JP2000008278A - Resin composition for sound-insulating carpet backing for vehicle - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a resin composition for sound-insulating carpet backing for vehicles, capable of compounding an inorganic filler at high concentration, having high sound-insulating ability and excellent in flexibility, softness, impact resistance, heat resistance and stitches-taking out strength. SOLUTION: This resin composition is obtained by mixing ethylene-α-olefin copolymer having <=120 deg.C extrapolated melting-finishing temperature in a temperature range of 10 to 170 deg.C measured by differential scanning calorimetry(DSC) with an inorganic filler. The resin composition is used as a carpet backing agent and molded in sheet-like shape and formed into a sound-insulating carpet for vehicles by carrying out backing processing, e.g. bonding the sheet to a carpet substrate.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a resin composition for carpet backing. More specifically, the present invention relates to a resin composition for a sound insulating carpet backing for an automobile having excellent flexibility, excellent thread removal properties, heat resistance, moldability, and high sound insulation.

[0002]

2. Description of the Related Art Carpets for automobiles are widely used as interior materials having a decorative effect, a dustproof effect, and a sound-insulating effect inside the car. A carpet lined with a resin material or the like by lamination processing or the like is mainly used for automobiles. What is press-formed so as to match the unevenness of the floor surface is used.

[0003] Therefore, materials (backing materials) used for backing such carpets include flexibility (wearability) and high bending strength (flexibility) that can follow complicated floor shapes, and such floor surfaces. In addition to the formability with a mold with deep irregularities according to the shape, and the yarn pulling strength that can sufficiently prevent fraying (yarn pull-out) of the pile yarn of the carpet, it also has dimensional stability, rigidity, heat resistance, room temperature and low temperature Are required to have impact resistance and sound insulation performance.

[0004] In recent years, the development of carpets for automobiles has tended to focus particularly on the improvement of comfort and decoration in automobiles, and various performances such as decoration and heat insulation in cars, and particularly, sound absorption and sound insulation performances. It is becoming increasingly important to have. The sound absorption and sound insulation performance is necessary to reduce the noise from the outside such as the engine sound of a car and improve the comfort of the room.This performance is proportional to the mass per unit area of the backing material. There is a demand for the development of a backing material having a certain thickness.

Heretofore, latex, elastomer, synthetic resin, asphalt and the like have been known as backing materials, and high-pressure low-density polyethylene has been particularly widely used. However, when these are used, there are drawbacks such as insufficient backing material thickness, low thread removal strength, and insufficient rigidity and sound insulation performance.
When trying to increase the thickness, there arises a problem that the moldability is reduced, and the flexibility is reduced to be rigid and the mountability is inferior.

[0006] Against this background, recently, an ethylene-vinyl acetate copolymer (hereinafter sometimes abbreviated as EVA), which is blended with an inorganic filler to enhance the sound insulation performance, has been widely used as a backing material. (Japanese Patent Publication No. 62-9010, etc.). However, in the conventional product using EVA,
As the compounding amount of the inorganic filler increases, it becomes difficult to obtain a uniform compound, and even if a uniform compound is obtained, the compound becomes hard and brittle, lowers flexibility, and lacks flexibility. Therefore, the mixing ratio is limited to about 50 to 60% by weight, and sufficient sound insulation cannot be exhibited.

Further, a carpet backing composition has been developed in which an inorganic filler is blended at a high density with an ethylene / α-olefin copolymer to improve flexibility, low-temperature properties, heat resistance and sound insulation. Japanese Patent Publication No. 2-10271). However, ethylene • α- obtained by a Ziegler-type catalyst using the titanium compound used here.
A resin composition for carpet backing using an olefin copolymer is inferior in tensile strength and flexibility.

[0008]

According to the present invention, it is possible to increase the sound insulation performance by blending an inorganic filler at a higher concentration than conventional products, and it is possible to improve flexibility, flexibility, impact resistance and heat resistance. Another object of the present invention is to provide a resin composition for a carpet backing for sound insulation of a vehicle or the like, which has excellent thread removal strength.

[0009]

Means for Solving the Problems As a result of intensive studies, the present inventors have found that a resin composition containing a specific ethylene / α-olefin copolymer and an inorganic filler as essential components can solve the above problems. Thus, the present invention has been completed.

