KR20130136625A - Flame-retardant coating composition, preparation thereof, and flame-retardant expanded polystyrene foam using the same - Google Patents
Flame-retardant coating composition, preparation thereof, and flame-retardant expanded polystyrene foam using the same Download PDFInfo
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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Abstract
According to the present invention, a metal hydrate, an inorganic flame retardant, a polyphosphate compound, a graphite compound, and a water-soluble polymer adhesive are dispersed as a flame retardant composition in water as a solvent, kneaded at 20 to 70 degrees for 10 minutes to 3 hours, and Provided are a method for producing a flame retardant coating composition for expanded polystyrene comprising adding a curing agent as an auxiliary composition, and a flame retardant coating composition obtained and a flame retardant EPS foam.
The flame-retardant coating composition prepared according to the present invention is water-based, environmentally friendly, long pot life, simple to manufacture and use, economical manufacturing cost, flame-retardant EPS foam foam produced using the flame-retardant coating composition of the present invention And fire retardant building materials are manufactured by eco-friendly process because the raw material is water-based, and it can be manufactured by using existing manufacturing equipment, and it is economical and it is safe because it does not generate toxic gas, and it is based on EPS through existing chemical modification. It can provide excellent flame retardant performance compared to insulation.
Description
The present invention relates to a flame retardant coating composition, a method for preparing the same, and a flame retardant expanded polystyrene foam using the same. Specifically, the present invention relates to a flame retardant coating composition for expanded polystyrene comprising water, a metal hydrate, an inorganic flame retardant, a polyphosphate compound, a graphite compound, a water-soluble polymer adhesive, and a curing agent, a method for preparing the same, and a foamed polystyrene foam using the same. will be.
Expanded Polystyrene (EPS) is one of the insulation materials that is widely used as a building insulation material because of its excellent thermal insulation performance and low manufacturing cost. The melting point of polystyrene is very low around 100 degrees and has a disadvantage of being very vulnerable to fire when used as a heat insulating material because it is vulnerable to flame. For this reason, the foamed polystyrene is required by law to be used only in some temporary buildings or prefabricated buildings that do not require flame retardant performance.
In order to solve the above-mentioned problems of polystyrene, many studies have been conducted to impart flame retardant performance to polystyrene polymers. One research direction is to synthesize flame retardant polystyrene resin that is hardly burned by chemically modifying the molecular chain of polystyrene, and the other research direction is to give flame retardant performance by coating a flame retardant solution on expanded polystyrene. .
The first method is one of the major research topics of large chemical companies in the United States and Europe, and aims to improve the flame retardant performance by compounding flame retardant molecular chains with polystyrene structures. It is well known that in recent years, research has been carried out not only in Europe and Europe, but also in Japan, Korea, and almost all countries that use EPS insulation. Samsung Group in South Korea is also known for the final inspection of the current process aimed at mass production by producing chemically-retardant polystyrene. It is known that the flame retardant performance is improved by using the first method compared to general EPS, but it is difficult to expect dramatic performance improvement such as not burning because the polystyrene molecular chain itself is a heat sensitive material.
The second method is a technique of coating a flame retardant material on a polystyrene bead, and it is possible to commercialize it more easily if only the proper ratio of the flame retardant material and the coating material can be understood. .
Representatively, Korean Patent Application No. 10-2010-0046175 discloses a method of multi-coating a flame retardant material through a polymer coating material (adhesive) by first coating and drying the flame retardant layer with a hydrophobic resin component, followed by secondary coating and drying. Has published a way to obtain expanded polystyrene with excellent flame retardancy. However, this method raises the manufacturing cost by repeating the coating and drying, there is a problem that the detachment of the primary coating flame retardant may occur during the second coating.
