KR20170078934A

KR20170078934A - Sealant composition for fireproofing materials and the manufacturing method thereof

Info

Publication number: KR20170078934A
Application number: KR1020150188435A
Authority: KR
Inventors: 이승윤
Original assignee: (주)탑프라
Priority date: 2015-12-29
Filing date: 2015-12-29
Publication date: 2017-07-10
Also published as: KR102039767B1

Abstract

The present invention relates to a sealant composition for a fireproof material and a method of manufacturing the same. More particularly, the present invention provides a fireproof material having improved fire resistance by adding expanded graphite, which has not been applied to a conventional sealant composition for a fireproof material, The present invention relates to a novel sealant composition for a fireproof material and a manufacturing method for manufacturing the sealant composition with high quality.

Description

FIELD OF THE INVENTION [0001] The present invention relates to a sealant composition for fireproofing materials,

Almost all interior and exterior building materials used in everyday life require flame retardancy and fire resistance.

As construction materials for interior and exterior, the most widely used materials for interior and exterior materials for sound absorption, insulation, fireproofing and condensation prevention are fibrous materials such as glass surface, rock surface, ceramic fiber and cellulose, synthetic wood using wood powder, Composite building materials and so on. The panels used as prefabricated building materials include EPS, urethane, MDF, glasswool, concrete PC, and ALC panel.

However, the interior and exterior materials of the above-mentioned building materials have various problems such as environmental pollution, vulnerability to fire, generation of toxic gas by combustion.

In order to solve such a problem, a composition of a solvent capable of blocking the generation of toxic gas against the vulnerability of fire occurrence and combustibility has been developed, but its effectiveness is still a problem. Particularly, Performance, and smoke generation index, but can be easily manufactured and molded, so that there is no commercialized composition for a fire retardant that can be applied to various fires.

Particularly, in the case of a sealant composition used as a sealing material when various building materials and interior materials are applied, fire resistance and flame retardancy are required, and a sealing effect against toxic gas and heat due to sealing is required.

However, the conventional sealant composition is expected to have a certain degree of fire resistance, but the problem of deterioration of toxic gas or fire shielding effect due to the modification of the sealant due to heat and the maintenance of complete sealing state is not maintained.

Especially, it is used in various buildings to maintain the waterproofness and airtightness of joints and gaps in buildings, and thus plays an important role in preventing the shortening of the life of buildings. Sealant is able to achieve optimum performance in various use environments and construction methods. It is essential to develop a high performance, eco-friendly composite material with various materials.

Korean Patent Laid-Open No. 10-2013-0039469 as a prior art discloses the use of an expandable sealant as a technology relating to a fire-resistant filler for a pipe-penetrating portion of a building, Korean Patent Publication No. 10-2011-0027363 discloses a fire- The use of an expandable sealant in a hanok roof structure has been proposed.

However, such a conventional technique does not suggest a specific composition of a specific sealant composition.

In Korean Patent Laid-Open No. 10-2013-0073469, 100 parts by weight of a silicone compound base resin containing 50 to 70% by weight of polymethylvinylsiloxane resin, 10 to 30% by weight of silicon dioxide and 10 to 30% by weight of quartz powder , 10 to 20 parts by weight of a carbon black master batch, 1 to 3000 parts by weight of an addition reaction catalyst and 5 to 20 parts by weight of an organohydrogenpolysiloxane containing at least two Si-H in a molecule I am proposing.

However, in this technology, it is expected that the improvement of the fire resistance is expected. However, there is a need for a more improved sealant in order to maintain the fire resistance and flame retardancy while improving the sealing effect while applying environmentally friendly materials. There is also a need to improve the dispersibility of the sealant composition to produce a sealant composition having excellent physical properties.

Korean Patent Publication No. 10-2013-0039469 Korean Patent Publication No. 10-2011-0027363 Korean Patent Publication No. 10-2013-0073469

In order to solve the problems of the prior art as described above, the present invention aims to provide a high-quality sealant composition which doubles the physical properties and functionality of the modified silicone-based sealant composition of environmentally friendly components and improves the fire resistance.

Accordingly, an object of the present invention is to provide a sealant composition for an incendiary material, which is obtained by mixing expansive graphite, which has not been used in the prior art, with an environment-friendly modified silicone-based sealant at a specific ratio, and which has been imparted with high expansibility, high functionality and high degree of freedom.

