KR20140083360A - Flame-retarded thermal insulating foam of chemical cross-linked polyvinyl chloride based and manufacturing method of the same - Google Patents
Flame-retarded thermal insulating foam of chemical cross-linked polyvinyl chloride based and manufacturing method of the same Download PDFInfo
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- KR20140083360A KR20140083360A KR1020120153019A KR20120153019A KR20140083360A KR 20140083360 A KR20140083360 A KR 20140083360A KR 1020120153019 A KR1020120153019 A KR 1020120153019A KR 20120153019 A KR20120153019 A KR 20120153019A KR 20140083360 A KR20140083360 A KR 20140083360A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
- B29C44/34—Auxiliary operations
- B29C44/36—Feeding the material to be shaped
- B29C44/46—Feeding the material to be shaped into an open space or onto moving surfaces, i.e. to make articles of indefinite length
- B29C44/50—Feeding the material to be shaped into an open space or onto moving surfaces, i.e. to make articles of indefinite length using pressure difference, e.g. by extrusion or by spraying
- B29C44/505—Feeding the material to be shaped into an open space or onto moving surfaces, i.e. to make articles of indefinite length using pressure difference, e.g. by extrusion or by spraying extruding the compound through a flat die
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0012—Combinations of extrusion moulding with other shaping operations combined with shaping by internal pressure generated in the material, e.g. foaming
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0019—Use of organic additives halogenated
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- C08J9/0014—Use of organic additives
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
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- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
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- C08J9/103—Azodicarbonamide
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- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0025—Crosslinking or vulcanising agents; including accelerators
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- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/26—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
- C08L23/28—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment by reaction with halogens or compounds containing halogen
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- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2027/00—Use of polyvinylhalogenides or derivatives thereof as moulding material
- B29K2027/06—PVC, i.e. polyvinylchloride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
- B29K2105/04—Condition, form or state of moulded material or of the material to be shaped cellular or porous
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
- B29K2105/24—Condition, form or state of moulded material or of the material to be shaped crosslinked or vulcanised
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
- B29K2995/0012—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds having particular thermal properties
- B29K2995/0015—Insulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
- B29K2995/0012—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds having particular thermal properties
- B29K2995/0016—Non-flammable or resistant to heat
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- C08J2201/00—Foams characterised by the foaming process
- C08J2201/02—Foams characterised by the foaming process characterised by mechanical pre- or post-treatments
- C08J2201/026—Crosslinking before of after foaming
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- C—CHEMISTRY; METALLURGY
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- C08J2201/00—Foams characterised by the foaming process
- C08J2201/02—Foams characterised by the foaming process characterised by mechanical pre- or post-treatments
- C08J2201/03—Extrusion of the foamable blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
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- C08J2323/28—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment by reaction with halogens or halogen-containing compounds
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- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
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- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
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Abstract
Description
More particularly, the present invention relates to a chemically crosslinked polyvinyl chloride-based flame retardant foamed insulation material which can be used as a heat insulating material for construction due to excellent heat insulating property through production of a high-expansion foam, and a process for producing the same will be.
From the viewpoint of efficient use and conservation of energy, the development and effective use of the insulation material is also very important. Currently, insulating materials are largely classified into organic polymer resin and inorganic materials, and their utilization methods are also changed depending on their physical properties and properties. Generally, organic insulation has better heat insulation, lighter weight, water resistance, processability and impact resistance than inorganic insulation, but is less resistant to heat or durability. Therefore, when multifunctional insulation materials complementary to each characteristic are developed, the limitation of the use range can be greatly alleviated and new applications can be realized.
On the other hand, the polyvinyl chloride (PVC) foam is a new functional insulation material which is further improved in heat resistance, low temperature resistance, chemical resistance and mechanical strength in addition to the general characteristics of the organic insulation material. Which is an organic insulating material capable of exerting an effect. Therefore, such crosslinked polyvinyl chloride-based foam is widely used as a single structural material in various industries such as housing, construction, refrigeration, freezing, LNG storage tanks, aircraft, and ships, and its application is continuously developed. It is a product that is being done.
In particular, when a fire occurs in a building, it causes damage due to smoke or gas generated during combustion. As the combustion becomes active, oxygen around the area becomes insufficient and harmful gas is generated. The smoke generated by incomplete combustion is a large amount of human injury Can be generated. Therefore, it is required that the heat insulating material for construction has excellent flame retardancy in order to minimize the occurrence of a risk factor in the event of a fire. Polyvinyl chloride contains chlorine, which is a flame retardant element, and is basically excellent in flame retardancy.
