooling and aging from the heated temperature to room temperature for the next 2 to 6 hours. Therefore, the preservability of the undercoat or topcoat itself can be preserved from 6 months to 1 year.

Effect 6. Stirred material D has good dispersibility, so the intermediate agent of the stirred material E, in which inorganic particles are added to the stirred material D, provides stable heat insulation, corrosion resistance, and water resistance, and the contact time of the intermediate agent is also shortened to about 2 hours.

effect 7; The intermediate agent, which is an inorganic agitator E, has high viscosity and water resistance, so the coating adhesion is improved, allowing the intermediate agent coating to be continued after only the touch time after the primer coating. When the setting time has elapsed, the coating can be continued after the intermediate agent, reducing the coating work time.

Effect 8. A primer and a top coat are obtained by preparing the agitated material D, and inorganic additives are added to the obtained primer to separate and manufacture each intermediate agent, so the storage period of each primer (top coat) and intermediate coat is extended, and the primer Since the touch time of the and middle coats is less than 2 hours, it is possible to coat in one day even if the touch time passes after the undercoat, then the top coat after the touch time passes, while maintaining the heat shield and waterproof function, and inorganic substances. It is composed mainly and does not rot, enabling a new concept floor coating method that extends the effect maintenance period from 3 years to 10 years.

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

Hereinafter, the present invention will be described in detail.

Glossary

＋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 [alkyl group] It is a group of atoms excluding one hydrogen from chain-shaped saturated hydrocarbons. general formula

It is marked with - and its abbreviation is R. CH3- excluding one hydrogen of methane includes methyl, ethyl C ₂ H ₅ -, propyl CH ₃ CH ₂ CH ₂ -, and butyl CH ₃ CH ₂ CH ₂ CH ₂ -.

◎TEOS

It is a compound of formula Si (OC ₂ H ₅ ) ₄ which is tetraethylorthosilicate, formally tetraethoxy silane, abbreviated TEOS. TEOS is a colorless liquid that dissolves 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 produced by alcoholysis of silicon tetrachloride.

SiCl ₄ + 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 the Si-OR bonds.

◎Glycidoxy propyl trimethoxysilane-OFS-6040

XIAMETER™ OFS-6040 Silane is a difunctional silane containing glycidoxy reactive organic groups and trimethoxy silyl inorganic groups. It is represented by γ-glycidoxy propyl trimethoxy silane. These glycidoxy functional silanes are reactive with many different types of organic polymers. OFS-6040 silane can be applied to inorganic surfaces as a dilute aqueous solution (0.1 to 0.5% silane concentration). It is recommended that the aqueous solution of OFS-6040 silane be used within 24 hours of preparation. Old solutions start to become hazy. In the case of mineral fillers, the minerals can be treated by mixing with silane at very low shear for several minutes without additional solvent. Silane can be diluted with water or solvent.

Summary of Ingredients and Additions

1) 330 to 370 parts by weight of methyltrimethoxysilane

]-[OFS-6070](다우실리콘 코퍼레이션 사 제품)(분산제)[

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

(Silane compound → alkoxysilane → methyltrimethoxysilane)

2) 330 to 370 parts by weight of isopropyl alcohol

,

]--용해 용[

,

]--for melting

[1):2)=1:1 stirring]

3) 30-40 parts by weight of tetraethoxysilane

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

]-[OFS-6697] (product of Dow Silicon Corporation) (dispersant)

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

COOH 촉매) 20중량부4) Acetic Acid (C

COOH catalyst) 20 parts by weight

In the agitation of 1), 2), 3), 4) [stirred material A] [3): 4) = 1.5 to 2: 1] there is no catalytic reaction and it can be stored as an agitated material,

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

5) 258-300 parts by weight of colloidal silica

SiO ₂ particles in a colloid state, usually called silica, and the size of the particles varies from several tens of nm to several μm. Colloidal silica is a substance in which silica particles are dispersed in a dispersed phase of water or ethanol. - Cataloid SN, Japanese Ilhui Catalyst Co., Ltd.]