Another object of the present invention is to provide a method for mixing expanded graphite with an expanded graphite to improve the fire resistance and expandability of the expanded graphite, and to disperse the expanded graphite having poor dispersibility into an excellent dispersibility, And to provide a method of manufacturing a sealant composition which enables high-quality production of the sealant composition.

In order to achieve the above object of the present invention, the present invention provides a thermoplastic resin composition comprising 30 to 40 wt% of a modified silicone (MS) polymer, 10 to 15 wt% of a silicone plasticizer, 3 to 5 wt% of a crosslinking agent, 5 to 10 wt% To 15% by weight of at least one additive selected from the group consisting of silica, silane, an adhesion promoter, and an addition catalyst as an additive.

The present invention also relates to a process for the preparation of a flame retardant composition comprising 30 to 40 wt% of a modified silicone (MS) polymer, 10 to 15 wt% of a silicone plasticizer, 3 to 5 wt% of a crosslinking agent, 5 to 10 wt% A raw material containing 30 to 40% by weight of at least one additive selected from silica, silane, an adhesion promoter and an addition reaction catalyst is compounded using a stirrer,

As the stirrer, a pair of rotatable paddles are provided in a cylindrical mixing vessel, and each of the paddles is provided with wings provided with four U-shaped grids facing each other in four chambers. Wherein the wings of the paddles are located at different heights, and the inner bottom of the mixing vessel is installed at a predetermined interval and a slope along the bottom of the mixing vessel and below the middle of the mixing vessel, Mixing an agitating member of a supersonic stacking structure with a stirrer provided so as to be rotatable so that the pair of paddles are rotatable within a radius of rotation of the agitating member while rotating the agitating member;

Stirring the mixture at 100 to 500 rpm using an agitator in the mixing process;

Maintaining the mixing temperature at 100 to 200 DEG C in the mixing step

And a method for producing the sealant composition for an incendiary material.

According to the present invention, the sealant composition for an anti-fouling material prepared as described above can be used as a sealant for an anti-fouling material exhibiting an environmentally friendly, high expansibility and high functionality by adding a graphite component to a modified urethane.

In particular, the present invention relates to a silicone rubber composition which is excellent in elasticity, weatherability, and durability using surface-modifiable modified silicone, which is capable of surface coating and maintains flame retardancy by the application of various additives and expanded graphite, It is possible to use a high-tech, high-function silane for the purpose of preventing flame.

According to the present invention, when expanded graphite and various additives are mixed with such a modified silicone-based sealant composition, problems of low dispersibility due to high viscosity are mixed and dispersed by using a stirrer of a new constitution, It is possible to easily produce an expandable sealant composition having a high quality.

BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a diagrammatic representation of a stirrer structure applied in an apparatus used in the manufacture of conventional sealant compositions.
FIG. 2 is a schematic view showing an embodiment of the configuration of a stirrer used in an apparatus for producing a sealant composition for an fireproof material according to the present invention.
3 is a view showing the construction of a water jacket which is additionally mounted outside the mixing vessel of the stirrer according to the present invention.
4 is an image showing a simulation result of a longitudinal vector according to a stirring state when the conventional stirrer (existing wing) of FIG. 1 and the stirrer (improved blade) structure used in the present invention of FIG. 2 are applied .
5 is an image showing a result of a stream line simulation according to a stirring state when the conventional stirrer (conventional wing) shown in FIG. 1 and the stirrer (improved wing) structure according to the present invention shown in FIG. 2 are applied.
FIG. 6 is an image showing the result of simulation of velocity distribution according to the stirring state of the conventional stirrer (conventional wing) of FIG. 1 and the stirrer (improved blade) structure of FIG. 2 according to the present invention.
7 is an image showing the result of a comparison of the convective heat transfer state of the sealant liquid according to the stirring state, when the conventional stirrer (conventional wing) of FIG. 1 and the stirrer (improved blade) to be.

Hereinafter, the present invention will be described in more detail as an embodiment.

The present invention relates to a method for producing a high-functionality, high-expansion, high-quality fire-retardant sealant composition by mixing expanded graphite-based sealant composition with expanded graphite and excellent dispersibility of such a sealant composition.