Similarly, Korean Patent Application No. 10-2007-0121147 discloses a method for preparing a flame retardant composition comprising an inorganic flame retardant, a silicate flame retardant, and various other inorganic materials, which can be used to prepare a flame retardant expanded polystyrene, but mainly a liquid silicate. The flame retardant effect can be maximized by using the compound, but there is room for improvement due to the problem that the inorganic material is so high that the loss of inorganic material is greater than that of the coating material when used as a coating material.
Korean Patent Application No. 10-2005-0119183 discloses a device for manufacturing a flame-retardant expanded polystyrene foam using a flame-retardant coating solution, a special apparatus for producing a flame-retardant EPS compared to conventional EPS is envisioned. It was.
Meanwhile, a method of producing flame retardant polystyrene (black) by using a method of adding carbon black and expanded graphite to EPS beads in a large amount by extrusion foaming has been proposed (LG chemistry). It is difficult to use universally because it is only available in large-scale businesses.
In general, it is required to have the following basic properties for the general purpose flame retardant coating liquid composition for expanded polystyrene:
1) delay the chain reaction of the radical active material generated by the flame,
2) Non-combustible gas (H 2 O, CO 2 , NH 3 To increase the flash point of the gas,
3) Forming glass coating on combustion materials prevents the access of oxygen,
4) promote the production of non-combustible carbide (char),
5) It needs functionality that inhibits combustion heat through endothermic reaction.
In order to develop a flame retardant coating liquid composition for expanded polystyrene having the basic characteristics as described above, the present inventors have separately studied the characteristics of components (hereinafter, referred to as flame retardant materials) constituting the flame retardant coating solution, and combine them again. By selecting the flame retardant materials that can achieve the optimum flame retardant performance, and by selecting a polymer adhesive material suitable for the selected flame retardant materials to develop a new flame retardant coating composition for expanded polystyrene.
As a result, the present inventors have found that in the composition comprising 1) metal oxide and metal hydrate, 2) metal hydrate and amine flame retardant, 3) liquid silicate compound and polyphosphate compound, 4) expanded graphite, 5) metal hydrate, By exhibiting the flame retardant mechanism as shown in Table 1 below, it was found that the basic characteristics required for the flame retardant coating liquid composition for expanded polystyrene which can be used universally as described above was completed and the present invention was completed.
The flame-retardant coating composition prepared according to the present invention is water-based, so it is environmentally friendly, long pot life, simple to manufacture and use, and economical to manufacture.
Flame-retardant EPS foam and flame-retardant building materials produced using the flame-retardant coating composition of the present invention is manufactured in an environmentally friendly process because the raw material is water-based, and can be manufactured using the existing manufacturing apparatus, economical, generating toxic gas Not only is it safe, but it can provide excellent flame retardant performance compared to EPS-based insulation through conventional chemical modification.
1 is a photograph of a flame-retardant EPS foam foam prepared using a flame-retardant coating solution of the present invention.
A first object of the present invention is a flame retardant coating composition for expanded polystyrene comprising water as a solvent, metal hydrate as a flame retardant, an inorganic flame retardant, a polyphosphate compound and a graphite compound, a water-soluble polymer adhesive as an adhesive composition, and a curing agent as an adhesive aid. To provide.
The second object of the present invention is to disperse a water-soluble polymer adhesive as a flame retardant composition in water as a solvent, a metal hydrate, an inorganic flame retardant, a polyphosphate compound and a graphite compound, and an adhesive composition, kneading at 20 to 70 ° C. for at least 30 minutes, and adhering It provides a method for producing a flame-retardant coating composition for expanded polystyrene comprising the addition of a curing agent as an auxiliary composition.
A third object of the present invention is a flame retardant coating composition for expanded polystyrene comprising water as a solvent, a metal hydrate, an inorganic flame retardant, a polyphosphate compound and a graphite compound as a flame retardant composition, a water-soluble polymer adhesive as an adhesive composition, and a curing agent as an adhesive aid. It is to provide a flame-retardant EPS (foam polystyrene) foam foam prepared using.
The invention is explained in more detail below with reference to the drawings.