6) 60 parts by weight of water (H ₂ O) --- [5): 6) = 4.3 to 5: 1 stirring-stirring material B]

The agitated substance B is divided into a certain amount and repeatedly added to the stirred substance A, but when the temperature rises and changes from initial opaque to transparent, the addition and stirring are repeated, and when the temperature reaches 60 ° C. .

to the agitator 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;

]--Delays binder drying, dissolves thickener well--

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

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

--Coupling agent and binder for various thermosetting resins and glass or minerals--

The above 7) hydroxypropyl cellulose, 8) butoxyethanol, and 9) glycidoxy propyl trimethoxy silane are sequentially added and stirred to obtain a stirred material D, which is a ceramic binder, as a primer and a top coat agent.

Stirring material 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 successively added and mixed to obtain stirring substance E as a middle agent.

Manufacture process

I. Undercoat and top coat manufacturing process (Agitator) --250~300rpm

In the agitator 1 shown in FIG. 2, a sensor 2 for detecting internal temperature is installed on the side wall, and the sensing value of the sensor 2 is converted into a digital value by an analog-to-digital converter built into the sensor 2, and the controller ( 3) is provided in a recognizable state. The controller 3 displays the recognized temperature value as a character 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 rotation of the motor M), and if necessary, the supply unit ( The supply is controlled by opening and closing the valve V1 for supplying the raw material additive supplied in 6). Opening and closing of the valve V1 may be exemplified by, for example, opening and closing by driving a solenoid to operate the valve in forward or reverse rotation, but is not limited thereto. (7) is a stirring blade. After stirring and adding, the stirrer 1 of FIG. 2 is used, and related symbols are not described individually.

FIG. 4 is an exemplary block diagram showing the control configuration of FIG. 2. The sensor 2 for recognizing the internal temperature includes a sensor unit 2-1 for recognizing ultraviolet light emitted by a temperature change in a stirring object, and a sensor unit 2 It consists of an analog-to-digital converter (2-2) that converts the recognition value of -1) into a digital value and provides it to the input terminal (I2) of the controller (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 conjunction 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 sequentially supplied by opening the valve V1 through the feeder 6 installed with the feeder for supplying additives to the stirrer 1 to be stirred. That is, 1) methyltrimethoxysilane (

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

2) 330-370 parts by weight of isopropyl alcohol- is supplied in a 1: 1 ratio for dissolving 1) methyltrimethoxysilane so that the viscosity due to alcohol is lowered. After stirring for 10 to 20 minutes by rotating the stirring blades (7) linked to the operation of the motor (M) of 5),

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

4) In the feeder (6), acetic acid 15-20 parts by weight [3): 4) is 1.5 to 2: 1 ratio] , 1) methyltrimethoxysilane + 2) isopropyl alcohol + 3) 690-780 parts by weight of the agitated tetraethoxysilane is added dropwise so that acetic acid is dispersed together to obtain 710-800 parts by weight of the stirred material A.

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

5) 260-300 parts by weight of colloidal silica (Cataloid SN, Ilhui Catalyst Co., Ltd., Japan),

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

Divide the agitated substance B (320-360 parts by weight) several times in equal amounts and slowly drop and stir into the stirred substance A (710-800 parts by weight), but when the temperature rises after the initial stirring reaction and changes from opaque to transparent, additional stirring The process of repeating the process of stirring is stirred in the same process as shown in FIG.

1) When an amount (eg 80 parts by weight) divided equally several times (eg 4 times) of the agitated material B is added to the stirred material A, colloidal silica and alkoxysilane (methyltrimethoxysilane, tetraethoxy Silane) forms bubbles in the hydrolysis reaction and changes to an opaque state due to the start of exotherm, and then changes from opaque to transparent after 3-5 minutes of stirring. And it is difficult to confirm the exact time point due to the delivery delay time for recognizing it, etc., in the present invention, the confirmation plate 8-1 shown in FIGS. After taking a picture of the verification plate 8-1 through 8), the picture taken is enlarged as shown in FIG. 5 (b), and the transparency recognition process is performed to determine whether or not the line can be identified, and the transparency is determined as shown in FIG. 6 [ Process 1 (S1)].