The raw material composition of the sealant composition for an incendiary material according to the present invention comprises a modified silicone (MS) polymer as a main component. The modified silicone polymer used in the present invention is used in an amount of 30 to 40% by weight based on the total raw material components, 10 to 15% by weight of a silicone plasticizer and 3 to 5% by weight of a crosslinking agent.

In the present invention, DINP can be used as the plasticizer. As the crosslinking agent, VTMS and the like can be used.

The present invention is characterized by using expanded graphite.

The expanded graphite used in the present invention is an interlaminar structure composed of carbon chains, and is a flame retardant material having a characteristic that when a sulfur or a nitrogen compound is injected between the layers, heat is applied and the layer is expanded several hundred times.

According to a preferred embodiment of the present invention, expanded graphite having a carbon content of 70 to 99% can be used, and it is possible to use those having a particle size of 10 to 300 mesh, more preferably 30 to 150 mesh. An expansion ratio of 50 to 600 ml / g, preferably 100 to 400 ml / g may be used, and a foaming initiation temperature of 100 to 300 ° C may be used.

If the carbon content of the expanded graphite is too small, there is a problem in that the flame retardancy is lowered. If the particle size is too small, there is a problem that the viscosity of the sealant becomes too low. If the particle size is too large, there is a problem that the viscosity becomes too high.

Such expanded graphite has excellent extensibility, heat retention, lubricity, plasticity, chemical stability and excellent plastic formability as well as excellent corrosion resistance, heat resistance, durability, high pressure resistance, adsorption property, heat dissipation property and sealing property.

In particular, expanded graphite is a flame retardant that forms a solid layer of halogen free. In most cases, it suppresses the generation of smoke, and the expanded carbon layer acts as an insulating layer, which interferes with the heat transfer and is combined with a non- halogen type environmentally friendly flame retardant And thus exhibits excellent physical properties when applied to a sealant for an fireproof material.

However, despite the excellent physical properties as described above, such expanded graphite has problems of poor dispersibility due to poor mixing due to high viscosity when applied to modified silicone-based sealants, so that even when mixed with a modified silicone-based sealant, it's difficult.

According to the present invention, the expanded graphite is used in an amount of 5 to 10% by weight in the entire raw material composition. When the content of the expanded graphite is less than 5% by weight, it is difficult to expect physical properties such as high expansion and high- There is a problem that the physical properties are lowered and the dispersibility is lowered, so that the manufacturing time for dispersing becomes longer.

In addition to the above components, the present invention also includes 10 to 15% by weight of a flame retardant and 30 to 40% by weight of at least one additive selected from silica, silane, adhesion promoter and addition catalyst as additives. As the flame retardant, aluminum hydroxide, a platinum flame retardant and the like can be used. As the adhesion-imparting agent, aminosilane and the like can be used. As the catalyst, a titanium catalyst or the like can be used.

According to the present invention, the modified silicone polymer is prepared by mixing expanded graphite with various additives. In this case, since the dispersibility of expanded graphite and various additive components is significantly lowered due to the high viscosity of the mixed components, a high-quality sealant composition having excellent physical properties as a whole There is a disadvantage that it is difficult to manufacture.

That is, the operation of incorporating the expanded graphite component having the above-mentioned flame retardancy into the sealant is performed by adding a cross-linking agent, a viscosity enhancer, etc. to the liquid silicone having a viscosity of about 50,000 cps to increase the viscosity to 1,000,000 cps or more, This is a low serious difficulty.

Therefore, when the sealant is manufactured by using the existing planetary structural stirrer, the physical property deviations are generated by batch or lot. In addition, since the reaction state varies in the mixing of materials having different specific gravity and characteristics of various raw materials in the production of silicon, there arises a problem of physical properties due to a technical limitation that can not achieve a sufficient dispersing effect.

In the case of a modified silicone-based sealant composition, it is necessary to cure it slowly and to mix it in the liquid form during the production process, and it is more difficult to uniformly disperse the mixed components as compared with other sealants in that a designated primer must be used.

Therefore, in order to produce a high viscosity sealant, most of the existing methods such as planetary structured batch mixer (stirrer) are not sufficient in terms of quality.

In order to solve such a problem, a new batch mixer having a dissolver-type structure is used in the present invention to greatly increase the dispersing effect, thereby manufacturing a high-quality sealant composition for a fireproof material.