On the other hand, since the air existing inside the foam insulating material blocks the heat loss by preventing the heat from entering and leaving, the more the pores are contained therein, the better the heat insulating property. In order to form a lot of pores inside the foam insulation, it is necessary to foam at a high magnification. However, the conventional polyvinyl chloride-based foam insulation has a low degree of crosslinking and is difficult to foam at a high magnification, which makes it difficult to secure a certain level of heat insulation.
A problem to be solved by the present invention is to provide a chemically crosslinked polyvinyl chloride-based flame retardant foamed insulation material which is improved in heat insulation due to foaming at a high magnification while maintaining excellent flame retardancy, and a method for producing the same.
According to an aspect of the present invention, there is provided a resin composition comprising 30 to 70 parts by weight of a polyvinyl chloride (PVC) resin and 30 to 70 parts by weight of a chlorinated polyethylene (CPE) resin; 10 to 100 parts by weight of chlorinated paraffin oil (CPO) based on 100 parts by weight of the resin mixture; And 1 to 10 parts by weight of a crosslinking agent is extrusion-foam-molded into a chemical crosslinked polyvinyl chloride-based flame retardant foamed insulation material.
The chlorinated paraffin oil (CPO) may be 20 to 80 parts by weight based on 100 parts by weight of the resin mixture.
The crosslinking agent may be 2 to 5 parts by weight based on 100 parts by weight of the resin mixture.
The cross-linking agent may be at least one selected from the group consisting of dicumyl peroxide (DCP), t-butyl peroxylaurate, t-butyl peroxyisopropyl carbonate, benzoyl peroxide, t-butyl peroxyacetate, Butyl peroxide, cyclohexanone peroxide, t-dibutyl peroxymaleic acid, t-butyl hydroperoxide, 2,3-dimethyl-2,5-dihexane, di- 3-bisbenzene, 1,1-bis-3,3,5-trimethylcyclohexane, p-chlorobenzoyl peroxide, 2,4-dichlorobenzoyl peroxide, or at least two Lt; / RTI >
The limiting oxygen index of the chemically crosslinked polyvinyl chloride-based flame retardant foamed insulation material may be 28 or more.
The density of the chemically crosslinked polyvinyl chloride-based flame retardant foamed insulating material may be 0.025 g / cm 3 to 0.500 g / cm 3 .
The thermal conductivity of the chemically crosslinked polyvinyl chloride-based flame retardant foamed insulation material may be 0.04 W / mK or less.
On the other hand, the raw material composition may contain 5 to 50 parts by weight of a flame retardant based on 100 parts by weight of the resin mixture; And 1 to 5 parts by weight of a heat stabilizer.
Here, the flame retardant may be any one selected from the group consisting of antimony trioxide, decabromophenyl oxide, and magnesium hydroxide, or a mixture of two or more thereof.
The heat stabilizer may be any one selected from the group consisting of tin maleate, tin laurate, and powder tin maleate esters, or two or more of them.
(S1) 30 to 70 parts by weight of a polyvinyl chloride (PVC) resin and 30 to 70 parts by weight of a chlorinated polyethylene (CPE) resin, 100 parts by weight of the resin mixture From 10 to 100 parts by weight of chlorinated paraffin oil (CPO), from 1 to 10 parts by weight of a crosslinking agent, from 5 to 50 parts by weight of a flame retardant, from 1 to 5 parts by weight of a heat stabilizer, from 5 to 50 parts by weight of a foaming agent, Kneading the mixture to prepare a raw material composition; (S2) injecting the raw material composition into an extruder and melt-extruding the extruded material to produce an extruded sheet; And (S3) heating the extruded sheet to chemically crosslink and foaming the foaming agent to form a foamed body. The present invention also provides a method for producing a chemically crosslinked polyvinyl chloride-based flame retardant foamed insulating material.