The transparency recognition process is a picture of the identification table (8-1) as shown in FIG. An enlargement process of doubling the horizontal and vertical bars of the identification tag photo to recognize transparency by determining whether the vertical bar is longer than the horizontal bar, as shown in FIG. 5 (b),

Transparency is determined by comparing whether the line at the corner boundary of the enlarged vertical bar and horizontal bar is straight, by comparing the enlarged pixel part (which is arbitrarily marked like a grid by the control unit 3 to recognize the location with the number of digits, which is not in the actual picture). perform a verification process,

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

2) Following step 1 (S1), a portion of the remaining stirring material B (80 parts by weight) is dropped again, bubbles are generated by hydrolysis, an exothermic reaction occurs, and after 3-5 minutes of stirring, the reaction is completed in opaque according to the reaction becomes transparent, repeating process 2 (S2) several times to determine whether or not to be transparent by taking a picture of the confirmation plate (8-1) through the camera (8) [Process 4 (S3, Up to S4)], the stirring condition is 250 to 350 rpm, the stirring time increases when it is less than 250 rpm, and the viscosity becomes too high due to gelation when it exceeds 350 rpm. In process 1 (S1), if the initial heat generation temperature (starting from room temperature 20 ℃) is 30 ℃, process 2 (S2) is 40 ℃, process 3 (S3) is 50 ℃, process 4 (S4) temperature is 60 ℃ It is regarded as rising, but based on whether it is transparent, the present invention functions to accurately determine this point in time without delay. When the temperature rises to 60 ° C., then only stirring is performed, and when the temperature reaches 80 ° C., the stirring is terminated. In the present invention, the delay time determined based on the temperature is quickly determined based on transparency to perform stirring, thereby enabling accurate and rapid stirring.

3) When the agitated substance reaches 60° C. in the stirrer, further agitation (until it reaches 80° C.) is performed to obtain a sol state, agitated substance C [Step (S5)].

To the stirred material C, 7) 7-15 parts by weight of hydroxypropyl cellulose powder (thickener) is gradually dropped, the viscosity is increased by adding the thickener, and 8) butoxyethanol Adding 10-12 parts by weight, delaying drying of stirred material C, 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.

When stirred for 2 to 6 hours in a sealed state, an exothermic reaction occurs, and when stirred for 2 to 6 hours in a second time, it matures (stops heating, the temperature cools down to room temperature) to obtain a ceramic binder, Stirred Water D, which is a heat-shielding waterproof floor coating. It is used as a primer and a top coat.

II. Inorganic powder mixing process (Homo Mixer)

Put 100 parts by weight of the remaining agitation 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 ° C)

11) 5-12 parts by weight of alumina (Al ₂ O ₃ ) (heat shielding agent, melting point 2050 ° C),

12) 5-12 parts by weight of chromium (Cr) (heat shielding agent and pigment, melting point 1907 ° C) are sequentially mixed and mixing is performed for 3-4 hours so that inorganic particles are uniformly dispersed and maintained. An intermediate agent of the inorganic agitator E is obtained. Inorganic agitator E has a high melting point of additive inorganic substances and is an inorganic powder, so when used as an intermediate agent, it becomes opaque green (chromium pigment), and it provides heat insulation due to the high melting point of inorganic substances, so that fire may occur when coated with a waterproof coating. It performs a firewall function to prevent ignition by blocking heat conduction from inside the case 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) Methyltrimethoxysilane, Dow Silicone Corporation trade name OFS-6070 420 grams, 2) Isopropyl alcohol 300 grams are mixed and stirred for 15 minutes, 3) Tetraethoxysilane, Dow Silicone Corporation trade name OFS-6697 Mix 20 grams more and stir for 15 minutes, mix 4) 20 grams of acetic acid, which is an acid catalyst, to make a mixture (1 liquid),

2. 5) 140 grams of Cataloid SN, trade name of Ilhui Catalyst Co., Ltd., Japan, which is silica sol, is mixed with 120 ml of water to make stirred water 2 (2 liquids),

3. A coating composition is prepared by mixing and stirring the 2nd liquid with the 1st liquid to function as a separate coagulant.

4. 60 g of fluoride, 50 g of zinc phosphate, and 60 g of green carbide were mixed and stirred with 1100 g of the coating composition to coat the bottom.

At the time of painting, it was painted after preheating on a sand blasted floor and dried at a temperature between 130 and 150 ° C.

As a result, the dried floor had an excellent appearance and a good gloss of 65. In addition, the adhesiveness 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 ° C.