According to a preferred embodiment of the present invention, a step of mixing the modified silicone polymer and the plasticizer in the above amounts to prepare a silicone compound base resin, and adding a cross-linking agent or the like for maintaining the characteristics of the modified silicone added in the step It goes through. Next, expanded graphite, calcium carbonate, and silica, silane, and catalyst are added as additives and compounding proceeds for 2 hours.

At this time, in order to overcome the difficulty of dispersion as described above in the mixing process of each component, a high-quality sealant composition for a fireproof material can be obtained by stirring using an improved type stirrer.

According to a preferred embodiment of the present invention, the viscosity of the sealant composition during the mixing process is preferably 1,000,000 to 1,500,000 cps, and the silicon is produced at a temperature of 100 ° C to 200 ° C, more preferably 100 ° C to 150 ° C, To 5 hours, more preferably 2 to 3 hours. At this time, the agitation speed of the agitator for mixing is preferably maintained at 100 to 500 rpm, more preferably 200 to 400 rpm.

Hereinafter, the stirrer used in the present invention will be described in detail as a specific example.

In the present invention, the stirrer used for mixing the raw material constituting the sealant composition is provided with a pair of rotatable paddles in a cylindrical mixing container. Preferably, the paddles are provided with vanes having four umbrella-type gratings facing each other in four chambers, and the pair of paddles are installed such that the wings of the paddles are positioned at different heights.

In the stirrer, an agitating member of a grid-like lattice structure having a predetermined gap and a slope is provided at an inner lower end of the mixing vessel along the bottom of the mixing vessel and below the middle of the mixing vessel, As shown in FIG.

Therefore, the stirrer may have a configuration of an agitator configured such that the pair of paddles are rotatable within a radius of rotation thereof while the stirrer rotates.

In addition, according to a preferred embodiment of the present invention, the stirrer may further include a water jacket installed to be able to adjust the temperature in the form of being wrapped around the outer side surface of the cylindrical mixing vessel.

According to the present invention, such a water jacket is covered with a heat insulating material on its outer side surface, and its inner side is in direct contact with the wall surface of the mixing vessel. Hot and cold water supply pipes through which hot water or cold water is supplied are densely arranged inside the water jacket, And the heat exchanging liquid is filled to transfer the heat generated in the supply line to the inside of the mixing vessel.

The construction of the stirrer of the present invention will be described in detail with reference to the accompanying drawings.

Figure 1 is a diagrammatic representation of a stirrer structure applied to the preparation of conventional sealant compositions.

1, the conventional stirrer 10 is composed of a stirrer having a pair of blades 40a and 40b, each of which is a shaped lattice 30 that rotates in a cylindrical container 20. The stirrer 10 having such a conventional wing stirs the sealant composition in the mixing vessel 20 while the wings 40a and 40b rotate in the same direction so that the sealant raw material components are mixed and dispersed.

In the present invention, a new stirrer having different wing structures is proposed in the conventional stirrer.

FIG. 2 is a schematic view showing one embodiment of the structure of a stirrer applied to the production of a sealant composition for an fireproof material according to the present invention.

According to a preferred embodiment of the present invention, the stirrer 100 of the present invention having an improved blade is provided with a pair of rotatable paddles 300a and 300b in a cylindrical mixing vessel 200, The lower ends of the paddles 300a and 300b may be provided with vanes 400a and 400b having four U-shaped gratings facing each other in four chambers. These four U-shaped gratings are installed on the paddles 300a and 300b so that individual gratings form a quadrangular grating structure.

According to a preferred embodiment of the present invention, the blades 400a and 400b of the C-shaped grid of each of the paddles 300a and 300b are arranged such that the four C-shaped grids are inclined at an angle of 20 to 50 degrees, (A) of 25 to 35 degrees and inclined at the same angle, so that the wings 400a and 400b are structured to be twisted in one direction as a whole, thereby further improving the stirring effect.

According to a preferred embodiment of the present invention, the four U-shaped gratings constituting the wings of the paddles 300a and 300b have inclination angles opposite to the rotation direction in accordance with the rotating direction of the paddles 300a and 300b .

In FIG. 2, the pair of paddles 300a and 300b may be installed such that the two paddles 400a and 400b are at the same height, but they may be positioned at different heights.

