KR100898418B1 - The fire retardant adhesive compositon and the production method thereof - Google Patents

Abstract

The present invention relates to a composition of a flame-retardant adhesive, more specifically, melamine cyanurate (0.1-5 parts by weight, magnesium hydroxide 0.5-5 parts by weight, feldspar 7-15 parts by weight, zeolite 15-30 parts by weight and A flame retardant adhesive composition comprising 60 to 75 parts by weight of sodium silicate and a method for manufacturing the same, comprising an organic flame retardant, an inorganic flame retardant, and sodium silicate, which are environmentally friendly and flame retardant having excellent flame retardancy, heat shielding property, adhesiveness, and water resistance. A composition of an adhesive and a method for producing the same.

Flame Retardant Adhesive, Organic, Inorganic, Non-Halogen-Based

Description

Flame retardant adhesive composition and its manufacturing method {THE FIRE RETARDANT ADHESIVE COMPOSITON AND THE PRODUCTION METHOD THEREOF}

The present invention relates to a composition of a flame-retardant adhesive, more specifically, melamine cyanurate (0.1-5 parts by weight, magnesium hydroxide 0.5-5 parts by weight, feldspar 7-15 parts by weight, zeolite 15-30 parts by weight and A flame retardant adhesive composition comprising 60 to 75 parts by weight of sodium silicate and a method for manufacturing the same, comprising an organic flame retardant, an inorganic flame retardant, and sodium silicate, which are environmentally friendly and flame retardant having excellent flame retardancy, heat shielding property, adhesiveness, and water resistance. A composition of an adhesive and a method for producing the same.

Flame retardants are materials added to prevent burning by physically or chemically improving most combustible materials such as paper, cloth, plastics, and wood, which are easily burned. In general, flame retardants widely used are divided into additive type and reactive type according to the method applied to the combustible material, and the additive type is divided into organic type and inorganic type flame retardant according to constituents. Additive flame retardant is to physically add the flame retardant to improve the flame retardancy, the reactive flame retardant is to cause a chemical reaction to improve the flame retardancy.

Organics are mainly classified into non-halogen flame retardants including phosphorus and nitrogen, and halogens including bromine and chlorine, and inorganics are classified into aluminum hydroxide, magnesium hydroxide and antimony-based products.

Of the halogen-based flame retardants that are currently used the most, brominated flame retardants have excellent flame retardant effects and are excellent in cost / performance. They are housing materials for electrical and office equipment, ABS (acrylonitrile butadiene styrene copolymer) resins and PS (polystyrene). ), PBT (poly butylene terephthalate), PET (polyethylene terephthalate), epoxy resins, etc. are used as a main flame retardant, but serious problems that dioxin occurs during combustion has been pointed out, especially the compound used for the production of bromine-based flame retardant It is known that restrictions on the use of decabromophenyl dioxide and octabromophenylether are under consideration in various European countries. In addition, among inorganic flame retardants, antimony compounds are also endlessly harmful to humans.

In Europe, there is a recent restriction on the halogen and antimony-containing flame retardants, such as 'Ecolabel', and the recent development of the flame retardant is not merely excellent in flame retardancy, but also has low toxicity, low smoke, It is attracted by the development of non-halogen-based and non-antimony-based flame retardants having low corrosion resistance and heat resistance.

Inorganic flame retardants are widely used flame retardants and dehydrated at high temperatures to cause fire extinguishing, which acts as a flame retardant, but it is difficult to sustain the flame retardant.Phosphorous flame retardants in non-halogen flame retardants are polymerized by dehydration reactions as phosphoric acid is generated during combustion. It forms a phosphate film to block oxygen to express a flame retardant effect, but when phosphate becomes a liquid has a disadvantage that flows well. In addition, phosphorus-based flame retardants satisfy the two aspects of low toxicity and high performance, but has been spotlighted as a substitute for halogen-based flame retardants, but the process cost of replacing the phosphorus-based flame retardant in the existing product is a disadvantage that is relatively expensive.

