KR101368864B1 - Method for producing a foam sheet with flame-retardant silicon composition - Google Patents

Abstract

The present invention is a liquid type liquid silicone resin 20-40kg, 3-glycidoxypropyl) trimethoxy silane (specific gravity 1,06kg / m 3) which is any compound selected from polydimethylsiloxane, polydimethylsilanol, methylhydrogenpolysiloxane or methylphenylsiloxane. 1 to 10 kg, aluminum hydroxide 20 to 30 kg, bromine compound 25 to 35 kg, antimony trioxide 10 kg, ester phosphate 5 kg, benzotriazole type, benzophenol, sultin ester, hindered amine selected from any one of 1 The present invention relates to a foam sheet manufacturing method using a flame retardant silicone composition of ˜5 kg.

Description

Method for producing foam sheet using flame retardant silicone composition {Method for producing a foam sheet with flame-retardant silicon composition}

The present invention is to impregnate the foam having a continuous bubble structure in the impregnated tank containing the flame-retardant silicone composition by mixing the advantages of the foam and the characteristics of the flame-retardant silicone composition high elasticity heat resistance processability waterproof weather resistance, heat insulation, flame resistance, resilience, The present invention relates to a foam sheet manufacturing method using a flame retardant silicone composition which can be used in all industrial fields by improving high elongation, high tensile and non-oil properties .

In general, foams having a combustion bubble structure used as interior materials of buildings or vehicles fall in heat resistance, flame resistance, weather resistance, oil resistance, acid resistance, elasticity, and elongation compared to close cell foams and are subject to temperature changes (over 130 ° C). It is fragile and easily shrinks or hardens the surface, and after a certain period of time, it causes quality deterioration due to material deformation (tensile strength, tear strength flexibility, insulation, sound absorption, hygroscopicity) due to natural weathering scattering phenomenon.

For this reason, a cloth film aluminum foil nonwoven fabric or the like is used on urethane foam and foam surface. The use of non-ventilated skin material does not allow for the inherent sound absorption, elasticity and flexibility of urethane foams and foams.

Various technical developments have been attempted to solve this problem.

For example, Korean Laid-Open Patent Publication No. 1020060060294 (20060605) is characterized in that a polyurethane sponge is impregnated with a functional silicone solution consisting of silver-natural mineral powder, silver-iodine plated activated carbon, siloxane, and an organic solvent. Functional silicone sponges and manufacturing methods are disclosed,

Korean Patent Publication No. 1010497560000 (20110711) has a high density (10 ~ 50kg / m3) and high compressive strength (1.25 ~ 2.54 kg / cm2) of the properties on the surface of the pallet made of EPS, urethane foam, PP, PE High strength and high compressive strength to ensure durability by applying liquid polymer resin (Polyurethane, Polyurea, Polyurethane-Polyurea) after curing to prevent damages such as cracks caused by load during loading and unloading of goods and damages during handling Surface loading composition for EPS, urethane foam, PP, PE pallet coating material for achieving low specific gravity is described,

Korean Patent Publication No. 1009959530000 (20101116) has a high-density elastic member and a low-density elastic member which are manufactured by using a polyurethane elastic member to form a wall shape inserted into a heel portion of a shoe using a polyurethane elastic member. In the state of impregnating each of the other liquid silicone rubber, a technique related to a wall mold inserted to form a heel portion of a shoe that is formed by heating and compressing them in an overlapping state together with surface paper and applying it as a wall shape of a shoe is disclosed.

Registered Utility Model Registration No. 2003965150000 (20050914) in Korea is characterized in that the coating layer is formed by spraying the surface treatment solution and magnesium oxide solution while passing through the multi-stage roller after impregnating and piercing the pretreatment solution in the styrofoam panel. Flame retardant styrofoam panel is open to the public,

Korean Laid-Open Patent Publication No. 1020110131294 (20111206) is a resin foam comprising a resin and a flame retardant component, characterized in that the flame retardant component is a polysiloxane-coated flame retardant. In addition, it can be seen that the polysiloxane-coated flame retardant is a polysiloxane-coated metal hydroxide, and a flame-retardant resin foam having a content of the polysiloxane-coated metal hydroxide in a resin foam of 30 to 60% by weight is disclosed.