As described above, in order for the flame retardant coating liquid composition for expanded polystyrene to be used universally, it is necessary to have the following basic characteristics 1) to 5):
1) delay the chain reaction of the radical active material generated by the flame,
2) Non-combustible gas (H 2 O, CO 2 , NH 3 To increase the flash point of the gas,
3) Forming glass coating on combustion materials prevents the access of oxygen,
4) promote the production of non-combustible carbide (char),
5) It needs functionality that inhibits combustion heat through endothermic reaction.
It was investigated that the basic properties 1) to 5) described above could be achieved by the components as described in Table 1.
Delayed chain reaction
Oxygen Access Block
Reduction of heat of combustion
As a flame retardant coating composition for expanded polystyrene having the basic properties 1) to 5) described above, the present invention provides water as a solvent, a metal hydrate as a flame retardant composition, an inorganic flame retardant, a polyphosphate compound and a graphite compound, a water-soluble polymer adhesive as an adhesive composition, and Provided is a composition comprising a curing agent as adhesion aid.
As the metal hydrate, all metal hydrates produced commercially can be mentioned. Generally, Al (OH) 3 , Mg (OH) 2 and Ca (OH) 2 are mainly used for economic reasons, and the amount of the metal hydrate is flame retardant coating composition. 5 to 25% by weight, specifically 7 to 20% by weight, preferably 10 to 15% by weight based on the total weight of the.
As inorganic flame retardants, mention may be made of metal oxides such as SiO 2 , TiO 2 , MnO 2 , CaO, MgO, Fe 2 O 3 , Al 2 O 3 , Sb 2 O 3 , CuO, ZnO, Borax, Zinc Borate, etc. SiO 2 and MnO 2 may be used in particular, and the amount thereof may be used in an amount of 5 to 20% by weight, particularly 5 to 10% by weight, preferably 5 to 10% by weight, based on the total weight of the flame retardant coating composition. to be. On the other hand, as a metal oxide, Sb 2 O 3 is a compound having good flame retardant performance and can be used as an important component of a flame retardant coating composition, but the radical compound generated at the time of combustion may be harmful to the human body and is expensive, so be careful in use. do.
Examples of polyphosphate compounds that serve to block oxygen access by forming a glass coating film may include melamine polyphosphate and ammonium polyphosphate, and the amount of polyphosphate is 5% based on the total weight of the flame retardant coating composition. 20 weight%, Preferably it is 7-15 weight%.
On the other hand, the liquid silicate conventionally used as a material for forming a glass coating film is not used in the present invention, but does not depart from the scope of the present invention even if a small amount is included as necessary.
Examples of graphite compounds that form carbide during combustion may include expanded graphite and activated carbon. The amount of the graphite compound used is 13-25 wt%, preferably 17-25 wt%, based on the total weight of the flame retardant coating composition. . Graphite compounds can be advantageously used to expand the graphite of less than 100 mesh because the particle size is relatively small is effective.
In the present invention, the weight ratio of the polyphosphate compound and the graphite compound is 0.5: 1 to 1: 5, specifically 0.8: 1 to 1: 3, preferably 1: 1 to 1: 2.5, and most preferably 1: 1.1 to 1: 1.7.
As the adhesive composition, water-soluble polymer adhesives may include phenol adhesives, polyurethane adhesives, polyvinyl alcohol (PVA) adhesives, polyvinylacetate (PVAc) adhesives, polyacrylic acid (PAA) adhesives, and the like. Mention may be made of PVAc adhesives and PAA adhesives, more preferably PAA adhesives.
Phenolic adhesives used for wood have insufficient compatibility with graphite compounds and can react with polyphosphate compounds added together. However, when a commercially available water-soluble polyurethane adhesive is used together with an expensive diisocyanate-based curing agent as an adhesive auxiliary composition, the water resistance can be further improved and the elution of the flame retardant coating agent by water can be prevented.