That is, the present invention relates to a resin composition comprising an ethylene / α-olefin copolymer and an inorganic filler as essential components, wherein the ethylene / α-olefin copolymer comprises a differential scanning calorimeter. Extrapolation melting end temperature (Te in the temperature range -10 to 170 ° C measured by (DSC)
m) is 120 ° C. or lower. A resin composition for a sound insulating carpet backing for vehicles, wherein

In the present invention, the content of the inorganic filler in the resin composition is at least 30% by weight, and the density of the resin composition is at least 1.20 g / cm ^3. And a resin composition for the sound insulating carpet backing for vehicles.

Further, the present invention provides the above-mentioned ethylene / α-olefin copolymer, wherein the ethylene / α-olefin copolymer is a copolymer of ethylene and an α-olefin having 5 to 12 carbon atoms and has a density of 0.870 to 0.870.
0.910 g / cm ³ , melt flow rate 3-10
The resin composition for sound-insulating carpet backing for vehicles, wherein the resin composition is 0 g / 10 minutes.

[0013] The present invention also relates to the present invention, wherein the ethylene / α-olefin copolymer is eluted at a temperature of 80 ° C. or less by temperature rising elution fractionation (TREF) at 90% by weight based on the total amount of the ethylene / α-olefin copolymer. % Of the resin composition for soundproof carpet backing for vehicles.

Further, the present invention is characterized in that the ethylene / α-olefin copolymer is obtained by copolymerizing ethylene and α-olefin using a metallocene catalyst as a polymerization catalyst. A resin composition for sound-insulating carpet backing for vehicles.

Further, the present invention relates to the ethylene / α-olefin copolymer; 15 to 60% by weight of the ethylene / α-olefin copolymer;
Consisting of a coagulant and an inorganic filler that are compatible with the α-olefin copolymer, and comprising 70% by weight of the inorganic filler.
The present invention provides the resin composition for sound insulating carpet backing for vehicles, wherein the resin composition is obtained by mixing the inorganic filler mixture containing the above with 40 to 85% by weight.

[0016]

Embodiments of the present invention will be described below. The resin composition of the present invention contains an ethylene / α-olefin copolymer and an inorganic filler as essential components.

(1) Ethylene / α-olefin copolymer The ethylene / α-olefin copolymer used in the present invention is mainly composed of structural units derived from ethylene (hereinafter, referred to as “ethylene”).
(Hereinafter referred to as an ethylene unit), and a structural unit derived from an α-olefin as a copolymer component (hereinafter, referred to as a comonomer unit).

(A) Copolymer Composition The α-olefin for deriving the comonomer unit is preferably selected from those having 5 to 12 carbon atoms. Α having 5 to 12 carbon atoms
-As the olefin, specifically, pentene-1, hexene-1, octene-1, 4-methylpentene-1,
Decene-1, dodecene-1 and the like can be mentioned. Of these, hexene-1 is particularly preferred. The α-olefin used as a comonomer is not limited to one kind, and includes a multi-component copolymer using two or more kinds such as a terpolymer.

The proportion of ethylene units in the ethylene / α-olefin copolymer is preferably from 94 to 87.5 mol%, more preferably from 94 to 89.5 mol%, and the comonomer unit is preferably from 6 to 12 mol%. It is 0.5 mol%, more preferably 6 to 10.5 mol%.

The ethylene units and comonomer units in these ethylene / α-olefin copolymers are ¹³ C-
It is a value measured using NMR (nuclear magnetic resonance method).
Specifically, 270 MHz of FT-NMR manufactured by JEOL Ltd.
Is a value measured by the apparatus of FIG.

(B) Extrapolation melting end temperature (Tem) by differential scanning calorimetry (DSC) The ethylene / α-olefin copolymer of the present invention has a temperature range measured by differential scanning calorimetry (DSC). Is the extrapolated melting end temperature at −10 to 170 ° C. (Tem)
But not more than 120 ° C. The extrapolated melting end temperature is 12
If the temperature is higher than 0 ° C., the adhesive strength to the carpet substrate is poor, which is not preferable. The value of Tem in the present invention is:
This is a value measured according to JIS-K7121.

(C) Melt flow rate The ethylene / α-olefin copolymer used in the present invention has a melt flow rate [JIS-K7210 (1
90 ° C., 2.16 kg load).
Hereinafter, it is abbreviated as “MFR”. ], Preferably from 3 to 100
g / 10 minutes, more preferably 3 to 50 g / 10 minutes. When the MFR is within the above range, there is an advantage that extensibility and neck-in in extrusion lamination are excellent and a uniform molten thin film can be obtained. On the other hand, if the MFR is higher than the above range, the neck-in becomes large and a uniform molten thin film cannot be obtained, so that it is not preferable. If the MFR is less than the above range, the extensibility is poor and the extrusion load is large.