1. Domestic Publication No. 1020060060294 (20060605) 2. Korean Patent Publication No. 1020110131294 (20111206) 3. National Registered Patent Publication No. 1010497560000 (20110711) 4. National Registered Patent Publication No. 1009959530000 (20101116) 5. Registered Utility Model Registration No. 2003965150000 (20050914) in Korea

Conventional foams are lower than these close cell foams such as heat resistance, flame resistance, weather resistance, oil resistance, acid resistance, water resistance, elasticity, and elongation, and are easily shrunk or surface hardened due to temperature changes (over 130 ° C). After this, natural weathering scattering causes material deformation and deterioration.

For this reason, a cloth film aluminum foil nonwoven fabric or the like is used on urethane foam and foam surface. In case of using non-ventilated skin material, the inherent sound absorption, elasticity and flexibility of urethane foam and foam cannot be used.

In addition, the product coated with urethane liquid mixed with urethane liquid and flame retardant aid on the surface by absorbing 1-5mm on the surface of urethane was invented and used. It is not suitable for excavator engine room, bus engine room, forklift engine room, generator sound absorption and heat insulation which require long time, acid resistance, weather resistance, hygroscopicity and heat resistance.

Silicone foam was required for high-quality sheets that required elasticity and rebound cushion durability for a long time, but due to the high price and deterioration of foaming technology, it was impossible to produce the thickness and width required by consumers. The present invention is to solve the problem of the present invention to find an impregnation solution having both the advantages of urethane foam and silicone foam by impregnating the urethane foam with a silicone mixture composition (silicone mixture and flame retardant mixture mixture).

In order to solve this problem, the properties of urethane foams and foams have the properties of flame retardant silicone compositions (high elasticity, heat resistance, processability, water resistance, weather resistance, chemical resistance, heat insulation, restorability, high elongation, non-oil resistance) To implement at the same time,

By supplying a sheet made of foam such as urethane foam to an impregnated tank containing a flame retardant silicone composition, impregnating the foam with a flame retardant silicone composition so as to coat, penetrate or both, so that the silicone resin has sound absorption performance of the urethane foam and foam. It is a problem solving means to achieve the present invention to provide a foam sheet manufacturing method using a flame-retardant silicone composition that can combine the physical, chemical, and mechanical advantages it has.

The present invention is a high elasticity heat resistance, processability, waterproofness, weather resistance, chemical resistance, resilience, high elongation, high tensile resistance, non-oil resistance, flame retardancy, which is a physical property of the silicone resin by the silicone mixture composition that is effectively penetrated or coated inside the urethane foam It appears that the foam sheet is to be applied to a variety of industries.

The present invention is a liquid type liquid silicone resin 20-40kg, 3-glycidoxypropyl-trimethoxysilane (specific gravity 1,06kg / m3) 1 which is any compound selected from polydimethylsiloxane, polydimethylsilanol, methylhydrogenpolysiloxane or methylphenylpolysiloxane. Flame retardant which is any compound selected from ˜10 kg, aluminum hydroxide 20-30 kg, bromine compound 25-35 kg, antimony trioxide 10 kg, ester phosphate 5 kg, benzotriazole-based, benzophenol, sulfinate, hindered amine It relates to a foam sheet manufacturing method using a flame retardant silicone composition of 1 to 5 kg auxiliary.

The aluminum hydroxide of the present invention is known to escape the crystal water at about 200-300 ℃ when heated to obtain a flame retardant effect on the endothermic action and the incombustibles, less harmful gases during combustion, low smoke, high stability.

In the present invention, 20 to 30 kg was used.

The bromine compound produces a non-combustible gas by thermal decomposition to cover the surface of the polymer to prevent ignition and dilute the combustible gas to reduce the combustibility.

Phosphoric acid is generated during the combustion of ester phosphate to form a protective film of non-volatile line, thereby blocking oxygen.

In the present invention, 25 to 35 kg was used.

Antimony trioxide, when reacted with antimony trioxide, such as lean acid compounds, aluminum hydroxide, and bromine compounds, is highly flame retardant and has a synergistic effect of breaking the combustion chain.

In the present invention, 10 kg was used.

The present invention is capable of performing both a roll operation and a plate state, and considering the technical aspect of absorbing the flame-retardant silicone composition from the surface to the urethane internal bubble structure, the foamed sheet has the characteristics of the flame-retardant silicone composition which has high sound absorption performance and breakthrough flame retardancy. Appeared in.

It is formed by mixing inorganic flame retardant, flame retardant adjuvant, admixture and solvent in liquid type silicone compound to form one stage and dipping urethane foam in dipping tank which is two stage to compress through roller. When passed through and dried, it becomes a complete product and at the same time solves the high elasticity, heat resistance, processability, waterproofness, weather resistance, chemical resistance, restorability, high elongation, high tensile strength, non-oil resistance effect and flame resistance of silicone resin in urethane foam bubble structure. It is a method of manufacturing a breakthrough completely urethane foam + flame retardant silicone composition impregnated (silox foam) foam sheet.