Accordingly, the present invention relates to a flame-retardant adhesive composition having excellent flame retardancy, low toxicity, low toxicity, and excellent adhesion, and a method for producing a flame-retardant adhesive composition having excellent storage properties.

The present invention to achieve the above object, melamine cyanurate (melamine cyanurate) 0.1 to 5 parts by weight, magnesium hydroxide 0.5 to 5 parts by weight, feldspar 7 to 15 parts by weight, zeolite 15 to 30 parts by weight and sodium silicate 60 to 75 It provides a flame-retardant adhesive composition and a method for producing the same, comprising a weight part.

The present invention is a composition of a flame retardant adhesive, melamine cyanurate (0.1-5 parts by weight, magnesium hydroxide 0.5-5 parts by weight, lead stone 7-15 parts by weight, zeolite 15-30 parts by weight and sodium silicate 60-75 parts) Environmentally friendly and flame retardant, heat shielding, adhesiveness, water resistance by the use, including the part, and excellent flame retardant adhesive method of the present invention, the inorganic flame retardant is first added to the sodium silicate and mixed by stirring and then added to the organic flame retardant Due to the use of stirring and mixing the storage stability is excellent effect.

In addition, the flame-retardant adhesive of the present invention is applied to wood, plastic, non-woven fabric, organic fiber felt, such as plywood, laminated wood, it is possible to give excellent flame retardancy and heat shielding properties.

The present invention relates to a composition of a flame-retardant adhesive, more specifically, melamine cyanurate (0.1-5 parts by weight, magnesium hydroxide 0.5-5 parts by weight, feldspar 7-15 parts by weight, zeolite 15-30 parts by weight and A flame retardant adhesive composition comprising 60 to 75 parts by weight of sodium silicate, and a method for manufacturing the same, comprising an organic flame retardant, an inorganic flame retardant, and sodium silicate, which are environmentally friendly and flame retardant having excellent flame retardancy, heat shielding, adhesiveness, and water resistance. A composition of an adhesive and a method for producing the same.

In more detail, the present invention uses melamine cyanurate as an organic flame retardant, and added a lead, magnesium hydroxide, and zeolite as an inorganic flame retardant to impart a heat shielding effect and a flame retardant synergistic effect, and an adhesive material. It characterized by using sodium silicate.

In the present invention, non-halogen melamine cyanurate is used as the organic flame retardant. Melamine cyanurate is less toxic than halogen-based and has an easy handling characteristic. In particular, there is no generation of toxic gas during pyrolysis of melamine-containing soft polyurethane foam products, and less smoke than other flame retardants. The United states Environmental Protection Agency has published studies showing that melamine has a low risk of toxicity to the environment and no evidence of adverse effects on human health or the environment. In the present invention, the amount of melamine cyanurate used was 0.1 to 5 parts by weight of the total weight. If the amount is less than 0.1 parts by weight, the flame retardant effect is lowered, if more than 5 parts by weight, the flame retardant effect is excellent, but organic-based flame retardant is expensive, there is a disadvantage that the raw material cost increases.

In addition, in the present invention, mixed with an organic flame retardant is used as an inorganic flame retardant for imparting synergistic effect, non-antimony-based leadstone, magnesium hydroxide, zeolite was used, especially due to magnesium hydroxide to provide heat shielding properties. Magnesium hydroxide is superior to aluminum hydroxide, which is an inorganic flame retardant, which has a different flame retardant effect per compounding amount, and is inexpensive and has advantages such as suppressing toxic gas and smoke generation. Pyrite and zeolite are excellent in heat resistance and fire resistance, when used in combination with the flame retardant increases the flame retardant effect and heat shielding effect. Conventionally, an antimony-based material (antimony trioxide, etc.) was used as an inorganic flame retardant in an organic flame retardant to increase the flame retardant effect. As described above, antimony trioxide corresponds to a human harmful substance, and in the present invention, aluminum hydroxide, lead stone, zeolite, and the like. The mixture was used to make it environmentally friendly and excellent in flame retardancy.