(D) Density The density of the ethylene / α-olefin copolymer of the present invention is not particularly limited, but is preferably 0.870 to 0.910.
g / cm ³ , particularly preferably 0.870 to 0.900 g
/ Cm ³ . If the density is within this range, the inorganic filler can be blended at a high concentration, and it has appropriate rigidity even after blending, and it has good shape retention after heat forming and fit to the floor of automobiles. It is preferable because it is excellent.

(E) Elution Curve by Elevated Temperature Elution Fractionation The ethylene / α-olefin copolymer of the present invention has an elution amount at 80 ° C. or less by temperature increase elution fractionation (TREF) of the ethylene / α-olefin copolymer. It is preferably 90% by weight or more based on the total amount of the polymer.

Here, the temperature rise elution fractionation (Temperature
Rising Elution Fraction (hereinafter sometimes abbreviated as “TREF”) means “Journal of AppliedPo
This is carried out as follows based on the principles described in "Solmer Science, Vol. 26, 4217-4231 (1981)" and "Preprints of the Society of Polymer Science 2P1C09 (1985)".

First, the polymer to be measured is completely dissolved in a solvent and then cooled to form a thin polymer layer on the surface of the inert carrier. Such a polymer layer is formed such that an easily crystallizable material is formed on the inner side (closer to the surface of the inert carrier), and a hardly crystallizable material is formed on the outer side. next,
The temperature is increased continuously or stepwise, and components eluted at each temperature are collected. At this time, at the low temperature stage, the polymer is eluted from the amorphous portion in the polymer composition, that is, the polymer having a short-chain branch having a high degree of branching. , And the measurement is completed. In this way, the concentration of the eluted component recovered at each temperature is detected, and the elution amount and elution temperature are determined. A graph drawn by the elution amount and the elution temperature is an elution curve, from which the composition distribution of the polymer can be known.

The ethylene / α-olefin copolymer used in the present invention has an elution amount at 80 ° C. or less determined by an elution curve obtained by the above TREF.
It is preferably at least 90% by weight, more preferably at least 95% by weight, based on the total amount of the ethylene / α-olefin copolymer. If the elution amount is less than 90% by weight, if the inorganic filler is blended in a high concentration, the flexibility and the flexibility may be poor, and the physical properties as a backing material may not be maintained.

(F) Production of Ethylene / α-Olefin Copolymer The method for producing the ethylene / α-olefin copolymer of the present invention having the above-mentioned physical properties is not particularly limited, but preferably a metallocene catalyst is used as the polymerization catalyst. By copolymerizing ethylene with the above-mentioned α-olefin having 5 to 12 carbon atoms, a copolymer having the above-mentioned properties can be obtained.

(I) Metallocene-based catalyst The ethylene / α-olefin copolymer of the present invention is prepared in the presence of a so-called metallocene-based catalyst comprising the following components A, B, and optionally component C. By copolymerizing ethylene with an α-olefin.

[Component A] Component A is a compound represented by the following general formula (I).

[0031]

Embedded image ^{_{Q 1 (C 5 H 4-}} a R 1 a) (C 5 H 4-b R 2 b) MeX 1 Y 1 ··· (I)

[Wherein Q ¹ is a binding group bridging two conjugated five-membered ring ligands, and is a divalent hydrocarbon group having 1 to 20 carbon atoms or a hydrocarbon group having 1 to 20 carbon atoms. And a germylene group having a hydrocarbon group having 1 to 20 carbon atoms. Me is zirconium or hafnium,
X ¹ and Y ¹ are each independently hydrogen, a halogen group,
A C1-20 hydrocarbon group, a C1-20 alkoxy group, a C1-20 alkylamide group, a trifluoromethanesulfonic acid group, a C1-20 phosphorus-containing hydrocarbon group or a C1 1 to 20 represents a silicon-containing hydrocarbon group. R ¹ and R ² each independently have 1 to 2 carbon atoms.
And 0 represents a hydrocarbon group, a halogen group, an alkoxy group, a silicon-containing hydrocarbon group, a phosphorus-containing hydrocarbon group, a nitrogen-containing hydrocarbon group or a boron-containing hydrocarbon group.