The present invention is the liquid type to be impregnated 20 ~ 40kg, 3-glycidoxypropyl-trimethoxysilane (specific gravity 1,06kg / m3) 1 ~ 10㎏, aluminum hydroxide 20 ~ 30kg, bromine compound 25 ~ 35㎏, antimony trioxide 10㎏ , 5 kg of ester phosphate, 1 to 5 kg of flame retardant adjuvant (benzotriazole type, benzophenol type, sulfinate ester, hindered amine) were mixed to prepare 200 kg of flame retardant compound, and two-component silicone mixture (viscosity 25 ℃ mpa) .s50000 ± 20000) is mixed and solvent (toluene) 300kg flame retardant compound 1: silicon compound 2 ~ 3: solvent 1 ~ 2 ratio to prepare final flame retardant silicone composition.

After impregnating the foam through the dipping tank, the final flame-retardant silicone composition is compressed, and then 20 to 80% of the flame retardant silicone composition is absorbed into the foam sheet through a roller, and then dried to absorb the flame retardant silicone composition into the foam. The present invention relates to a foam sheet manufacturing method of a urethane + flame retardant silicone composition (silicon foam).

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

Example 1

First step

20 kg of polydimethylsiloxane and 1 kg of 3-glycidoxypropyl-trimethoxysilane (1,06 kg / m3 specific gravity) were added to a stirrer and mixed at a rotation of RPM 200 to prepare a silicone mixture.

Second Step

20 kg of aluminum hydroxide, 25 kg of bromine compound, 10 kg of antimony trioxide, 5 kg of ester phosphate, and 1 kg of benzotriazole were mixed and mixed in a stirrer to prepare a flame retardant mixture by mixing with rotation of RPM 200.

Third step

The silicone mixture prepared in the first step and the flame retardant mixture prepared in the second step were mixed and introduced into a stirrer to prepare a flame retardant silicone composition by rotation of RPM 200.

Fourth step

After impregnating the foam sheet into the impregnated tank containing the flame-retardant silicone composition prepared as described above at a speed of 10 m / h, the flame-retardant silicone composition of 500g-4kg per square meter according to the thickness of the foam surface by passing between two compression rollers After penetrating from the inside of the air layer, and dried for 30 minutes at 150 ℃ to prepare a foam sheet using a flame-retardant silicone composition .

Example 2

First step

40 kg of methylhydrogenpolysiloxane and 10 kg of 3-glycidoxypropyl-trimethoxysilane (1,06 kg / m3 in specific weight) were mixed and mixed in a stirrer to prepare a silicone mixture.

Second Step

30 kg of aluminum hydroxide, 35 kg of bromine compound, 10 kg of antimony trioxide, 5 kg of ester phosphate, and 5 kg of hindered amine were mixed and mixed in a stirrer to prepare a flame-retardant mixture by mixing with rotation of RPM 200.

Third step

The silicone mixture prepared in the first step and the flame retardant mixture prepared in the second step were added to a stirrer and mixed in a rotation of RPM 200 to prepare a flame retardant silicone composition.

Fourth step

The flame-retardant silicone composition prepared as described above is injected into the upper rollers of the two upper and lower compression rollers to inject the flame-retardant silicone composition from the upper roller into the foam sheet introduced at a speed of 10 m / h and simultaneously by the compression of the lower compression roller. It was coated on the surface and partially penetrated into the foam sheet, and then dried at 150 ° C. for 30 minutes to prepare a foam sheet using a flame retardant silicone composition .

Example 3

First step

20 kg of polydimethylsiloxane and 1 kg of 3-glycidoxypropyl-trimethoxysilane (1,06 kg / m3 specific gravity) were added to a stirrer and mixed at a rotation of RPM 200 to prepare a silicone mixture.

Second Step

20 kg of aluminum hydroxide, 25 kg of bromine compound, 10 kg of antimony trioxide, 5 kg of ester phosphate, and 1 kg of benzotriazole were mixed and mixed in a stirrer to prepare a flame-retardant mixture by mixing with rotation of RPM 200.

Third step

The silicone mixture prepared in the first step and the flame retardant mixture prepared in the second step were mixed and introduced into a stirrer to prepare a flame retardant silicone composition by rotation of RPM 200.