Wherein the step (S1) comprises: mixing 30 to 70 parts by weight of a polyvinyl chloride (PVC) resin and 30 to 70 parts by weight of a chlorinated polyethylene (CPE) resin, 10 to 100 parts by weight By weight of chlorinated paraffin oil (CPO), and 1 to 5 parts by weight of a heat stabilizer at 70 to 150 캜 for 5 to 20 minutes; A first dispersion step in which 5 to 50 parts by weight of a flame retardant and 1 to 10 parts by weight of a crosslinking agent are added to the resultant product after the mixing step, at 70 to 150 DEG C for 2 to 10 minutes, based on 100 parts by weight of the resin mixture; And 5 to 50 parts by weight of a foaming agent and 0.1 to 3 parts by weight of a foaming auxiliary are added to the resultant product after the first dispersion step based on 100 parts by weight of the resin mixture and a second dispersion which is dispersed at 70 to 150 DEG C for 2 to 10 minutes Step; < / RTI >
The blowing agent may be at least one selected from the group consisting of ammonium bicarbonate, sodium hydrogencarbonate, sodium borohydride, azodicarbonamide, dinitrosopentamethylenetetramine, benzenesulfonylhydrazide, toluenesulfonylhydrazide, Zein and oxybis (benzenesulfonyl hydrazide), or a mixture of two or more thereof.
The foaming aid may be any one selected from the group consisting of a cadmium compound, a calcium compound, a zinc compound, a magnesium compound, an iron compound and a copper compound, or a mixture of two or more thereof.
The extruder may be a single extruder or a twin extruder, and the extrusion temperature may be maintained at 90 to 140 캜.
In the step (S3), the extrusion sheet may be heated to a temperature of 150 to 250 ° C to chemically crosslink and foam the foaming agent to form a foam.
The chemical crosslinked polyvinyl chloride-based flame retardant foamed insulation material according to the present invention includes a polyvinyl chloride resin excellent in flame retardancy and a chlorinated polyethylene resin, and thus can be used as a heat insulating material for construction.
The chemical crosslinked polyvinyl chloride-based flame retardant foamed insulating material according to the present invention comprises a chlorinated polyethylene resin excellent in compatibility with a polyvinyl chloride resin, thereby increasing the degree of crosslinking and enabling foaming at a high magnification, do.
Further, the chemically crosslinked polyvinyl chloride-based flame retardant foamed insulating material according to the present invention may contain chlorinated paraffin oil as a plasticizer to further improve the flame retardancy.
Hereinafter, the present invention will be described in detail. The terms and words used in the present specification and claims should not be construed as limited to ordinary or dictionary terms and the inventor may appropriately define the concept of the term in order to best describe its invention It should be construed as meaning and concept consistent with the technical idea of the present invention.
It is to be understood that both the foregoing general description and the following detailed description of the present invention are exemplary and explanatory only and are not to be construed as limiting of the invention, And the like.
The chemical crosslinked polyvinyl chloride-based flame retardant foamed insulation material according to the present invention is a resin mixture comprising 30 to 70 parts by weight of a polyvinyl chloride (PVC) resin and 30 to 70 parts by weight of a chlorinated polyethylene (CPE) resin; 10 to 100 parts by weight of chlorinated paraffin oil (CPO) based on 100 parts by weight of the resin mixture; And 1 to 10 parts by weight of a crosslinking agent are formed by extrusion foam molding.
At this time, if the content of the polyvinyl chloride resin is less than 30 parts by weight and the content of the chlorinated polyethylene resin exceeds 70 parts by weight, the limit oxygen index to be described later becomes low, which is disadvantageous for securing the flame retardancy. Is more than 70 parts by weight, and when the content of the chlorinated polyethylene resin is less than 30 parts by weight, the state of the test piece of the resin mixture becomes poor, and crosslinking and foaming are not performed well.
Since the foam made of a polyvinyl chloride resin has a good breaking property, a certain amount of plasticizer should be included. In the present invention, 10 to 100 parts by weight, or 20 to 80 parts by weight, based on 100 parts by weight of the resin mixture, Chlorinated paraffin oil is included as plasticizer. If the value is out of the above range, the limit oxygen index becomes low, which is disadvantageous in ensuring flame retardancy. In addition, as described later, the chlorinated paraffin oil is excellent in flame retardancy of the foamed thermal insulation material of the present invention, and degradation does not occur even if a heat stabilizer is added in the future, so that performance deterioration as a foamed thermal insulation material does not occur.
On the other hand, in order for a heat insulating material to be used as a construction material, it should have excellent flame retardancy and heat insulation.