According to a preferred embodiment of the present invention, the positions of the paddles 300a and 300b of the agitator 100 are most preferably the positions of the paddles 300a and 300b of the stirrer composition 200 filled in the mixing vessel 200, And 3/2, respectively, with respect to the height of the mixed raw material, and it is preferable that they are provided at positions 3/1 and 3/2 on the left and right with respect to the diameter of the mixing vessel 200. It is preferable that the paddles 300a and 300b are positioned in consideration of the height and the interval of the paddles 300a and 300b from the viewpoint of the stirring effect.

The structure of the blades 400a and 400b of the stirrer 100 according to the present invention is characterized by a dissolver type stirrer completely different from the structure of the wings 40a and 40b of the conventional stirrer 10, An excellent dispersion effect which can not be achieved by conventional stirrers can be obtained even for a composition component having a high viscosity.

According to the present invention, the shape of the vanes 400a and 400b is a very characteristic structure, which is characterized by the rotational power of the agitator, average flow rate, stream line and velocity distribution analysis, fluid flow resistance, turbulent kinetic energy, Deformation rate, stirring condition, and the like, and is designed with the characteristic structure of the present invention in consideration of durability and stability.

According to a preferred embodiment of the present invention, the bottom of the mixing vessel 200 is installed with a predetermined gap and a slope along the bottom of the mixing vessel 210 and the vessel wall 220 below the middle of the mixing vessel An agitating member 500 having an upper opening and a lower light grating structure is rotatably installed.

According to the present invention, the stirring member 500 of the shaped grating structure having the above-mentioned upper light blocking structure has a slope at an inclination angle (b) of 5 to 20 degrees, more preferably 7 to 12 degrees with the wall surface of the mixing vessel 200 . &Lt; / RTI > The agitating members 500 may be spaced apart by a predetermined distance, for example, 10 to 50 cm, so as not to touch the container wall 220 of the mixing container 200. However, the interval may vary significantly depending on the size of the mixing vessel 200.

According to the present invention, the stirrer 100 of the present invention includes a pair of paddles 300a and 300b (not shown) inside a turning radius of the stirring member 500 while the stirring member 500 rotates in a lower portion of the mixing container 200, Can be rotatably arranged.

Therefore, when the stirrer 100 is operated after the raw material component of the sealant composition is injected into the mixing vessel 200 according to the present invention, at the center of the mixing vessel 200, vanes 400a And 400b are rotated and stirred, and the stirring member 500 is rotated and stirred at the bottom and the edge of the mixing vessel 200. [

In addition, according to a preferred embodiment of the present invention, a water jacket 600 installed to be able to adjust the temperature in the form of being wrapped around the outer side surface of the cylindrical mixing vessel 200 having the stirrer 100 is further included can do.

According to the present invention, the water jacket 600 can be applied to the mixing vessel 200 in such a manner that its outer side is covered with a heat insulating material 610 and its inner side is in direct contact with the outer wall surface of the mixing vessel 200 have.

3 is a view showing the construction of a water jacket 600 mounted outside the mixing vessel 200 of the stirrer 100 according to the present invention.

According to a preferred embodiment of the present invention, a cold / hot water supply pipe 620 to which hot water or cold water is supplied is densely arranged inside the water jacket 600.

The cold / hot water supply pipe 620 may have a vertically vertically arranged structure.

The cold / hot water supply pipes 620 of the present invention may be vertically arranged vertically and connected together, or may have several independent connection structures or independent structures.

In addition, the cold / hot water supply pipe 620 of the present invention may be installed to supply cold / hot water separately or separately, depending on the connection structure, but the hot water may be supplied to the upper portion and the cold water may be supplied to the lower portion.

According to a preferred embodiment of the present invention, the water jacket 600 may be filled with a heat exchange fluid 630 to transfer the heat generated from the cold / hot water supply pipe 620 to the interior of the mixing vessel 200. As the heat exchange liquid 630 used herein, water may be used. When the heat exchange liquid 630 is used, the heat exchange efficiency can be increased when the cold heat or the heat generated in the cold / hot water supply pipe 620 is supplied to the surface of the mixing container 200.

In the case of producing the sealant composition using the stirrer according to the present invention, the dispersing effect can be improved by 50% or more as compared with the case of using the stirrer having the conventional wing shape.

In order to confirm the dispersion effect of the stirrer having the improved wing structure of the present invention as described above, various simulations were performed in comparison with the conventional wing stirrer. The results are shown in comparison with FIG. 4 to FIG.

