KR102016877B1 - Flame-retardant epoxy sealing agent and manufacturing method of the same - Google Patents

Abstract

The present invention relates to a non-flammable epoxy sealing agent and a production method thereof and, more specifically, to a non-flammable epoxy sealing agent comprising: an epoxy resin; an activated carbon; paraffin chloride; phosphoric acid; limestone; titanium oxide; a leveling agent; and a dispersant. When reinforcing a structure using the non-combustible epoxy sealing agent of the present invention, it is possible to prevent the propagation of fire along the structure when the fire occurs.

Description

Non-flammable epoxy sealing agent and its manufacturing method {FLAME-RETARDANT EPOXY SEALING AGENT AND MANUFACTURING METHOD OF THE SAME}

The present invention relates to a nonflammable epoxy sealing agent and a method for producing the same, and more particularly to a nonflammable epoxy sealing agent including an epoxy resin, activated carbon, paraffin chloride, phosphoric acid, limestone, titanium oxide, a leveling agent and a dispersant.

Structures such as reinforced concrete will deteriorate due to various causes as time passes after completion, and measures such as repair or reinforcement should be made at an appropriate time to restore the durability of the structure. Repair and reinforcement are essential to increase the service life of the structure and to ensure the safety as a structure. Accurate structural strength must be assessed and appropriate repair and reinforcement methods must be selected accordingly.

In the past, steel plate adhesion reinforcement has been the mainstream for repairing and reinforcing structures. However, due to the inconvenience of handling and poor corrosion and fire resistance, recently, carbon fiber, glass fiber, aramid fiber, etc. The fiber-attached method and the panel-attached method for attaching the FRP panel with an adhesive have been widely used.

However, when these reinforcements are applied directly to the surface of the structure with an adhesive, the reinforcement may be easily separated or separated from the structure due to defects or bends in the surface of the structure. Therefore, it is necessary to fill the sealing portion in the indented portion of the structure surface in order to flatten the structure surface before applying the reinforcement to the structure surface.

Epoxy resin is mainly used as a material of such a sealing agent, but a general epoxy resin may have a low heat resistance or flame retardancy, so that a sealing agent may be a medium of fire propagation when a fire occurs. In particular, when a material such as bromine or phenol is used, the sealing agent component present in the concrete interface in the event of fire may cause toxic gases, leading to enormous personal injury.

Accordingly, some heat resistant or flame retardant sealing agents have been developed, but in order to impart flame retardance to epoxy resins, a mixture of inorganic fillers such as halogen-based inorganic materials, antimony trioxide, and aluminum hydroxide is used. These materials can impart flame retardancy in the event of a fire, but have the problem of generating another toxic gas that is deadly to humans.

In addition, this method can express the effect only when the content of the inorganic filler is high, there is a limit that the adhesive strength of the epoxy sealing agent is lowered as the amount of the inorganic filler increases.

Republic of Korea Patent Registration No. 10-1944463

The present invention is to solve the above problems by making the surface of the structure flat to improve the adhesion strength between the structure and the reinforcement, while having heat resistance and flame retardant has an epoxy resin sealing agent that can prevent fire propagation and minimize the emission of toxic gas in the event of a fire It aims to provide.

In order to achieve the above object, the present invention provides a non-combustible epoxy sealing agent comprising an epoxy resin, activated carbon, paraffin chloride, phosphoric acid, limestone, titanium oxide, leveling agent and dispersant.

Component content of the non-combustible epoxy sealing agent is 20-30% by weight epoxy resin, 3-8% by weight activated carbon, 3-8% by weight paraffin chloride, 2-5% by weight phosphoric acid, 55-65% by weight limestone, titanium oxide 1 It is preferable that they are -3 weight%, a leveling agent 0.1-2 weight%, and a dispersing agent 0.1-2 weight%.

At this time, the epoxy resin is preferably bisphenol A diglycidyl ether (Bisphenol A diglycidyl ether), the phosphoric acid is used with a phosphorus-containing organic flame retardant, the mixing ratio of phosphoric acid and phosphorus-containing flame retardant is 1 ~ 2: 1. It is preferable that it is (w / w).

On the other hand, the present invention, in order to achieve the above object, after mixing the epoxy resin, activated carbon, paraffin chloride, phosphoric acid and limestone, the first high-speed stirring step of stirring the mixture solution at 8 to 12 ℃ for 1 to 2 hours, After adding titanium oxide to the mixed solution, a second high-speed stirring step of rapidly stirring at 15 to 20 ℃ for 1 to 2 hours, and after adding a leveling agent and a dispersant to the mixed solution to which the titanium oxide is added, 13 to 17 It provides a method for producing a nonflammable epoxy sealing agent comprising a low speed stirring step of low temperature stirring for 1 to 2 hours.