The standard specification for building machinery facilities established by the Ministry of Land, Transport and Maritime has a limiting oxygen index (LOI) of 28 or more, which is a flammability measurement index measured by KS M ISO 4589-2, a test method relating to flame retardancy of insulation .
According to the present invention, the polyvinyl chloride resin, the chlorinated polyethylene resin and the chlorinated paraffin oil contain chlorine as a flame-retardant element and are excellent in flame retardancy, and the chemical oxygen-scaled polyvinyl chloride- 28 or more.
On the other hand, the heat insulating property of the foamed heat insulating material means the degree of the air existing inside the foamed heat insulating material blocks the heat from entering and leaving to prevent heat loss. Therefore, the foamed heat insulating material composed of the polyvinyl chloride resin conventionally has a low degree of crosslinking due to the chain structure of the polymer, so that foaming of about 20 times is performed, and a certain level of heat insulating property .
However, in the present invention, a resin mixture comprising 30 to 70 parts by weight of a polyvinyl chloride (PVC) resin and 30 to 70 parts by weight of a chlorinated polyethylene (CPE) resin excellent in compatibility with the polyvinyl chloride resin is used as a base resin , The crosslinking degree is increased, foaming at a high magnification of about 30 to 40 times is possible, and the heat insulating property is improved. At this time, the thermal conductivity of the foamed insulating material according to the present invention may be 0.04 W / mK or less.
In the present invention, 1 to 10 parts by weight or 2 to 5 parts by weight of a crosslinking agent may be contained. If the amount is less than 1 part by weight, the degree of crosslinking may be lowered and the expansion ratio may be poor and the heat insulating property may be deteriorated. It is not good because the surface of the cell is roughened due to the phenomenon of cell popping.
The crosslinking agent that can be used herein is at least one member selected from the group consisting of dicumylperoxide (DCP), t-butylperoxylaurate, t-butylperoxyisopropyl carbonate, benzoylperoxide, t- butylperoxyacetate, Octyl peroxide, t-dibutyl peroxymaleic acid, t-butyl hydroperoxide, 2,3-dimethyl-2,5-dihexane, di-t-butyl peroxide, 2,2- 1,3-bisbenzene, 1,1-bis-3,3,5-trimethylcyclohexane, p-chlorobenzoyl peroxide, 2,4-dichlorobenzoyl peroxide, or 2 Or more.
And, due to the high expansion rate foaming, the foam insulation of the present invention achieves lightness by showing a relatively small density of 0.025 g / cm 3 to 0.500 g / cm 3 .
On the other hand, the raw material composition may contain 5 to 50 parts by weight of a flame retardant based on 100 parts by weight of the resin mixture; And 1 to 5 parts by weight of a heat stabilizer.
If the content of the flame retardant is less than 5 parts by weight, the effect of addition of the flame retardant is insignificant. If the content of the flame retardant exceeds 50 parts by weight, the durability of the foamed heat insulating material may be deteriorated.
If the content of the heat stabilizer is less than 1 part by weight, the processability at the time of extrusion and foaming is lowered and the resin is decomposed to deteriorate the physical properties. When the amount is more than 5 parts by weight, The mechanical properties may be deteriorated.
Here, the flame retardant may be any one selected from the group consisting of antimony trioxide, decabromophenyl oxide, and magnesium hydroxide, or a mixture of two or more thereof.
The heat stabilizer may be any one selected from the group consisting of tin maleate, tin laurate, and powder tin maleate esters, or two or more of them.
Hereinafter, a method for producing the chemically crosslinked polyvinyl chloride-based flame retardant foamed insulator according to the present invention will be described.
First, a resin mixture comprising 30 to 70 parts by weight of a polyvinyl chloride (PVC) resin and 30 to 70 parts by weight of a chlorinated polyethylene (CPE) resin, 10 to 100 parts by weight of chlorinated paraffin oil (CPO 1 to 10 parts by weight of a crosslinking agent, 5 to 50 parts by weight of a flame retardant, 1 to 5 parts by weight of a heat stabilizer, 5 to 50 parts by weight of a foaming agent and 0.1 to 3 parts by weight of a foaming auxiliary.
In this case, step (S1) may be performed through the following steps to prevent efficient mixing of raw materials and deterioration of physical properties of the product.