The amount of the inorganic flame retardant is preferably 22 to 50 parts by weight of the total weight.

When the amount is less than 22 parts by weight, the flame retardant synergistic effect is insignificant, and when it is used by more than 50 parts by weight, the specific gravity becomes high, resulting in poor storage performance. In particular, heat shielding properties could be imparted by using 0.5 to 5 parts by weight of magnesium hydroxide in the inorganic flame retardant. This is because magnesium hydroxide dehydrates when heat is applied. In addition, the present invention was able to increase the flame retardancy and heat shielding properties by further adding a lead and zeolite. Preferably, 0.5 to 5 parts by weight of magnesium hydroxide, 7 to 15 parts by weight of feldspar, and 15 to 30 parts by weight of zeolite are preferably used.

In addition, inorganic adhesives for imparting adhesion may include sodium silicate, potassium silicate, silicalazol, alumina sol, and the like, and among them, the cheapest sodium silicate is preferably used, and the lowest viscosity is considered in consideration of mass production. It is preferable to use three kinds of sodium silicate. The amount of sodium silicate used was 60 to 75 parts by weight of the total parts. The adhesion was poor at less than 60 parts by weight, and the adhesion was poor at a sensitivity of 75 parts by weight or more, and the drying time was long. In addition, since sodium silicate is foamed when contacted with the flame to form a fine air layer, the flame retardant and heat shielding effects are brought about.

Hereinafter, the present invention will be described in detail by way of examples. The following examples are merely illustrative of the present invention, but the scope of the present invention is not limited to the following examples.

Preparation of Flame Retardant Adhesives

A flame-retardant adhesive was prepared in the blending parts shown in Table 1.

Ingredient Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Magnesium hydroxide 3 0.5 0.5 0.5 0 0.5 3 Feldspar 10 10 10 10 10 10 7 zeolite 18 18 13.5 18 18 18 18 Sodium Silicate 70 70 70 56 70 70 70 Melamine cyanurate  2  2  2  2  2  0.1  2

Flame retardancy, heat shield, adhesion test

Test method for measuring the adhesion, flame retardancy, heat shielding properties of the flame retardant adhesive prepared in the compounding amount of Table 1 are as follows.

When the flame-retardant adhesive composition was applied to a 5 mm thick plywood (200 ~ 300 g / ㎡) for the test piece for the adhesion test, laminated 5 sheets of plywood and dried, and then throwing the 25 mm thick plywood prepared on the floor Adhesiveness was tested by dropping of the plywood.

Specimens for flame retardancy test were prepared by the same method as the above-mentioned adhesive specimen manufacturing method, and then applied by flame while meeting the temperature conditions in the furnace specified in KS F2257-1 (Test method for fire resistance of building structural members) in a simple fire resistance test furnace. The test was performed by measuring the time when a hole was formed and the flame passed. The flame passing test was based on 60 minutes, and the flame retardancy evaluation criteria were used. The flame retardancy effect was excellent when the fire retardancy was 60 minutes or more, and the flame retardant effect was poor when the fire resistance was 60 minutes or less.

 The specimen for thermal insulation test is manufactured by the same method as the above-mentioned adhesive specimen production method, and then, in a simple fire resistance test furnace, flame is applied while meeting the temperature conditions in the furnace specified in KS F2257-1 (Test method for the fire resistance of building structural members). The temperature on the back of the flame was measured using a thermograph. The evaluation criteria for the back surface temperature were evaluated according to the back surface temperature standard specified in KS F2257-1 (if the average elevated temperature of the non-heated surface is above 140 ° C or the maximum rise temperature is above 180 ° C, the thermal insulation is failed).

Table 2 below shows the adhesion, flame retardancy, and heat shield test results of the flame retardant adhesives prepared in the compounding amounts of Table 1.

Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Adhesive Good Anho Good Bad Good Good Good Flame Pass 72 minutes 65 minutes 51 minutes 67 minutes 67 minutes 47 minutes 56 minutes Back temperature (℃) 89 142 146 150 215 152 114

Analyzing the test results of Table 2 above, when melamine cyanurate and magnesium hydroxide, zeolite, feldspar, and sodium silicate were used in certain parts by weight, that is, 2 parts by weight of melamine cyanurate, 3 parts by weight of magnesium hydroxide, and feldspar 10 In the case of Example 1 using 18 parts by weight, 18 parts by weight of zeolite and 70 parts by weight of sodium silicate, the best results were obtained in terms of adhesion (good), flame retardancy (72 minutes), and heat shielding (back temperature 89 ° C.).

In Example 2, when the magnesium hydroxide parts were reduced compared to Example 1, the flame passage time was shortened to 65 minutes, and the back temperature was also increased to 142 ° C., which means that the magnesium hydroxide is used above a certain weight ratio. It can be seen that it is preferable.

In particular, in the case of Example 5, when only magnesium hydroxide was not added to the flame-retardant adhesive composition compared to Example 1, it can be seen that the back temperature rapidly rises to 215 ° C as a result of the test. It can be seen that it plays a leading role, and also has a secondary effect on the flame retardant synergistic effect. Therefore, in the present invention, it is preferable to use 0.5 to 5 parts by weight of the magnesium hydroxide in the flame-retardant adhesive composition.

When comparing the weight of the zeolite in the flame retardant adhesive composition in Example 2 and Example 3 from 18 parts by weight to 13.5 parts by weight, the flame passage time is shortened from 65 minutes to 51 minutes, it can be seen that the flame retardancy is sharply reduced. The temperature is also increased from 142 ℃ to 146 ℃ it can be seen that the heat shielding effect is also reduced. Therefore, it is preferable to use 18 weight part or more by weight of zeolite in a flame-retardant adhesive composition.

When Example 2 and Example 4 were compared to reduce the weight of sodium silicate in the flame retardant adhesive composition from 70 parts by weight to 56 parts by weight, poor adhesion was observed, and the back temperature was also increased from 142 ° C. to 150 ° C. It can be seen that the effect is also reduced. Therefore, it is preferable to use 60-75 weight part of weight parts of silica in a flame-retardant adhesive composition. When more than 75 parts by weight is used is poor adhesion, it is not preferable as the drying time is long.

When comparing the weight of the melamine cyanurate in the flame retardant adhesive composition from Example 2 to Example 6 from 2 to 0.1, the flame passage time rapidly decreased from 65 minutes to 47 minutes, showing a poor flame retardant effect. In addition, it can be seen that the back temperature is also increased from 142 ° C. to 152 ° C., so that the heat shielding effect is also reduced. Therefore, the melamine cyanurate in the flame retardant adhesive composition is preferably used in an amount of 0.1 parts by weight or more, and preferably 5 parts by weight or less due to the high cost.

When Example 7 compared with Example 1, when the feldspar weight ratio in the flame retardant adhesive composition was reduced from 10 parts by weight to 7 parts by weight, the flame passage time was decreased from 72 minutes to 56 minutes, and the flame retardant effect was poor. It can be seen that the heat shielding effect is also reduced by increasing from 89 ° C to 114 ° C. Therefore, it is preferable to use 7 parts by weight or more by weight of leadstone in the flame-retardant adhesive composition.

Table 3 below is a table showing the blending amount of the optimum Example 1 and Comparative Example of the present invention and the results of the adhesion, flame retardancy, and thermal insulation test results.