4 is an image showing simulation results of a longitudinal vector according to a stirring state when the conventional stirrer (conventional wing) shown in FIG. 1 and the stirrer (improved wing) structure according to the present invention shown in FIG. 2 are applied.

5, 6, and 7 are graphs showing the results of simulation of the stream line according to the agitation state, when the conventional agitator (conventional wing) of FIG. 1 and the agitator (improved blade) , The velocity distribution simulation result, and the results of the comparison of the convection heat transfer state of the sealant liquid, respectively.

As a result of the above simulation test, when the wing structure of the stirrer is compared with the case where the existing wing is applied and the stirrer having the structure of the improved wing according to the present invention is applied, the stirrer of the improved structure according to the present invention It was confirmed that the dispersing effect in the mixing and stirring step of the high viscous sealant raw material component was remarkably improved and the stirring effect was very excellent.

Therefore, when the sealant composition is manufactured using the manufacturing apparatus including the stirrer of the improved structure according to the present invention, excellent dispersion effect can be obtained.

In addition, when the temperature jacket is applied to adjust the temperature, it is possible to maximize the uniform dispersing effect. In particular, it has the advantage of maintaining the temperature by using hot water or cooling water, so that the sealant composition Can be produced.

According to the present invention, the above raw material components can be applied to a stirrer capable of dispersing even when raw materials having a viscosity of 1,000,000 to 1,500,000 cps and having a high viscosity are used.

According to the present invention, the raw material components used in the step of injecting the raw materials may be injected into a mixing vessel equipped with a stirrer in such a manner that a part of the raw materials are mixed in a master batch form. For example, a silicon compound base resin may be separately prepared, and a flame retardant master batch may be separately prepared and mixed.

According to the present invention, a pair of paddles installed in the mixing container under vacuum while injecting the raw material are rotated at 100 to 500 rpm, the stirring member is rotated at 100 to 500 rpm, and the raw material is mixed with stirring It is subjected to a mixing step.

According to a preferred embodiment of the present invention, the rotating direction of each paddle and the stirring member in the stirrer can be configured to rotate in the same direction or in opposite directions to each other. However, it is preferable that the paddles determine the direction of rotation in consideration of the direction in which the wings are inclined.

According to the present invention, it is advantageous for the dispersing effect to rotate the pair of paddles, preferably in opposite directions.

According to a preferred embodiment of the present invention, after the raw material is injected in the mixing step, the mixture is allowed to be in a vacuum state before the agitation can be started.

According to the present invention, the agitation time can be appropriately adjusted in accordance with the amount of the raw material to be injected, the injection method, the stirring speed, and the like.

According to a preferred embodiment of the present invention, when the mixing is completed in the mixing step, the operation of the stirrer can be completely stopped and then the combing operation can be performed. Further, when the shearing operation is completed, stirring is again performed, and the vacuum state is maintained to perform the dispersion effect of the raw material component and bubble removal, and then the vacuum is removed to complete the manufacture of the sealant composition.

According to the present invention, the stirring speed of the paddle and the agitating member may include a step of preparing the sealant composition by maintaining the internal temperature of the mixing vessel at 100 to 200 DEG C using the water jacket during the execution of the raw material mixing step .

Herein, the water jacket is supplied with cold / hot water through a cold / hot water supply pipe, and the supply amount thereof is controlled to maintain the temperature in the mixing container at a desired temperature.

In the case of preparing the sealant composition using the stirrer of the improved structure as described above, the stirrer may be prepared by mixing the highly viscous sealant of 1,000,000 cps or more, which is a sealant composition for an incendiary material containing expanded graphite according to the present invention, .

Particularly, according to the present invention, due to the structure of the stirrer having the above-described blades, the dispersing effect due to stirring of the highly viscous raw material component can be remarkably improved.

Further, since the dispersing effect is excellent by using the stirrer having the wings of the above-described improved structure, the production time of the expanded graphite-containing sealant composition of the present invention can be greatly shortened.

Therefore, it is possible to stably produce a homogeneous high-quality sealant composition having excellent dispersibility through controlling the stirring speed, agitation time, and temperature of the mixing vessel of the stirrer having such improved wings.

The water jacket may be mounted on the outer surface of the mixing vessel of the stirrer according to the present invention so that the temperature can be controlled according to the viscosity during stirring of the raw material components. Thus, a sealant composition containing various kinds of additives including modified silicon Dispersion and mixing efficiency in manufacturing can be increased.