First, a resin mixture comprising 30 to 70 parts by weight of a polyvinyl chloride (PVC) resin and 30 to 70 parts by weight of a chlorinated polyethylene (CPE) resin, 10 to 100 parts by weight of chlorinated paraffin oil (CPO ) And 1 to 5 parts by weight of a heat stabilizer are mixed at 70 to 150 캜 for 5 to 20 minutes. This mixing process can be performed in a wet kneader.
Then, 5 to 50 parts by weight of a flame retardant and 1 to 10 parts by weight of a crosslinking agent are added to the resultant product after the mixing step based on 100 parts by weight of the resin mixture, and a first dispersion step of dispersing the mixture at 70 to 150 DEG C for 2 to 10 minutes .
Next, 5 to 50 parts by weight of the foaming agent and 0.1 to 3 parts by weight of the foaming auxiliary are added to the resultant product after the first dispersion step, based on 100 parts by weight of the resin mixture, and the second A dispersion step is performed.
At this time, the product after the second dispersion step may be produced in the form of a pellet so that it can be easily injected into the extruder.
On the other hand, the reason why the polyvinyl chloride resin, the chlorinated polyethylene resin and the chlorinated paraffin oil should satisfy the above-described numerical range is as described above.
When the foaming agent and the foaming auxiliary satisfy the above-described numerical ranges, foaming is sufficiently performed, and the physical properties of the product do not decrease.
Although various kinds of foaming agents are already known, they should be able to form fine and uniform bubbles and should be used so as to minimize the early decomposition which may occur during extrusion. Non-limiting examples of such foaming agents include inorganic foaming agents such as ammonium bicarbonate, sodium hydrogencarbonate, sodium borohydride, and the like; and azo compounds such as azodicarbonamide, N, N'-dinitrosopentamethylene tetramine Benzenesulfonyl hydrazide, toluenesulfonyl hydrazide, toluenesulfonyl semicarbazide, oxybis (benzenesulfonylhydrazide) (P, P '), benzenesulfonyl hydrazide, -oxybis (benzenesulfonyl hydrazide)).
A cadmium compound, a calsium compound, a zinc compound, a magnesium compound, an iron compound, a copper compound and the like are used as the foaming auxiliary agent , And it is particularly preferable to use zinc oxide among the zinc compounds.
Subsequently, the raw material composition is introduced into an extruder and melt-extruded to produce an extruded sheet (S2).
The step (S2) is a step of extruding the raw material composition produced in the step (S1) into an extruded sheet having a predetermined width and thickness, and the extruded sheet is extruded by using a single extruder or an extruded sheet In order to further prevent premature foaming, a twin extruder, which is a twin extruder in which a foaming agent is introduced in a side feeding manner by using a separate screw, is used, and a cylinder having a screw inside and having a temperature of 90 to 140 ° C And a die having a temperature of 90 to 140 DEG C, the raw material composition is kneaded and extrusion-molded, thereby uniformly mixing the entire composition contained in the raw material composition prepared in the step (S1). When the temperature of the cylinder and the die is kept below 90 ° C, the resin mixture is slightly melted and the kneading property of the foam mixture is reduced. If the temperature is higher than 140 ° C, there arises a problem of premature decomposition of the foaming agent , It is preferable to maintain the temperature of the cylinder and the die of the extruder at 90 to 140 占 폚. At this time, it is apparent that the width and thickness of the extruded sheet can be variously adjusted according to the judgment of a person skilled in the art.
Subsequently, the extrusion sheet is heated to chemically crosslink and foam the foaming agent to form a foam (S3).
The step (S3) may be performed by heating the extruded sheet through a foaming furnace at a temperature of 150 to 250 ° C to chemically crosslink the foaming agent, and foaming the foaming agent to form a foam. If the temperature is lower than 150 ° C, the foaming agent is not activated and foaming is not properly performed. If the temperature is higher than 250 ° C, the foaming agent may be decomposed to cause problems in product formation.
At this time, the step (S3) may be carried out by any one of a horizontal foaming method for horizontally installing the foaming furnace, a vertical foaming method for vertically installing the foaming furnace, and a foaming method for the slurry using the liquid phase as the heat transfer medium .