Epoxy sealing agent according to the present invention is to solve the problems due to the low heat resistance and flame retardancy of the general epoxy sealing agent, when the reinforcement of the structure using the non-flammable epoxy sealing agent of the present invention, when a fire occurs along the structure The propagation can be prevented.

In addition, the non-flammable epoxy sealing agent according to the present invention, unlike the conventional flame retardant sealant does not emit toxic gas from the adhesive component in the fire and does not lower the adhesive strength.

Specifically, epoxy resins generally used are mediators of fire propagation, which greatly increases the fires in buildings and cause not only human damage, but also harmful components used in buildings, which can cause air pollution. In addition, the combustion of the building can be controlled to have an effect of preventing human injury and air pollution.

Hereinafter, the present invention will be described in detail with reference to embodiments and drawings of the present invention. These examples are only presented by way of example only to more specifically describe the present invention, it will be apparent to those skilled in the art that the scope of the present invention is not limited by these examples. .

Also, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and in the case of conflict, the specification including definitions The description of will prevail.

In the drawings, parts irrelevant to the description are omitted to clearly describe the proposed invention, and like reference numerals designate like parts throughout the specification. In addition, when a part "contains" a certain component, this means that the component may further include other components, without excluding other components, unless specifically stated otherwise. In addition, the "unit" described in the specification means one unit or block that performs a specific function.

In each step, an identification code (first, second, etc.) is used for convenience of description, and the identification code does not describe the order of each step, and each step does not explicitly describe a specific order in context. It may be carried out in a different order than described above. That is, each step may be performed in the same order as specified, may be performed substantially simultaneously, or may be performed in the reverse order.

Non-flammable epoxy sealing agent of the present invention 20-30% by weight epoxy resin, 3-8% by weight activated carbon, 3-8% by weight paraffin chloride, 2-5% by weight phosphoric acid, 55-65% by weight limestone, titanium oxide 1-3 It is characterized by comprising a weight%, 0.1 to 2% by weight leveling agent and 0.1 to 2% by weight dispersant. Look at each configuration in detail below.

The epoxy resin is a compound having two or more epoxy groups in a molecule, bisphenol A type epoxy resin, bisphenol F type epoxy resin, bisphenol S type epoxy resin, novolac type epoxy resin and the like may be used, but other components It is preferable to use bisphenol A diglycidyl ether in consideration of compatibility and adhesive strength with each other.

It is preferable that the content of the epoxy resin is 20 to 30% by weight, and if less than this, the adhesive strength may be lowered. If the content of the epoxy resin is greater than this, the content of other functional components may be reduced, so that it is difficult to have a sufficient nonflammable effect.

The chlorinated paraffin and phosphoric acid play a role of imparting plasticity and nonflammability to the resin, and when used together, the effect can be further maximized. In particular, phosphoric acid can accelerate decomposition of carbohydrates in fibers or panels into water and carbon at high temperatures.

The content of the chlorinated paraffins and phosphoric acid is preferably 3 to 8% by weight and 2 to 5% by weight, respectively, if less than this, the plasticity and non-combustible effect may be lowered, and if it exceeds, the adhesion may be reduced.

On the other hand, the phosphoric acid may be used alone, but may be used in combination with a phosphorus-containing organic flame retardant in order to increase the compatibility and workability with other components, and to increase the plasticity and non-combustible effect. At this time, the mixing ratio of phosphoric acid and phosphorus-containing flame retardant is preferably about 1-2: 1 (w / w). The phosphorus-containing organic flame retardant may be used a variety of phosphorus-containing flame retardant on the market, preferably tris (2,6-dimethylphenyl) phosphine, tetrakis- (2,6-xylyl) resorcinol bisphosphate, tetra Phenyl resorcinol diphosphate, triphenyl phosphate, phosphazene flame retardant, 10- (2,5-dihydroxyphenyl) -10-hydro-9-oxa-10-phosphaphenanthrene-10-oxide, 10- ( 2,5-dihydroxynaphthyl) -10-hydro-9-oxa-10-phosphaphenanthrene-10-oxide or 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10- Any one or at least two mixtures selected from oxide flame retardants can be used.