<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, a methoxysilane, and stirred at 300 rpm first for 7 minutes while tetraethoxysilane (TEOS), trade name of Dow Corning's OFS, was stirred. -1-1st step of preparing 1-1 liquid while gradually adding 20 grams of 6697 and dispersing;

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

A second step of preparing a second liquid by mixing and stirring 120 g of distilled water with 140 g of colloidal silica (silica sol) at 300 rpm;

The 2 liquids are repeatedly dropped into the 1-2 liquids little by little, but if they change to white at the initial drop, they are stirred at 300 rpm until they become transparent. A third step of reacting for a total of 30 minutes by stirring at 300 rpm until it becomes;

Subsequently, a coating composition was prepared by performing a fourth step of gradually adding 10 grams of Dow Corning OFS-6040, an ethoxysilane, to improve adhesion,

The bottom was coated by mixing and stirring 80 g of fluoride, 80 g of zinc phosphate, and 80 g of green carbide in 1100 g of the coating composition.

It was painted after preheating on a sand blasted floor and dried at a temperature between 60 and 100 ° C.

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

Example 1

I. Undercoat and topcoat manufacturing process (agitator)

Agitation A manufacturing process

on the stirrer 1,

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

2) After stirring 330 g of isopropyl alcohol in 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 stirred material A.

Agitated material B manufacturing process in another agitator 2

5) 260g of colloidal silica (Cataloid SN, Ilhui Catalytic Chemicals Co., Ltd., Japan)

6) 60 g of water (H2O) was stirred and mixed to obtain 320 g of stirred material B.

Agitation C manufacturing process

3. Divide the stirring material B (320g) evenly (1/4) and slowly drop and stir 80g of the stirring material B to the stirring material A (710g), and check the time when the stirring condition becomes transparent from opaque through the camera (8 -1) It is added after judging by recognition. The process of adding may exemplify the state of FIG. 3 .

1) 80g of a portion (1/4) of the stirring material B is dropped into the stirring material A, and when stirred in the stirrer, the colloidal silica forming the stirring material B and the alkoxysilane (methyltrimethoxysilane, tetraethoxysilane) forming the stirring material A ) is changed to an opaque state as it starts to exotherm while generating bubbles due to the hydrolysis reaction. Stirring is 3-5 minutes, and the time when the temperature starts to heat up at room temperature (20 ℃) and becomes transparent coincides with the time when the temperature rises by 10 ℃, and the camera 8 shown in FIG. The confirmation plate 8-1 is photographed as shown in FIG. 5 (a), and the photographed photograph is recognized through the input terminal I1 of the control unit 3 through the input/output interface 9 in the memory shown in FIG. In order to determine whether a picture has the desired transparency, the picture is enlarged and the enlarged pixel portion (eg (13,21) (14,22) (22,31) (24,33) 33, 41) (34, 42) (51, 42) (53, 44) is determined whether the division line is flat If the controller 3 recognizes it as transparent, the controller 3 outputs the output to the output terminal O1. is stopped, and at this time, it is T1 time in FIG. 3 when the stirring is 30 ° C ( step 1),

2) The controller 3 stops the output to the output terminal O1, opens the valve V1 (opens it by applying a high-level signal for driving the valve), drops 80 g of the agitated substance B again, and returns to the camera. When the picture of the confirmation plate (8-1) through (8) becomes transparent, the control unit 3 regards it as the T2 time in FIG. 3 rising to 40 ° C. by hydrolysis and stops stirring ( step 2), Adding 80 g of B again until time (T3, T4 in FIG. 3) It is repeated (up to process 4 when the stirring material B is exhausted), and the stirring condition is 250 to 350 rpm, and the stirring time increases when it is less than 250 rpm, and the viscosity becomes too high due to gelation when it exceeds 350 rpm.

3) Step 4 is stopped when the temperature reaches 60 ° C (time T4 in FIG. 3) when it is transparent. Obtain stirring substance C. Of course, the temperature measurement is to recognize the recognition value through the sensor 2 in the control unit 3.

Agitation D manufacturing process

to the agitator C,

7) 7 g of hydroxypropyl cellulose powder (thickener) is slowly added and stirred for 3-5 minutes

8) Adding 10 g of butoxyethanol dropwise,

9) After adding 7g of glycidoxy propyl trimethoxy silane (XIAMETER ™ OFS-6040 silane), it is sealed, and an exothermic reaction occurs during the first 6 hours of stirring, and the second time of stirring for 6 hours, aging (cooling to room temperature) results in a ceramic binder, Agitation D is obtained for top and bottom coats.