At this time, all of the three foaming methods are performed at normal pressure, and are classified according to the method of installing the foaming furnace and the heat transfer medium. In the first horizontal foaming method, the foaming furnace is installed horizontally so that the foams are produced horizontally at the time of foaming, and all processes proceed horizontally. Such a horizontal foaming method is advantageous in that the physical properties in the longitudinal direction and the width direction are small because the expansion ratio in the longitudinal direction is small at the time of foaming since there is little influence by the gravity in the arrangement and the process progress of the foaming furnace. In the second vertical foaming method, the foaming furnace is vertically installed, and the extruded sheet is foamed while being lowered. Such a vertical foaming method is advantageous in appearance because it is foamed in air at the time of foaming, and the deviation in the width direction is small. In the third method, the liquid phase sulphate is used as a heat transfer medium. In the third method, the liquid phase sulphate is used. However, unlike the vertical firing method, the air is not used as a heat transfer material, The heat transfer effect is excellent and the foaming can be performed uniformly on the sheet. Especially, since the physical property deviation in the longitudinal direction and the width direction is very small as compared with the foam product produced by the above-described horizontal or vertical foaming method, And the characteristic is evaluated excellent.
BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail with reference to examples. However, the embodiments according to the present invention can be modified into various other forms, and the scope of the present invention should not be construed as being limited to the embodiments described below. The embodiments of the present invention are provided to enable those skilled in the art to more fully understand the present invention.
One. Example - Preparation of resin mixture
The mixture ratio of polyvinyl chloride (PVC) resin and chlorinated polyethylene (CPE) resin was adjusted by mill roll at a temperature of 140 ° C for 15 minutes to prepare resin mixtures. The limit oxygen index and the specimen state are shown in Table 1 below.
(Specimen status indication: ⊚ very good, good good, △ fair, poor)
The samples 1 to 5 according to the respective formulations were measured to have a limit oxygen index exceeding 28, so that there was no problem in flame retardancy. However, the following experiment was conducted using Sample 3 having the best specimen condition.
2. Example - Chemical bridge Polyvinyl chloride system Manufacture of flame retardant foam insulation
(One) Example One
100 parts by weight of a resin mixture having the composition of the sample 3, 50 parts by weight of chlorinated paraffin oil (CPO) as a plasticizer and 2 parts by weight of tin maleate as a heat stabilizer were mixed in a wet kneader at 70 캜 for 10 minutes .
Thereafter, 10 parts by weight of magnesium hydroxide as a flame retardant and 2 parts by weight of dicumyl peroxide (DCP) as a crosslinking agent were added and dispersed at 90 DEG C for 5 minutes. Then, 25 parts by weight of azodicarbonamide as a foaming agent, 1 part by weight was added and dispersed at 110 DEG C for 5 minutes and then pelletized.
Subsequently, the pelletized foam raw material composition was put into a single extruder maintained at 120 ° C, and melt extruded to produce an extruded sheet. Then, the extruded sheet was put into an oven maintained at 200 ° C to crosslink and foam to produce a foamed insulator Respectively.
(2) Example 2
A foaming insulation material was prepared in the same manner as in Example 1, except that 10 parts by weight of magnesium hydroxide, 2 parts by weight of antimony trioxide and 6 parts by weight of decabromophenyl oxide were added as flame retardants.
(3) Example 3
A foaming insulation material was prepared in the same manner as in Example 1, except that 10 parts by weight of magnesium hydroxide, 3 parts by weight of antimony trioxide and 9 parts by weight of decabromophenyl oxide were added as flame retardants.
(4) Example 4
A foaming insulation material was prepared in the same manner as in Example 1, except that 10 parts by weight of magnesium hydroxide, 4 parts by weight of antimony trioxide and 16 parts by weight of decabromophenyl oxide were added as flame retardants.
(5) Example 5
Except that 10 parts by weight of magnesium hydroxide, 3 parts by weight of antimony trioxide and 9 parts by weight of decabromophenyl oxide were added as the flame retardant and 10 parts by weight of azodicarbonamide was added as the foaming agent. A heat insulating material was prepared.
(6) Example 6
Except that 10 parts by weight of magnesium hydroxide, 3 parts by weight of antimony trioxide and 9 parts by weight of decabromophenyl oxide were added as the flame retarder and 20 parts by weight of azodicarbonamide was added as the foaming agent. A heat insulating material was prepared.
(7) Example 7
Except that 10 parts by weight of magnesium hydroxide, 3 parts by weight of antimony trioxide and 9 parts by weight of decabromophenyl oxide were added as flame retardants and 30 parts by weight of azodicarbonamide was added as the foaming agent. A heat insulating material was prepared.