When using a PVA-based adhesive, a low molecular weight PVA powder having a molecular weight of 50,000 or less can be purchased and dissolved in warm water at a concentration of 1 to 5%, and a dialdehyde compound can be used as a curing agent to ensure water resistance during drying. . However, PVA is relatively low in adhesion and lacks in water resistance, so it is highly reactive, but a dialdehyde such as expensive glutaraldehyde should be used.
PVAc adhesives are usually prepared by dissolving high molecular weight PVAc in an organic solvent, or may use a commercially available water-soluble PVAc adhesive. PVAc adhesives can improve water resistance by using a small amount of methylenediphenyl diisocyanate as an adhesion aid. do. The PVAc adhesive shows good adhesion when the flame retardant coating liquid is dried, but the adhesive strength may decrease with time, and thus an additional component may be required.
Polyacrylic acid (PAA) -based water-soluble adhesives are widely used in paint, industrial, and construction applications. Recently, due to environmental problems, there are also improvements to improve the relatively poor adhesive strength of water-soluble acrylic adhesives. In addition, there is an advantage that the inorganic flame retardant compositions can be well dispersed in the flame retardant coating liquid due to the effects of various surfactants contained in the adhesive.
The amount of the water-soluble polymer adhesive is 10 to 30% by weight, preferably 15 to 25% by weight based on the total weight of the flame retardant coating liquid.
On the other hand, since the water-soluble polymer adhesive itself is water-soluble, its water resistance is low after drying, and therefore, even if the adhesive is completely dried, the dried surface melts little by little when it is exposed to moisture, thereby failing to maintain the original adhesive performance properly. May occur. For this reason, a hardening | curing agent can be used as adhesion | attachment auxiliary property for assisting the water resistance of water-soluble polymer adhesive.
As the adhesion assistant, a curing agent may include a difunctional compound such as a diisocyanate compound or a dialdehyde compound, and specifically, glutaraldehyde, methylene diphenyl diisocyanate, and toluene diisocyanate. (toluene diisocyanate, TDI) and the like can be mentioned.
On the other hand, as the adhesion aid, various starches, cellulose thickeners and the like can be further used together with or independently of the above-described bifunctional compound.
The amount of the auxiliary adhesive aid is 0.1 to 3.5% by weight, specifically 0.2 to 3% by weight, preferably 0.5 to 2% by weight, based on the total weight of the flame retardant coating liquid.
The second object of the present invention is to disperse a water-soluble polymer adhesive as a flame retardant composition in water as a solvent, a metal hydrate, an inorganic flame retardant, a polyphosphate compound and a graphite compound, and an adhesive composition, kneading at 20 to 70 ° C. for at least 30 minutes, and adhering It is to provide a method for producing a flame-retardant coating composition for expanded polystyrene, comprising adding a curing agent as an auxiliary composition.
According to one embodiment of the invention, the kneading described above is at least 30 minutes at a temperature of 20 to 70 ℃, especially 25 to 65 ℃, preferably 30 to 60 ℃, more preferably 35 to 55 ℃, Especially at least 45 minutes, preferably at least 1 hour, more preferably at least 2 hours. The temperature can be maintained, for example, by direct heating or bath. By boiling water and kneading at the above temperature, it is possible to shorten the time required to fully hydrate the expanded graphite, to prevent the viscosity change of the flame-retardant coating composition in the future and to improve the water resistance. If the kneading is performed at a low temperature, for example, room temperature, the welding performance may be insufficient, and thus the molding of the flame-retardant EPS foam may not be performed properly.
In the present invention, even if the kneading is performed even at a low temperature such as room temperature for a very long time, for example, 24 hours or more, the flame retardancy and the physical properties desired in the present invention may be achieved, and therefore there is no upper limit to the kneading time. However, if the kneading time is too long, the productivity decreases and the manufacturing cost increases, so it is preferable to perform the kneading for a short time at an elevated temperature. It is advantageous to adjust the kneading temperature so that the kneading can be carried out for 30 minutes to 6 hours, specifically for 45 minutes to 5 hours, preferably for 1 hour to 4 hours.