The activated carbon serves to increase the rigidity of the resin and prevent cracking, the content of which is preferably 3 to 8% by weight. If less than this, the functional effect of the activated carbon may be lowered, and if exceeded, the overall adhesive strength of the resin may be lowered.

In this case, in order to increase miscibility with other components and increase incombustibility, the activated carbon may be a zinc-activated carbon composite. The zinc-activated carbon composite is obtained by dispersing an organometallic coupling agent and activated carbon in an aqueous medium, adding zinc chloride or zinc iodide to the dispersion, followed by drying to obtain a zinc / coupling agent / activated carbon composite, and then drying the dried composite. It can be obtained by baking.

At this time, the activated carbon is preferably used by surface oxidation modification, for example, 1) dry oxidation method of contacting the oxidant gas such as water vapor, carbon dioxide, oxygen and ozone with activated carbon at a high temperature, and 2) activated carbon and oxidant There is wet oxidation in which reagent solutions react (eg hydrogen peroxide, nitric acid, sulfuric acid, etc.). In addition, there are electrochemical oxidation, ozone treatment, annealing, microwave cooling plasma heat treatment, and the like.

의 화학식을 가지는 커플링제가 사용될 수 있으며, 상기 식에서, RO는 가수분해기 또는 기질 반응성기로, 상기 R은 탄소수 2 내지 10개이고, 상기 Z는 알루미늄, 실리콘, 티타늄, 아연 및 지르코늄으로 구성된 군에서 선택되는 1종 이상의 원소이며, 상기 R'는 지방족, 나프텐계 또는 방향족의 열가소성 작용기로서, 탄소수 10 내지 40을 가지고, Y는 비닐, 알릴, 아크릴 또는 메타크릴의 열반응성 또는 열경화성 관능기이며, n은 1 내지 3의 정수이다. 상기 유기금속계 커플링제의 사용량은 특별히 한정되지 않지만, 활성탄 중량을 기준으로, 0.1~5중량%의 양으로 사용될 수 있다. The organometallic coupling agent

A coupling agent having a chemical formula of A may be used, wherein RO is a hydrolyzable or substrate reactive group, wherein R is 2 to 10 carbon atoms, and Z is selected from the group consisting of aluminum, silicon, titanium, zinc and zirconium. At least one element, wherein R 'is an aliphatic, naphthenic or aromatic thermoplastic functional group having 10 to 40 carbon atoms, Y is a thermally reactive or thermosetting functional group of vinyl, allyl, acrylic or methacryl, and n is 1 to 1 Is an integer of 3. The amount of the organometallic coupling agent used is not particularly limited, but may be used in an amount of 0.1 to 5% by weight based on the weight of activated carbon.

The use conditions and reaction conditions such as the addition temperature, the addition method, the addition rate, and the stirring rate of the organometallic coupling agent are not particularly limited, and may be determined based on the ordinary knowledge and level of those skilled in the art.

The limestone (limestone) serves as a filler, the content is preferably 55 to 65% by weight, if less than this may reduce the strength and workability, if it exceeds the content of other functional components is reduced It is difficult to have sufficient incombustibility and adhesion.

The titanium oxide serves to maximize the nonflammable effect by the melting point, the content is preferably 2 to 5% by weight. If less than this, the non-combustible effect may be lowered, and if exceeded, the overall adhesive strength of the resin may be lowered.

The leveling agent is a smoothing additive that improves the fluidity of the resin, and serves to prevent defects on the surface of the resin during the drying process and deterioration of adhesive strength with the reinforcing material. It is preferable that the content of the leveling agent is 0.1 to 2% by weight, and if it is less than this, the effect of improving fluidity may be lowered. If the content of the leveling agent is exceeded, the content of other functional components of the resin may be lowered, resulting in a decrease in overall physical properties.

The leveling agent may be used a variety of leveling agents, such as silicone, fluorine-based, but considering the miscibility and smoothing effect with other components in the resin, it is preferable to use a polyether modified silicone, more preferably the following formula ( It is preferable to use the polyether modified silicone of I).

(I)

(I)

In said formula, R <3>, R <4> and R <5> are respectively independently a C1-C5 alkyl group, a C1-C5 alkoxy group, or a C2-C5 alkoxyalkyl group, an acetoxy group, a carboxyl group, and R2 is an alkylene , Preferably it is ethylene, R1 is a hydrogen atom or a C1-C5 alkyl group, n1 and n2 are the numbers of 0-10 each independently, m is a number of 2-30;

As the dispersant, various commercially available dispersants may be used, and the content thereof is preferably 0.1 to 2 wt%. If less than this, the dispersing effect may be lowered, and if it exceeds this, the content of other functional components of the resin may be lowered, resulting in a decrease in overall physical properties.