When the agitated material D is used as a primer, dust is removed from the concrete floor forming the floor and the primer is coated. The primer of the present invention penetrates between the pores of the concrete and hardens, so the pores are blocked and waterproofness is excellent, and isopropyl alcohol Since it contains good volatility, the touch drying time is reduced from one day to 2-3 hours.

II. Inorganic powder mixing process (Homo Mixer)

Leaving the amount of the primer and the top coat in the stirring material D, put 100 g of the remaining stirring material D into the homomixer at 800-900 rpm and rotate the mixer rotor,

10) 10 g of titanium oxide (TiO ₂ ) (heat shielding agent, melting point 1843 ° C),

11) 5 g of alumina (Al ₂ O ₃ ) (heat shielding agent, melting point 2050 ° C),

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

As a result, the dried coating film was excellent in appearance and had a green opaque bottom. In addition, the adhesiveness was good because it did not exfoliate, and the pencil hardness was also good at 8H. Flexibility was average. The storage stability was 1 year, and the port life of the coating agent was 240 hours. The thermal insulation temperature was 1100°C.

Example 2

Same as Example 1, but 1) methylmethoxysilane 340g, 2) isopropyl alcohol 340g to obtain a primer, 10) titanium oxide powder 13g, 11) alumina powder 8g, 12) chromium powder 8g added Except for doing, it was manufactured in the same way to remove dust from the floor of the building and coated with an intermediate agent when drying to the touch after 2 hours had elapsed on the floor coated with the primer.

As a result, the dried coating film had an excellent appearance and was a matte green color. In addition, the adhesiveness was good because it did not exfoliate, and the pencil hardness was also good at 8H. Flexibility was average. The storage stability was 1 year, and the port life of the coating agent was 240 hours. The thermal insulation temperature was 1100°C.

Example 3

Same as Example 1, but 1) 350 g of methyl methoxysilane, 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 the addition of 12 g of chromium powder, it was prepared in the same way, dust was removed from the floor of the building, and the floor coated with the primer was coated with the intermediate agent when drying to the touch after 2 hours had elapsed.

The resulting dried coating film was excellent in appearance and was opaque and green in color. In addition, the adhesiveness was good because it did not exfoliate, and the pencil hardness was also good at 8H. Flexibility was average. The storage stability was 1 year, and the port life of the coating agent was 240 hours. The thermal insulation temperature was 1150°C.

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

In Examples 1 to 3, the primer and the middle coat are coated, and if necessary, the primer is coated with the top coat after the middle coat is dry to the touch, and the primer, the middle coat, and the top coat are coated with three layers. If the middle coat is coated after dry to touch on the surface of the transparent primer coating layer shown on the left side of FIG. 7, an opaque green layer is formed as in the center of FIG. As shown in the right picture of 7, the surface becomes transparent.

In the present invention, the primer provides a waterproof function by blocking the pores of the floor concrete floor, and the intermediate agent provides opacity and heat insulation by adding inorganic materials, so that the coating layer of the present invention blocks thermal shear in the event of a fire, so that the flames of the fire do not transfer. If you want to make the surface transparent, you can use the remaining primer on top of the middle coat and coat it again with the top coat. Since it can be done in 3 hours, the coating process of the undercoat, intermediate coat and top coat can be completed within one day, reducing the coating work time. Of course, until the complete curing time, 65 hours must pass after the coating of the middle or top coat, 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 picture of FIG.