Hereinafter, the present invention will be described in detail with reference to Examples, but the present invention is not limited to the Examples.

[Production Example 1] Production of silicone compound base resin (A)

60% by weight of HR-U 10,000 of HRS (weight) of 60,000 g / mol and a vinyl group content of 4 mol% was mixed for 30 minutes. 20% by weight of silicon dioxide (EVONIC Co. B.E.T., 300 m2 / g) and 20% by weight of quartz powder were compounded at 200 DEG C for 6 hours to the silicone polymer resin composition.

[Production Example 2] Production of silicone compound base resin (B)

50 weight% of HR-U (10,000) having a weight average molecular weight of 80,000 g / mol and a vinyl group content of 3 mol%, a weight average molecular weight of 10,000 g / mol and a vinyl group content of 5 mol% 10% by weight of HR-U (65,000) manufactured by HRS Corporation was mixed for 30 minutes. 20% by weight of silicone dioxide (EVONIC Co. B.E.T., 300 m2 / g) and 20% by weight of quartz powder were compounded at 200 DEG C for 6 hours to the silicone polymer resin composition.

[Production Example 3] Production of silicone compound base resin (C)

40 weight% of HR-U (10,000) of HRS, which has a weight average molecular weight of 80,000 g / mol and a vinyl group content of 3 mol%, a weight average molecular weight of 100,000 g / mol and a vinyl group content of 0.5 mol% 20% by weight of HR-U (65,000) was mixed for 30 minutes. 20% by weight of silica powder (EVONIC Co. B. E.T: 300 m2 / g) and 20% by weight of quartz powder were compounded in the silicone polymer resin composition at 200 DEG C for 6 hours.

Example, Comparative Example

A sealant composition for an incendiary material was prepared using the above-described stirrer with the composition shown in Table 1 below.

In the manufacturing process, a silicone compound base resin is prepared by mixing a modified silicone polymer and a plasticizer, a UV stabilizer and a crosslinking agent are added and mixed, and then expanded graphite, calcium carbonate, silica, silane, Lt; / RTI >

The viscosity of the raw material was 1,300,000 cps, and the temperature for preparing the sealant was 100 ° C to 150 ° C for 2 to 3 hours.

NO code Ingredients Standard amount (Kg) weight% One) X100101 MS POLYMER 410.00 29.53% 2) X100107 DINP 186.00 13.40% 3) X100103 UV stabilizer 20 1.44% 4) X1001013 Platinum flame retardant 0.3 0.02% 5) X100104 VTMS 15 1.08% 6) X1001015 Expanded graphite 100.00 7.20% 7) X100201 Silica MT-10 40.00 2.88% 8) X100203 Aluminum hydroxide 400.00 28.81% 9) X100202 OM5T-CACO3 200.00 14.40% 10) X100106 Aminosilane 7 0.50% 11) X100107 DINP 5 0.36% 12) X100109 Titanium catalyst 5 0.36% 13) X1001011 Platinum catalyst 0.2 0.01% TOTAL 1,388.5 100.00%

In Table 1, the following components were used.

- VTMS: cross linker

- DINP: Plasticizer

- Aminosilane: Adhesion promoter

- Aluminum hydroxide, platinum flame retardant: flame retardant

- Expanded Graphite: Carbon content of 90%, size 180 mesh, expansion rate of 400 ml / g, foaming initiation temperature of 150 ° C

Experimental Example

The prepared sealant composition was evaluated for flame retardancy after 168 hours of curing at room temperature 24 ° C / 50% with a specimen thickness of 2 to 3 mm, a length of 130 mm and a width of 13 mm.

The evaluation method is that the specimen is placed on the jig and the burner is removed for 10 seconds, and the time until the fire on the specimen is turned off, ie the burn time of the specimen, shall not exceed 10 seconds, The same test shall be repeated 10 times for 1 set, and the total burning time shall not exceed 50 seconds. Do not ignite the cotton wool which lies below about 30 seconds by the spark that melts when burning.

The compositions used in the experiments were adjusted while controlling the content of expanded graphite as shown in Table 2 (Examples 1 to 9 and Comparative Examples 1 to 3).

The experimental results are shown in Table 3 below.