On the other hand, the sealing agent of the present invention may further comprise 0.1 to 2% by weight of a silica compound of formula (II) in order to increase the overall adhesive strength of the resin that can be reduced by the functional-containing materials. The silica compound serves to reinforce the adhesive strength and durability of the sealing agent, if less than the content may decrease the adhesive force synergistic effect, if it exceeds the content of other functional components of the resin is lowered overall physical properties will appear Can be.

(II)

(II)

In Formula (II), X represents a nano-sized silica compound produced by a sol-gel reaction of an alkoxysilane compound, Z is a mercapto group, an amino group, an alcohol group, Ra, b is an aliphatic alkyl group having 2 to 18 carbon atoms, C4-C15 alicyclic alkyl group and C6-C15 aromatic alkyl group are shown, for example, butylene, hexamethylene, octamethylene, isophorone, cyclohexylene, phenylene, naphthalene, diphenylmethyl, etc. are shown. Rc represents a C1-C5 linear or pulverized alkyl group, and examples thereof include methyl, propyl, isopropyl, and the like, wherein n is an integer of 1 to 10.

The material can be prepared as follows. First, an alkoxysilane containing a compound having a non-covalent electron pair such as a mercapto group, an amino group, an alcohol group, an epoxy group, and a diisocyanate are reacted at a reaction temperature of normal temperature to 80 ° C to prepare a silane compound containing a terminal isocyanate group. Subsequently, an epoxy compound containing a hydroxy group is continuously added thereto, and the temperature is raised to 50 to 100 ° C. and stirred until all of the isocyanates react for 1 to 5 hours to prepare an alkoxysilane compound containing an epoxy group.

Thereafter, a silane compound including three or more alkoxy groups is used in combination with the alkoxy silane complex at the end of the epoxy group, water is added thereto, and then 0.1 M HCl aqueous solution is added as a catalyst to adjust the pH to 5, followed by hydrolysis by stirring at room temperature for one day. Through the condensation process, the silica compound of Formula (II) may be prepared. In this case, instead of the silane compound containing three or more alkoxy groups, nano silica sol, for example, MEK-ST (nano silica dispersed in methyl ethyl ketone, Nissan Chemical Industries, Ltd), etc., may be used. It can be used after removing water and solvent with a molecular sieve.

On the other hand, the non-combustible epoxy sealing agent of the present invention i) a first high speed stirring step of mixing the epoxy resin, activated carbon, paraffin chloride, phosphoric acid and limestone, and then stirring the mixture solution at 8 to 12 ℃ for 1 to 2 hours, ii) adding a titanium oxide to the mixture, followed by a second high-speed stirring step of rapidly stirring at 15 to 20 ° C. for 1 to 2 hours, and iii) adding a leveling agent and a dispersant to the mixed solution to which the titanium oxide is added. It can be prepared through a low speed stirring step of stirring at low speed for 1 to 2 hours at 13 ~ 17 ℃.

Description of each of the components is as described above, when the silica compound is added, it may be added together in step i).

Hereinafter, look at the examples and experimental examples of the present invention. However, the scope of the present invention is not limited to the following preferred embodiments, and those skilled in the art can implement various modified forms of the contents described herein within the scope of the present invention.

Comparative Example 1

25 g of bisphenol A diglycidyl ether, 5 g of activated carbon, 5 g of paraffin chloride and 60 g of limestone were mixed, followed by high speed stirring at 10 ° C. for 1 hour at RPM 2000. Thereafter, after adding 2 g of titanium oxide to the mixture, stirring at high speed with RPM 2000 for 1 hour at 18 ° C., and then adding 1 g of polyether-modified silicone leveling agent and 1 g of dispersant, and then at 15 ° C. for 1 hour Epoxy sealing agent was prepared by stirring at a low speed of 1000 rpm.

Comparative Example 2

25 g of bisphenol A diglycidyl ether, 5 g of activated carbon, 5 g of paraffin chloride and 60 g of limestone were mixed, followed by high speed stirring at 10 ° C. for 1 hour at RPM 2000. Thereafter, 1 g of the polyether-modified silicone leveling agent and 1 g of the dispersant were added to the mixed solution, followed by low-speed stirring at 15 ° C. for 1 hour at RPM 1000 to prepare an epoxy sealing agent.