Fourth step

After impregnating the foam sheet into the impregnated tank containing the flame-retardant silicone composition prepared as described above at a speed of 10 m / h, the flame-retardant silicone composition of 500g-4kg per square meter according to the thickness of the foam surface by passing between two compression rollers After penetrating from the inside of the air layer, and dried for 30 minutes at 150 ℃ to prepare a foam sheet using a flame-retardant silicone composition .

Example 4

First step

40 kg of methylhydrogenpolysiloxane and 10 kg of 3-glycidoxypropyl-trimethoxysilane (1,06 kg / m3 in specific weight) were mixed and mixed in a stirrer to prepare a silicone mixture.

Second Step

30 kg of aluminum hydroxide, 35 kg of bromine compound, 10 kg of antimony trioxide, 5 kg of ester phosphate, and 5 kg of hindered amine were mixed and mixed in a stirrer to prepare a flame retardant mixture by mixing with rotation of RPM 200.

Third step

The silicone mixture prepared in the first step and the flame retardant mixture prepared in the second step were added to a stirrer and mixed in a rotation of RPM 200 to prepare a flame retardant silicone composition.

Fourth step

The flame-retardant silicone composition prepared as described above is injected into the upper rollers of the two upper and lower compression rollers to inject the flame-retardant silicone composition from the upper roller into the foam sheet introduced at a speed of 10 m / h and simultaneously by the compression of the lower compression roller. It was coated on the surface and partially penetrated into the foam sheet, and then dried at 150 ° C. for 30 minutes to prepare a foam sheet using a flame retardant silicone composition .

Flame-retardant silicone composition prepared as described above is a liquid type liquid silicone resin 20 ~ 40kg, 3-glycidoxypropyl) trimethoxy silane (specific gravity) of any compound selected from polydimethylsiloxane, polydimethylsilanol, methylhydrogenpolysiloxane or methylphenylsiloxane 1,06kg / ㎥) 1-10kg, aluminum hydroxide 20-30kg, bromine compound 25-35kg, antimony trioxide 10kg, ester phosphate 5kg, benzotriazole, benzophenol, sultin ester, hindered amine It can be seen that any one flame retardant aid is composed of 1 ~ 5kg.

Experimental Example 1

Thickness 10mm The general urethane foam sheet was compressed after 60 hours by compressing the thickness through the KSM 6672 test method.

Experimental Example 2

Thickness 10mm The foam sheet prepared in Example 1 was compressed after the thickness of 60 mm through the KSM 6672 test method, and as a result, 2% was deformed.

Experimental Example 3

Thickness 10mm The urethane foam sheet was compressed by repeated repeated 89,000 times through the KSM 6672 test method, resulting in 21% shrinkage.

Experimental Example 4

Thickness 10mm The foam sheet prepared in Example 1 was repeatedly compressed for 89,000 times through the KSM 6672 test method, and the shrinkage was 2%.

Experimental Example 5

Ten-mm-thick foam sheets made of urethane foam were cut at 95% elongation as a result of measuring elongation (extension) through KSM 7214, ISO Standard 2006 test method.

Experimental Example 6

Thickness of 10mm The foam sheet prepared in Example 1 was cut at 210% in an elongation state as a result of measuring the elongation (extension) through the KSM ISO 7214 standard test method.

Experimental Example 7

The thickness of 10mm thick urethane foam sheet was measured at 10,7 / Ncm as a result of measuring the strength of the tearing force of the material through the KSM 6518 (tear strength) test method.

Experimental Example 8

Thickness 10mm The foam sheet prepared in Example 1 was measured at 46.7 N / cm as a result of measuring the strength of the tearing force of the material through the KSM 6518 (tear strength) test method.

Experimental Example 9

The thickness of 10mm thick urethane foam sheet was measured by the KSM ISO 7214 standard (tensile strength) test method.

Experimental Example 10

Thickness of 10mm The foam sheet prepared in Example 1 was measured by KSM ISO 7214 standard (tensile strength) test method, the strength of the breaking force of the material was measured, the test piece was broken at 84 N / ㎠.

Experimental Example 11

Ten-mm-thick foam sheet made of general urethane foam was measured by KSM 3802 test method (heating dimension change), and after 2 hours heating at 130 ° C, the dimensional change was -0.7%.

Test Example 12

Thickness of 10mm The foam sheet prepared in Example 1 was measured by KSM 3802 test method (heating size change) after heating at 130 ° C. for 2 hours, and no change occurred.