The compositions of the foamed insulating materials prepared in Examples 1 to 7 are summarized in Table 2, and the density, the limiting oxygen index, the thermal conductivity, and the product state of each example are summarized in Table 3 below.
As shown in Table 3, all of the foamed insulation materials prepared in the Examples were manufactured in a good condition, exhibited proper density and thermal conductivity, and the limit oxygen index was measured to be 28 or more. Satisfaction.
Particularly, in Examples 2 to 4, the foaming insulation material was prepared by varying the content of the flame retardant agent. However, as the amount of the flame retardant agent was increased, the thermal conductivity of the product was not significantly changed. However, since the limit oxygen index was increased, Could know.
In Examples 5 to 7, the foaming insulation material was prepared by varying the amount of the foaming agent only. As the amount of foaming agent was increased, the density of the product was decreased, but the thermal conductivity was decreased and the adiabatic property was improved.
3. Comparative Example - Chemical bridge Polyvinyl chloride system Manufacture of flame retardant foam insulation
(One) Comparative Example One
100 parts by weight of a polyvinyl chloride (PVC) resin, 40 parts by weight of chlorinated paraffin oil (CPO) as a plasticizer and 2 parts by weight of tin maleate as a heat stabilizer were mixed in a wet kneader at 70 캜 for 10 minutes.
Thereafter, 10 parts by weight of magnesium hydroxide, 3 parts by weight of antimony trioxide and 9 parts by weight of decabromophenyl oxide and 2 parts by weight of dicumyl peroxide as a crosslinking agent were added as flame retardants and dispersed at 90 DEG C for 5 minutes. Subsequently, 25 parts by weight of dicarbonamide and 1 part by weight of zinc oxide as a foaming auxiliary were added and dispersed at 110 DEG C for 5 minutes and then pelletized.
Subsequently, the pelletized foam raw material composition was put into a single extruder maintained at 120 ° C, and melt extruded to produce an extruded sheet. Then, the extruded sheet was put into an oven maintained at 200 ° C to crosslink and foam to produce a foamed insulator Respectively.
(2) Comparative Example 2
Instead of 100 parts by weight of a polyvinyl chloride (PVC) resin, 100 parts by weight of a resin mixture having the composition of the above-mentioned Sample 3 was used and 50 parts by weight of diisononyl phthalate (DINP) was mixed in place of 40 parts by weight of chlorinated paraffin oil as the plasticizer , A foamed insulating material was prepared in the same manner as in Comparative Example 1.
(3) Comparative Example 3
Except that 100 parts by weight of the resin mixture having the compounding of the sample 3 was used instead of 100 parts by weight of the polyvinyl chloride (PVC) resin and 50 parts by weight of dioctyl phthalate (DOP) was mixed instead of 40 parts by weight of chlorinated paraffin oil as the plasticizer And a foaming insulation material was prepared in the same manner as in Comparative Example 1.
The compositions of the foamed insulation materials prepared in Comparative Examples 1 to 3 are summarized in Table 4, and the density, the limiting oxygen index, the thermal conductivity and the product state of each Comparative Example are summarized in Table 5 below.
As shown in Table 5, when polyvinyl chloride was 100% as in Comparative Example 1, crosslinking and foaming were not properly performed.
When the phthalate system was used as a plasticizer instead of the chlorinated paraffin oil as in the case of Comparative Example 2 and Comparative Example 3, plasticity was good, but a large amount of gas was generated at the time of foaming. In particular, .
It should be noted that the embodiments of the present invention disclosed herein are merely examples of specific examples for the purpose of understanding and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that other modifications based on the technical idea of the present invention are possible in addition to the embodiments disclosed herein.
Claims (16)
10 to 100 parts by weight of chlorinated paraffin oil (CPO) based on 100 parts by weight of the resin mixture; And 1 to 10 parts by weight of a cross-linking agent is extrusion-foam-molded into a polyvinyl chloride-based fire retardant foamed insulation material.
The chlorinated paraffin oil (CPO) is 20 to 80 parts by weight based on 100 parts by weight of the resin mixture.
Wherein the cross-linking agent is 2 to 5 parts by weight based on 100 parts by weight of the resin mixture.