<Example 1>

25 g of bisphenol A diglycidyl ether, 5 g of activated carbon, 5 g of paraffin chloride, 3 g of phosphoric acid, and 60 g of limestone were mixed, followed by high speed stirring at 10 ° C. for 1 hour at RPM 2000. Thereafter, after adding 2 g of titanium oxide to the mixture, the mixture was stirred at 18 ° C. for 1 hour at high speed with RPM 2000, and then 1 g of polyether-modified silicone leveling agent and 1 g of dispersant were added thereto, and then, at 15 ° C. for 1 hour. Epoxy sealing agent was prepared by stirring at a low speed of 1000 rpm.

<Example 2>

25 g of bisphenol A diglycidyl ether, 5 g of activated carbon, 5 g of paraffin chloride, 2 g of phosphoric acid, 2 g of tris (2,6-dimethylphenyl) phosphine and 60 g of limestone were mixed, followed by high speed stirring at RPM 2000 for 1 hour at 10 ° C. It was. Thereafter, after adding 2 g of titanium oxide to the mixture, the mixture was stirred at 18 ° C. for 1 hour at high speed with RPM 2000, and then 1 g of polyether-modified silicone leveling agent and 1 g of dispersant were added thereto, and then, at 15 ° C. for 1 hour. Epoxy sealing agent was prepared by stirring at a low speed of 1000 rpm.

<Example 3>

25 g of bisphenol A diglycidyl ether, 5 g of zinc-activated carbon composite, 5 g of paraffin chloride, 60 g of limestone and 3 g of phosphoric acid were mixed, followed by high speed stirring at 10 ° C. for 1 hour at RPM 2000. Thereafter, after adding 2 g of titanium oxide to the mixture, the mixture was stirred at 18 ° C. for 1 hour at high speed with RPM 2000, and then 1 g of polyether-modified silicone leveling agent and 1 g of dispersant were added thereto, and then, at 15 ° C. for 1 hour. Epoxy sealing agent was prepared by stirring at a low speed of 1000 rpm.

<Example 4>

25 g of bisphenol A diglycidyl ether, 5 g of activated carbon, 5 g of paraffin chloride, 3 g of phosphoric acid, 60 g of limestone, and 1 g of a silica compound were mixed, followed by high speed stirring at 10 ° C. for 1 hour at RPM 2000. Thereafter, after adding 2 g of titanium oxide to the mixture, the mixture was stirred at 18 ° C. for 1 hour at high speed with RPM 2000, and then 1 g of polyether-modified silicone leveling agent and 1 g of dispersant were added thereto, and then, at 15 ° C. for 1 hour. Epoxy sealing agent was prepared by stirring at a low speed of 1000 rpm.

The silica compound was reacted with 22 g of 3-aminopropyltrimethoxysilane, 25 g of methylene diphenyl diisocyanate (MDI) and 50 g of butylglycidyl ether at room temperature for 2 hours to prepare an isocyanate-terminated silane compound. 9 g of glycidol (glycidol), which is an epoxy compound containing a hydroxy group, was continuously added and reacted at 80 ° C. for 1 hour to prepare a silane alkoxide compound including an epoxy group. Then, 100 g of MEK-ST (nano silica dispersed in methyl ethyl ketone) and 15 g of water were added, and then 0.1 M HCl aqueous solution was added as a catalyst to adjust the pH to 5, and then stirred at room temperature for one day to hydrolyze and condense. Through the process to prepare a silica compound.

Experimental Example

1 Adhesion Test

Tensile shear bond strength test was conducted according to KSM3705. The tester used a breaking load within 15 to 85% of the tester volume, and the loading speed was set to 500 kgf {491 kN} or less per minute. The maximum load (kgf) N until the test piece broke was measured and divided by the shear area (cm 2) to obtain the adhesive strength (kgf / cm 2) N / cm 2.

2 hardness

The coating film was formed so that thickness might be set to 3 mm on the glass plate, and it measured using the Shere-D hardness meter.

3 flame retardant test

∪L-94 combustion test was conducted in accordance with KSM3015. The test was conducted in a non-ventilated area, and Burner's flame was a blue light with no yellow chip and the height was adjusted to 3/4 inch. The adjusted flame was infiltrated to the test piece (length 5 inches, width 0.5 inch, thickness 0.5 inch) for 10 seconds, and after flame dyeing, the combustion of the test piece was observed. The presence of toxic gas (smoke) was visually confirmed by the toxic gas from the flame retardant test. The results are shown in Table 1 below.