Experimental Example 13

The thickness of 10mm thick urethane foam sheet was measured by immersion of hydraulic fluid at room temperature for 24 hours through the KSM 3015 test method (oil resistance).

Experimental Example 14

Thickness of 10mm The foam sheet prepared in Example 1 was subjected to KSM 3802 test method (oil resistance), and the hydraulic fluid was immersed at room temperature for 24 hours, and there was no abnormality as a result of measuring deformation.

Experimental Example 15

The thickness of 10mm thick urethane foam sheet was put into the test chamber of Hyundai Motor's heat resistance test (lab) and heated at 150 ℃ for 8 hours.

Experimental Example 16

10 mm thick The foam sheet prepared in Example 1 was placed in a test furnace of the test specimen of the Hyundai Motors (Laboratory), and then heated at 180 ° C. for 10 hours.

Experimental Example 17

The thickness of 13mm thick urethane foam sheet was measured by the UL94 horizontal burning test (the time until the fire was removed after the fire was put on the specimen for 10 seconds with the burner removed and the specimen was turned off). The fire was extinguished and ignited on cotton wool below 30 cm by a fire that melted during combustion.

Experimental Example 18

13 seconds thick The foam sheet prepared in Example 1 was measured by the UL94 horizontal burning test (the time until the fire was removed after the fire was put on the specimen with a burner for 10 seconds and the specimen was turned off). The lights went out and no sparks occurred.

As described above, it was confirmed that the foam sheet of the present invention is a foam sheet having good or improved physical properties such as mechanical, physical, chemical change, and flame retardancy than conventional foam sheets.

Claims (4)

delete delete In the foam sheet manufacturing method using a flame-retardant silicone composition,
20 to 40 kg of liquid type liquid silicone resin, 3-glycidoxypropyl-trimethoxysilane (1,06 kg / m3 specific gravity), which is any compound selected from polydimethylsiloxane, polydimethylsilanol, methylhydrogenpolysiloxane or methylphenylpolysiloxane After mixing the mixture into a stirrer to mix at a rotation of RPM 200 to prepare a silicone mixture,
Flame retardant adjuvant 1-5, which is any one compound selected from aluminum hydroxide 20-30 kg, bromine compound 25-35 kg, antimony trioxide 10 kg, ester phosphate 5 kg, benzotriazole, benzophenol, sultin acid ester, and hindered amine. ㎏ mixed with the stirrer and mixed in a rotation of RPM 200 to prepare a flame retardant mixture,
After mixing the silicone mixture and the flame retardant mixture prepared above was added to the stirrer to rotate at RPM 200 to produce a flame-retardant silicone composition,
After impregnating the foam sheet into the impregnated tank containing the flame-retardant silicone composition prepared as described above at a speed of 10 m / h, the flame-retardant silicone composition of 500g-4kg per square meter according to the thickness of the foam surface by passing between two compression rollers Method of manufacturing a foam sheet using a flame-retardant silicone composition, characterized in that to penetrate from the inside of the air layer, and then dried for 30 minutes at 150 ℃. In the foam sheet manufacturing method using a flame-retardant silicone composition,
20 to 40 kg of liquid type liquid silicone resin and 3-glycidoxypropyl-trimethoxysilane (specific gravity 1,06 kg / m3) 1 to 10 kg of any compound selected from polydimethylsiloxane, polydimethylsilanol, methylhydrogenpolysiloxane or methylphenylpolysiloxane After mixing the mixture into a stirrer to mix at a rotation of RPM 200 to prepare a silicone mixture,
Flame retardant adjuvant 1-5, which is any one compound selected from aluminum hydroxide 20-30 kg, bromine compound 25-35 kg, antimony trioxide 10 kg, ester phosphate 5 kg, benzotriazole, benzophenol, sultin acid ester, and hindered amine. ㎏ mixed with the stirrer and mixed in a rotation of RPM 200 to prepare a flame retardant mixture,
After mixing the silicone mixture and the flame retardant mixture prepared above was added to the stirrer to rotate at RPM 200 to produce a flame-retardant silicone composition,
The flame-retardant silicone composition prepared as described above is injected into the upper rollers of the two upper and lower compression rollers to inject the flame-retardant silicone composition from the upper roller into the foam sheet introduced at a speed of 10 m / h and simultaneously by the compression of the lower compression roller. Method of manufacturing a foam sheet using a flame-retardant silicone composition characterized in that the coating is coated on the surface and partly penetrated into the foam sheet, and then dried at 150 ° C. for 30 minutes.