Silicone compound (parts by weight) Graphite expansion (parts by weight) Flame retardant (parts by weight) Catalyst (PPM) Example 1 Production Example 1 100 5 15 600 Example 2 Production Example 1 100 10 15 600 Example 3 Production Example 1 100 15 15 600 Example 4 Production Example 2 100 5 15 600 Example 5 Production Example 2 100 10 15 600 Example 6 Production Example 2 100 15 15 600 Example 7 Production Example 3 100 5 15 600 Example 8 Production Example 3 100 10 15 600 Example 9 Production Example 3 100 15 15 600 Comparative Example 1 Production Example 1 100 17 15 600 Comparative Example 2 Production Example 1 100 30 15 600 Comparative Example 3 Production Example 1 100 4 15 600

Magnetization Burning Time (Sec) Fire resistance performance test Degree of expansion (%) Example 1 9.4 120 minutes 30 Example 2 6.9 120 minutes 32 Example 3 9.7 120 minutes 39 Example 4 9.8 120 minutes 31 Example 5 7.2 120 minutes 34 Example 6 9.8 120 minutes 39 Example 7 9.9 120 minutes 32 Example 8 8.1 120 minutes 33 Example 9 9.9 120 minutes 36 Comparative Example 1 16.3 90 minutes 50 Comparative Example 2 19.5 90 minutes 60 Comparative Example 3 12.5 60 minutes 21

10, 100 - stirrer
20, 200 - mixing vessel
210 -
220 - Container wall
30-shaped lattice
40a, 40b, 400a, 400b-wing
300a, 300b - paddle
500 - stirring member
600 - Water jacket
610 - Insulation
620 - Cold and hot water pipe
630 - Heat exchange liquid

Claims

Wherein the additive is silica, silane, or a mixture of 30 to 40 wt% of a modified silicone (MS) polymer, 10 to 15 wt% of a silicon plasticizer, 3 to 5 wt% of a crosslinking agent, 5 to 10 wt% of expanded graphite, And 30 to 40% by weight of at least one additive selected from the group consisting of an additive and an addition reaction catalyst.

The expanded graphite according to claim 1, wherein the expanded graphite has a carbon content of 70 to 99%, a size of 10 to 300 mesh, an expansion ratio of 50 to 600 ml / g, and a foaming initiation temperature of 100 to 300 ° C Wherein the sealant composition comprises at least one silane compound.

Wherein the additive is silica, silane, or a mixture of 30 to 40 wt% of a modified silicone (MS) polymer, 10 to 15 wt% of a silicon plasticizer, 3 to 5 wt% of a crosslinking agent, 5 to 10 wt% of expanded graphite, A raw material containing 30 to 40% by weight of at least one additive selected from an additive and an addition reaction catalyst is formulated using a stirrer,
As the stirrer, a pair of rotatable paddles are provided in a cylindrical mixing vessel, and each of the paddles is provided with vanes having four umbrella grids facing each other in four chambers, And an agitating member of a grid-like lattice structure having an upper opening and an upper opening is installed so as to be rotatable with a predetermined gap and a slope along the bottom wall of the mixing vessel and the wall of the vessel below the middle of the mixing vessel, Mixing the pellet with the stirrer so arranged that the pair of paddles are rotatable within a radius of rotation thereof while the member is rotating;
Stirring the mixture at 100 to 500 rpm using an agitator in the mixing process;
Maintaining the mixing temperature at 100 to 200 DEG C in the mixing step
&Lt; / RTI > wherein the silane coupling agent is a silane coupling agent.

[3] The apparatus as claimed in claim 2, wherein each of the paddle blades has four U-shaped gratings inclined at an equal angle to each other at an oblique angle of 20 to 50 degrees obliquely in the same direction, Wherein the sealant composition is formed into a shape of a cylinder.

The method of claim 4, wherein the four U-shaped gratings constituting the wings of the paddles are configured to have a slope tilted in a direction opposite to the rotational direction in accordance with the direction in which the paddles rotate.

The water jacket according to claim 3, wherein the stirrer further comprises a water jacket installed to be able to adjust the temperature in the form of being wrapped around the outer surface of the cylindrical mixing vessel, the water jacket having an outer surface covered with a heat insulating material, Hot water or cold water is supplied to the interior of the water jacket and the heat exchanging fluid is filled to transfer the heat generated from the hot and cold water supply pipe to the inside of the mixing container &Lt; / RTI > wherein the silane coupling agent is a silane coupling agent.