Test Items Comparative Example 1 Comparative Example 2 Example 1 Example 2 Example 3 Example 4 Adhesion test 280kgf / cm ² 280kgf / cm ² 230kgf / cm ² 250kgf / cm ² 260kgf / cm ² 280kgf / cm ² Longitude (Share-D) 73 75 70 73 75 75 Flame retardant (V = 0) x x V = 0 V = 0 V = 0 V = 0 Toxic smoke O O x x x x

(Note: V = 0 1. Flaming within 10 seconds after infestation, 2. Flaming does not occur within 50 seconds in total after influx 10 times in a set of 5 sheets. 3. No flaming or growing until clamps. Do not drop the fire to ignite the line.

As can be seen in the table, the non-flammable epoxy sealing agent of the present invention is excellent in adhesiveness, hardness and non-flammability, and does not come out of toxic gas can be utilized in various ways, such as reinforcing the structure.

The present invention is not limited to the above specific embodiments and descriptions, and various modifications can be made by those skilled in the art without departing from the gist of the invention as claimed in the claims. Such variations are within the protection scope of the present invention.

Claims (5)

20-30% by weight epoxy resin, 3-8% by weight activated carbon, 3-8% by weight paraffin chloride, 2-5% by weight phosphoric acid, 55-65% by weight limestone, 1-3% by weight titanium oxide, 0.1-2 leveling agent Wt% and 0.1-2 wt% dispersant,
The epoxy resin is bisphenol A diglycidyl ether, the phosphoric acid is used together with a phosphorus-containing organic flame retardant, the mixing ratio of phosphoric acid and phosphorus-containing flame retardant is 1 ~ 2: 1 (w / w) ego,
The activated carbon is a zinc-activated carbon composite. The zinc-activated carbon composite is an organometallic coupling agent and activated carbon dispersed in an aqueous medium, and zinc chloride or zinc iodide is added to the dispersion of the coupling agent and the activated carbon, followed by drying. After obtaining a ring agent / activated carbon composite, it is prepared by calcining the dried composite,
The organometallic coupling agent

A coupling agent having a chemical formula of wherein RO is a C 2-10 hydrolyzable group, Z is at least one element selected from the group consisting of aluminum, silicon, titanium, zinc and zirconium, and R ' An aliphatic, naphthenic or aromatic thermoplastic functional group having 10 to 40 carbon atoms, Y is a thermally reactive or thermosetting functional group of vinyl, allyl, acrylic or methacryl, n is an integer of 1 to 3, and the organometallic coupling agent is activated carbon Nonflammable epoxy sealing agent, characterized in that used by 0.1 to 5% by weight based on the weight. delete delete delete 20 to 30% by weight of epoxy resin, 3 to 8% by weight of activated carbon, 3 to 8% by weight of paraffin chloride, 2 to 5% by weight of phosphoric acid and 55 to 65% by weight of limestone were prepared to prepare a mixture, and then the mixture was 8 to 8%. A first high speed stirring step of rapidly stirring at 12 ° C. for 1 to 2 hours; A second high speed stirring step of adding titanium oxide to the mixed solution and then stirring the mixture at high speed for 15 hours at 1 ° C. to 20 ° C .; And a low speed stirring step of adding a leveling agent and a dispersant to the mixed solution to which the titanium oxide is added, and then stirring at a low speed at 13 to 17 ° C. for 1 to 2 hours.
The activated carbon is a zinc-activated carbon composite, and the zinc-activated carbon composite includes dispersing an organometallic coupling agent and activated carbon in an aqueous medium; Adding zinc chloride or zinc iodide to the dispersion of the coupling agent and activated carbon and then drying to obtain a zinc / coupling agent / activated carbon composite; And firing the dried composite;
The organometallic coupling agent

A coupling agent having a chemical formula of wherein RO is a C 2-10 hydrolyzable group, Z is at least one element selected from the group consisting of aluminum, silicon, titanium, zinc and zirconium, and R ' An aliphatic, naphthenic or aromatic thermoplastic functional group having 10 to 40 carbon atoms, Y is a thermally reactive or thermosetting functional group of vinyl, allyl, acrylic or methacryl, n is an integer of 1 to 3, and the organometallic coupling agent is activated carbon A method for producing a nonflammable epoxy sealing agent, characterized in that 0.1 to 5% by weight based on weight.