The cross-linking agent may be at least one selected from the group consisting of dicumyl peroxide (DCP), t-butyl peroxylaurate, t-butyl peroxyisopropyl carbonate, benzoyl peroxide, t-butyl peroxyacetate, t-butyl peroxybenzoate, T-butyl peroxymaleic acid, t-butyl hydroperoxide, 2,3-dimethyl-2,5-dihexane, di-t-butyl peroxide, 2,2- Bisbenzene, 1,1-bis-3,3,5-trimethylcyclohexane, p-chlorobenzoyl peroxide, 2,4-dichlorobenzoyl peroxide, or a mixture of two or more thereof Wherein the polyvinyl chloride-based fire retardant foam insulation is a polyvinyl chloride-based fire retardant foam insulation.
Wherein the chemically crosslinked polyvinyl chloride-based flame retardant foamed insulating material has a critical oxygen index of at least 28. The chemical crosslinked polyvinyl chloride-
The chemical cross-linking density of the polyvinyl chloride-based flame-retardant foam insulation, chemical cross-linking a polyvinyl chloride-based flame-retardant foam insulation, characterized in that 0.025 g / cm 3 to 0.500 g / cm 3.
Wherein the chemical crosslinked polyvinyl chloride-based flame retardant foamed thermal insulating material has a thermal conductivity of 0.04 W / mK or less.
Wherein the raw material composition contains, based on 100 parts by weight of the resin mixture, 5 to 50 parts by weight of a flame retardant; And 1 to 5 parts by weight of a heat stabilizer; and a chemical crosslinked polyvinyl chloride-based flame retardant foamed insulation material.
Wherein the flame retardant is any one selected from the group consisting of antimony trioxide, decabromophenyl oxide and magnesium hydroxide, or a mixture of two or more thereof.
Wherein the heat stabilizer is at least one selected from the group consisting of tin maleate, tin laurate and powder tin maleate ester, or at least two kinds of organic stabilizers based on the same, wherein the heat stabilizer is a chemical crosslinked polyvinyl chloride- .
(S2) feeding the raw material composition into an extruder and melt extruding the extruded material to produce an extruded sheet; And
(S3) heating the extruded sheet to chemically crosslink and foaming the foaming agent to form a foamed polyvinyl chloride-based flame retardant foamed insulating material.
Wherein the step (S1) comprises: mixing a resin mixture comprising 30 to 70 parts by weight of a polyvinyl chloride (PVC) resin and 30 to 70 parts by weight of a chlorinated polyethylene (CPE) resin, 10 to 100 parts by weight 1 to 5 parts by weight of chlorinated paraffin oil (CPO) and heat stabilizer at 70 to 150 DEG C for 5 to 20 minutes;
A first dispersion step in which 5 to 50 parts by weight of a flame retardant and 1 to 10 parts by weight of a crosslinking agent are added to the resultant product after the mixing step, at 70 to 150 DEG C for 2 to 10 minutes, based on 100 parts by weight of the resin mixture; And
5 to 50 parts by weight of a foaming agent and 0.1 to 3 parts by weight of a foaming auxiliary are added to the resulting product after the first dispersion step based on 100 parts by weight of the resin mixture and then dispersed for 2 to 10 minutes at 70 to 150 캜 Wherein the chemical-crosslinked polyvinyl chloride-based flame-retardant foamed insulation material is a polyvinyl chloride resin.
The foaming agent may be selected from the group consisting of ammonium bicarbonate, sodium hydrogencarbonate, sodium borohydride, azodicarbonamide, dinitrosopentamethylenetetramine, benzenesulfonylhydrazide, toluenesulfonylhydrazide, toluenesulfonylsemicarbazide and (Benzenesulfonyl hydrazide), or a mixture of two or more thereof. The method for producing a chemical crosslinked polyvinyl chloride-based flame retardant foamed thermal insulation material according to claim 1,
Wherein the foaming aid is any one selected from the group consisting of a cadmium compound, a calcium compound, a zinc compound, a magnesium compound, an iron compound and a copper compound, or a mixture of two or more thereof, wherein the chemical crosslinking polyvinyl chloride- Method of manufacturing insulation.
Wherein the extruder is a single extruder or a twin extruder, and the extrusion temperature is maintained at 90 to 140 占 폚.
Wherein the step (S3) comprises heating the extruded sheet at a temperature of 150 to 250 ° C to chemically crosslink the foaming agent and foaming the foaming agent to form a foamed body.
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