In the present invention, after kneading the other components first, the curing agent is added, stabilized and then cured. The reactivity due to the interaction between the adhesive and the adhesive aid was measured by mixing the two compositions together with the flame retardant composition, and measuring the time required to produce a stable liquid phase without any further gas generation at the reaction temperature of 30 ° C. It was confirmed by measuring the curing time taken until the reaction solution was solidified by stirring.
Preparation of flame-retardant EPS foam using the flame-retardant coating composition prepared according to the present invention can be carried out according to the following procedure:
The primary foamed EPS beads, which are foamed water support materials, are injected into the steam heating unit of a conventional EPS foam manufacturing apparatus. The flame-retardant coating composition according to the present invention was administered in the same amount (100 parts by weight) based on 100 parts by weight of the first foamed EPS beads, kneaded for 5 minutes to 1 hour, particularly 10 minutes to 30 minutes, and dried to remove moisture. To obtain flame-retardant coating composition-coated EPS beads. The flame-retardant coating composition-coated EPS beads obtained are introduced into a foamer through a dry aging tube maintained at 40-70 ° C., especially 50-60 ° C., and heated to expand the beads to form a foam. After the resulting foam is air dried, flame retardancy is measured.
Flame retardancy is measured by cutting the flame-retardant EPS foam prepared above to 100 x 100 x 50 (mm), and then a matchstick is put on for 5 seconds and squeezed to measure the time remaining after burning. Depending on the time, it is classified into excellent (less than 5 seconds), good (between 5 seconds and 10 seconds), and poor (more than 10 seconds).
As can be seen in Figure 1, in the flame-retardant EPS foam foam prepared using the flame-retardant coating composition of the present invention, the expanded beads of EPS have a uniform particle size and most of the particle shape is hexagonal, so the filling rate is high almost without gaps, Therefore, the effect is high as a heat insulating material. In addition, it can be seen that the flame retardant coating composition of the present invention is uniformly coated.
Hereinafter, the present invention will be described in detail through various embodiments, and the present invention is not limited to these embodiments.
Example One:
Step 1) Flame Retardant Coating Composition Produce:
32 kg of water and 9 kg of PAA adhesive were introduced into a 100 L reactor and stirred for 10 minutes at room temperature. To this was added 8 kg of Al (OH) 3 , 2 kg of ZnO and 6 kg of melamine polyphosphonate and stirred at high speed to completely disperse or dissolve all the particles. To the resulting mixture was added 1 kg of activated carbon and 9 kg of expanded graphite (200 mesh) and stirred at high speed until the expanded graphite was well dispersed in the solution. When the dispersion was completed, the temperature of the reaction mixture was slowly raised and stirred for 1 hour while maintaining at 35 to 45 degrees. The reaction mixture was cooled to room temperature and a small amount of methylenediphenyl diisocyanate (MDI) was added as a curing agent to obtain a flame retardant coating composition.
Step 2) Flame Retardant EPS Foam Produce:
100 parts by weight of the flame retardant coating composition obtained in step 1) and 100 parts by weight of the primary foamed EPS beads were introduced into a conventional EPS foam manufacturing apparatus and dried with kneading for 20 minutes to remove moisture. As a result, EPS beads coated with a flame-retardant coating composition from which moisture was removed were transferred to a dry aging tube maintained at 50 to 60 degrees to completely remove the remaining moisture and to mature the EPS beads. The EPS beads fully dried in a dry aging tube were introduced into a foamer, and foamed by applying steam pressure, and then foamed to obtain a flame-retardant EPS foam by completely drying them to remove moisture from the surface.
The flame retardant EPS foam obtained was cut to 100 x 100 x 50 (mm), and the flame retardant performance was measured. The flame retardant performance was measured by applying a matched flame to the cut flame retardant EPS foam and keeping it for 5 seconds, then removing the flame and measuring the remaining time of flame retardation. If more than 10 seconds, read as bad. Foam foam obtained in Example 1 was excellent in flame retardant performance.