Example 1 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Comparative Example 6 Magnesium hydroxide 3 - 30 - 3 3 Feldspar 10 30 - - 10 10 zeolite 18 - - 30 18 18 Sodium Silicate 70 56 70 70 70 70 70 Melamine cyanurate  2  2  2  2  -  -  2 Triphenyl phosphate  -  -  -  -  -  2  - Adhesive Good Bad Good Good Good Good Good Flame Pass 72 minutes 65 minutes 43 minutes 71 minutes 45 minutes 54 minutes 40 minutes Back temperature (℃) 89 225 159 268 160 154 300

Table 3 shows that in the case of using only one of the magnesium hydroxide, feldspar, and zeolite in the flame-retardant adhesive composition of the present invention (Comparative Examples 1, 2, 3), even if the weight ratio is increased, compared with the case of using both magnesium hydroxide, feldspar, and zeolite The flame retardant effect and heat shielding effect were greatly reduced. However, in the case of Comparative Example 3, the flame retardant effect did not show a large difference compared to Example 1, but the heat shielding effect is greatly reduced, it can be seen that magnesium hydroxide and feldspar have a large heat shielding effect.

In addition, when compared with Example 1 and Comparative Example 2, when the lead-free and zeolite is not used, the flame retardant effect and heat shielding effect is greatly reduced, so that the lead-stone and zeolite play an important role in the flame retardant synergistic effect and heat shielding effect. Able to know.

In addition, in the case of Comparative Example 4, the flame retardant effect and the heat shielding effect was significantly reduced compared to the case of using the inorganic flame retardant when the melamine cyanurate is not used, in the case of Comparative Example 6 melamine cyanurate alone In case of mixing with inorganic flame retardant, the flame retardant effect and heat shielding effect are significantly reduced compared to the case of mixing with inorganic flame retardant. I can see it coming.

In addition, when using the flame retardant triphenyl phosphate (triphenyl phosphate) instead of using the melamine cyanurate as an organic flame retardant compared to Example 1 and Comparative Example 5 compared to the use of melanin cyanurate, the flame retardant effect and heat shielding effect The results were greatly reduced.

And when the content of sodium silicate was used in less than 60 parts by weight showed poor adhesion.

Therefore, the present invention was able to bring excellent heat shielding effect and flame retardant synergistic effect by using melamine cyanurate (melamine cyanurate) as an organic flame retardant, mixed with a lead, magnesium hydroxide, zeolite as an inorganic flame retardant, non-halogen-based In addition, the use of non-antimony flame retardants can bring environmentally friendly effects.

In addition, the method for preparing a flame retardant adhesive composition of the present invention is characterized in that the inorganic flame retardant is first added to and mixed with sodium silicate, followed by stirring and mixing by adding an organic flame retardant. The flame-retardant adhesive prepared in this way did not cause any problems during stirring mixing and showed a storage stability of 7 days or more. On the other hand, when a flame retardant adhesive is prepared by adding and mixing an organic flame retardant with sodium silicate and then stirring and mixing an inorganic flame retardant, the prepared flame retardant adhesive becomes a gel and has a fluidity, and thus the flame retardancy in a mixing tank is reduced. The problem of difficult transfer during adhesive transfer occurred. Therefore, the method for preparing a flame retardant adhesive composition of the present invention is characterized by being prepared by stirring and mixing magnesium hydroxide, zeolite and leadstone with sodium silicate as an inorganic flame retardant and then adding melamine cyanurate with an organic flame retardant to stir-mix.

Claims (5)

delete Flame retardant adhesive composition comprising 0.1 to 5 parts by weight of melamine cyanurate as an organic flame retardant, and 22 to 50 parts by weight of a mixture of magnesium hydroxide, lead stone and zeolite and 60 to 75 parts by weight of sodium silicate as an inorganic flame retardant. . delete 0.1 to 5 parts by weight of melamine cyanurate as an organic flame retardant and 0.5 to 5 parts by weight of magnesium hydroxide, 7 to 15 parts by weight of leadstone, 15 to 30 parts by weight of zeolite and 60 to 75 parts by weight of sodium silicate as an inorganic flame retardant. Flame retardant adhesive composition, characterized in that. The method for producing the flame retardant adhesive composition according to claim 2 or 4, wherein the inorganic flame retardant is first added to and mixed with sodium silicate, followed by stirring and mixing, followed by stirring and mixing of the organic flame retardant.