Reference Signs List 1; Stirrer 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 the stirrer 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),
Then 3) 30-40 parts by weight of tetraethoxysilane,
4) Secondary stirring of 20 parts by weight of acetic acid at a ratio of 1.5 to 2:1 to obtain agitated material A;
In a separate stirrer 2, 5) 260 to 300 parts by weight of colloidal silica,
6) obtaining a stirred material B by stirring 60 parts by weight of distilled water;
Stirred material B is equally divided by 1/n, 1/n of stirred material B is first added to stirred material A, and then firstly stirred (the point at which opaque to transparent after stirring), and a part of the remaining stirred material B, 1/ n is repeatedly added at each transparent time in turn, and the transparent point of view is identified by adding an identification mark to the bottom of the stirrer, installing an identification camera on the stirrer lid, and identifying transparency by whether or not the border line of the identification mark is straight with a camera photograph. Finishing the addition at the point of transparency, continuing only stirring, and stopping when the temperature reached 80 ° C to obtain the stirred material C;
7) Hydroxypropyl cellulose 7-13 parts by weight in stirring substance C,
8) 10-12 parts by weight of butoxyethanol,
9) 3-7 parts by weight of glycidoxypropyltrimethoxysilane
While stirring in turn, the initial 2 to 6 hours in a sealed state is an exothermic reaction, and an additional 6 hours after the exothermic reaction is stirred to mature at room temperature to obtain a ceramic binder, the agitation D, as a primer and a top coat. and
Put 100 parts by weight of the agitated substance D remaining as the undercoat and top coat in a homomixer, and add 10) titanium oxide 10-15 parts by weight, 11) alumina 5-12 parts by weight, 12) chromium 5-12 parts by weight of inorganic powder in turn. Inorganic ceramic thermal insulation waterproof floor coating manufacturing method, characterized in that by performing a homogenization process for heat resistance and water resistance by aging in a mixing state for 3-4 hours to perform an intermediate manufacturing process of preparing inorganic agitator E as an intermediate agent.
The method of claim 1, wherein the identification mark installed on the bottom of the stirrer in the process of obtaining the agitator C is a cross, and the identification mark is made so that the length of the vertical bar is longer than the horizontal bar. Transparency recognition Inorganic ceramic thermal insulation waterproof floor coating manufacturing method, characterized in that for performing the process.
The method of claim 2, wherein the transparency recognition process is an enlargement process of doubling the horizontal and vertical bars of the identification tag photo to recognize transparency based on whether the vertical bar is longer than the horizontal bar in the identification tag photo;
Performs a confirmation process to check transparency by checking whether the line at the edge boundary of the enlarged vertical bar and horizontal bar is straight,
The confirmation process is a method of manufacturing an inorganic ceramic heat shielding waterproof floor coating, characterized in that the line of the original shooting size and the line straightness of the enlarged part are transparently confirmed when they are within the error range of 10 to 15%.
A primer coating process of removing dust from the floor of a building and coating an inorganic binder primer;
Undercoat touch-drying process of touch-drying in the air for 2-3 hours after coating with primer;
An intermediate coating process of coating a matte intermediate agent on the surface of the primer after touch drying; and
Including an intermediate touch-drying process of touch-drying in the air for 2-3 hours after intermediate agent coating;
The primer is in the stirrer 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 material A by stirring 20 parts by weight of acetic acid;
In a separate stirrer 2, 5) 260 to 300 parts by weight of colloidal silica,
6) obtaining a stirred material B by stirring 60 parts by weight of distilled water;
Stirred material B is equally divided by 1/n, 1/n of stirred material B is first added to stirred material A, and then firstly stirred (the point at which opaque to transparent after stirring), and a part of the remaining stirred material B, 1/ adding n sequentially at each transparent time, finishing the addition at the transparent time of 60 ° C., continuing only stirring and stopping when it reached 80 ° C. to obtain an agitated substance C;
7) Hydroxypropyl cellulose 7-13 parts by weight in stirring substance C,
8) 10-12 parts by weight of butoxyethanol,
9) 3-7 parts by weight of glycidoxypropyltrimethoxysilane are stirred in turn, but in a sealed state, the initial reaction is exothermic for 2 to 6 hours, and after the exothermic reaction, stirring is performed to mature at room temperature for an additional 6 hours to obtain agitated substance D Obtaining as a primer;
100 parts by weight of the agitated substance D is put into a homomixer as the intermediate agent, and 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 are sequentially added to the inorganic powder to obtain a 3- An inorganic ceramic thermal barrier waterproofing floor coating method characterized in that it is obtained by performing an intermediate manufacturing process of preparing an inorganic agitator E aged in a mixing state for 4 hours as an intermediate agent.
The method of claim 4, further performing a top coat coating process in which the undercoat is coated with the top coat again on the surface of the middle coat after the intermediate touch drying process,
A top coat to touch drying process in which the top coat is touched to touch for 2-3 hours after the top coat coating process;
Inorganic ceramic thermal insulation waterproof floor coating method, characterized in that the curing process is further performed within 65 hours after the top coat touch drying process.

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