Example 2-9 and Comparative Example 1-2
As shown in Table 2, the flame retardant coating composition and flame retardant EPS foam were obtained by repeating the procedure of Example 1 except changing the type of metal hydrate and inorganic flame retardant. About the flame-retardant EPS foam obtained, flame-retardant performance was measured similarly to Example 1, and the result is shown in Table 2.
As shown in Table 2, the flame retardant performance of the finally obtained flame-retardant EPS foam was mostly excellent, it is shown that the flame retardant performance is reduced in the absence of any one of the metal hydrate and inorganic flame retardant (Comparative Examples 1 and 2) .
Example 10-18 and Comparative Example 3 to 6
The flame retardant performance was tested by changing the composition of expanded graphite and polyphosphoric acid. The used polyphosphoric acid was expressed as MPP (melamine polyphosphate) and APP (ammonium polyphosphate), and then flame-retardant EPS foam was prepared using the flame-retardant coating composition as in Example 1, and the flame-retardant performance was tested.
In Comparative Examples 3 to 6, flame retardant coating compositions were prepared using liquid silicates, and flame retardant EPS foams were obtained therefrom to test the flame retardant performance.
Kinds
input
Kinds
input
Liquid Silicate *
4 kg
Liquid Silicate *
4 kg
As compared with Example 12 and Example 18 of Table 3, polyphosphoric acid and expanded graphite was found to have a significant effect on the flame retardant performance even if any one of them is reduced.
The use of liquid silicates to form glass coatings has been found to adversely affect the flame retardant performance. In addition, as shown in Comparative Examples 3 and 4, when polyphosphoric acid and liquid silicate were used together, a phenomenon was observed that the polyphosphoric acid and the liquid silicate were not formed regardless of the use of expanded graphite. Estimated.
As shown in Comparative Example 5 and Comparative Example 6, the liquid silicate was found to adversely affect the flame retardant performance in this flame retardant composition.
Example 19
Except for using TDI as an adhesion aid, it was carried out in the same manner as in Example 1, and the flame retardant performance was tested for the flame-retardant EPS foam obtained.
Example 20
The reaction temperature was varied at the time of preparing the flame retardant coating composition and the results are summarized in Table 5. The measurement of water resistance confirmed that the flame-retardant composition flowed out after the foamed flame-retardant EPS foam was cut into 100 x 100 x 50 (mm) and then placed in warm water.
When the water resistance is poor, it can be seen that the expanded graphite detaches very easily. Such a method has shown a very reliable result by a simple test. In addition, even if the expanded graphite does not flow, the flame retardant composition flows out after about 5-6 hours, and the water is cloudy, which is very suitable for measuring the water resistance. The measurement was judged to be excellent if the aqueous solution containing the foam was cloudy within a day (24 hours), poor, if it flowed between two to three days, and stable without flowing for more than three days.
(Fusion performance)
As shown in the table, when the reaction was carried out at room temperature for 24 hours or more, it was found that the molding performance was improved and the water resistance was excellent. Therefore, if the reaction time is longer, it is expected that a product having excellent molding performance and water resistance can be obtained.
The flame-retardant coating composition prepared according to the present invention, the flame-retardant EPS foam foam prepared using the same is the environmentally friendly raw materials and processes, ease of use due to long pot life, safety without toxic gas generation, low manufacturing cost and conventional manufacturing Not only has the advantages of economics due to the use of the device, but also excellent flame retardant effect, it is commercially excellent as a flame retardant building materials and packaging materials.
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KR102572769B1 (en) | 2022-09-08 | 2023-08-30 | 주식회사 현대바이오랜드 | A cosmetic composition for scalp care damaged by external stimuli or for alleviating stress-related hair loss containing a complex extract of buckwheat sprouts and chamomile pretreated with ultra-high pressure |
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