Further, two adjacent R ¹ or R ² may be bonded to each other to form a ring. a and b are each 0
It is an integer satisfying ≦ a ≦ 4 and 0 ≦ b ≦ 4. Where R
^The two five-membered ligands bearing ¹ and R ² are asymmetric with respect to the plane containing Me in terms of their relative position via the group Q ¹ . ]

As described above, Q ¹ is a bonding group bridging two conjugated five-membered ring ligands, and is represented by the following (A):
It is selected from the groups shown in (b) and (c). (A) a divalent hydrocarbon group having 1 to 20 carbon atoms, preferably 1 to 6 carbon atoms, more specifically, an unsaturated hydrocarbon group such as an alkylene group, a cycloalkylene group, and an arylene; 20, preferably a silylene group having a hydrocarbon group of 1 to 12, (c) a germylene group having a hydrocarbon group of 1 to 20, preferably 1 to 12 carbon atoms.

The distance between the two bonds of the divalent Q ¹ group is about 4 atoms or less, preferably 3 atoms or less when Q ¹ is chain-like, irrespective of the number of carbon atoms. ,
When Q ¹ has a cyclic group, the cyclic group +2
It is preferable that the number of atoms is about equal to or less than one atom, particularly, only the cyclic group.

Therefore, in the case of alkylene, ethylene and isopropylidene (the distance between both bonds is 2 atoms and 1 atom), in the case of a cycloalkylene group, a cyclohexylene group (the distance between bonds is only a cyclohexylene group), In the case of alkylsilylene, a dimethylsilylene group (the distance between the bonds is 1 atom) is preferable.

Me is zirconium or hafnium. X ¹ and Y ¹ may be each independently, that is, mutually the same or different, and are selected from the following groups (d) to (l). (D) hydrogen (e) halogen (fluorine, chlorine, bromine, iodine, preferably chlorine) (f) a hydrocarbon group having 1 to 20 carbon atoms, preferably 1 to 12 carbon atoms (g) 1 to 20 carbon atoms Preferably, it is an alkoxy group having 1 to 12 carbon atoms. (H) An alkylamide group having 1 to 12 carbon atoms, preferably 1 to 12 carbon atoms. Hydrogen group (nu) a silicon-containing hydrocarbon group having 1 to 20 carbon atoms, preferably 1 to 12 carbon atoms (l) trifluoromethanesulfonic acid group

R ¹ and R ² are each independently:
It represents a hydrocarbon group having 1 to 20 carbon atoms, a halogen group, an alkoxy group, a silicon-containing hydrocarbon group, a phosphorus-containing hydrocarbon group, a nitrogen-containing hydrocarbon group or a boron-containing hydrocarbon group. Further, two adjacent R ¹ or two R ² may be bonded to each other to form a ring. a and b are each 0 ≦ a
≦ 4, 0 ≦ b ≦ 4.

As a specific example, see Japanese Patent Application Laid-Open No. 8-2087.
Compounds exemplified in JP-A No. 33 can be mentioned. For example, dimethylsilylenebis (2,4-dimethylindenyl) zirconium dichloride, dimethylsilylenebis (2-methyl-4-isopropylindenyl) zirconium dichloride, dimethylsilylenebis (2-methyl-
4-phenylindenyl) zirconium dichloride, dimethylsilylenebis (2-methyl-4,5-benzoindenyl) zirconium dichloride, and the like. Among them, it is preferable to use dimethylsilylenebis (2-methyl-4,5-benzoindenyl) zirconium dichloride or dimethylsilylenebis (2-methyl-4-phenylindenyl) zirconium dichloride.

[Component B] Component B comprises an aluminum oxy compound (component B-1), a Lewis acid (component B-2), and an ion capable of converting component A into a cation by reacting with component A. It is a compound selected from the active compounds (component B-3).

Here, some of the Lewis acids are referred to as “Component A”.
And an ionic compound capable of converting component A into a cation by reacting with cation. Therefore,
A compound belonging to both the "Lewis acid" and the "ionic compound capable of converting the component A to a cation by reacting with the component A" shall be interpreted as belonging to either one.

For the specific compounds and production methods for Component B-1, Component B-2 and Component B-3, refer to
Compounds and production methods exemplified in JP-A-239914 and JP-A-8-208733 can be exemplified.

For example, as component B-1, methylalumoxane, ethylalumoxane, butylalumoxane, isobutylalumoxane obtained from one type of trialkylaluminum and water, and two types of trialkylaluminum and water are obtained. Methylethylalumoxane, methylbutylalumoxane, methylisobutylalumoxane, and examples of the alkylboronic acid include methylboronic acid, ethylboronic acid, butylboronic acid, and isobutylboronic acid.

The component B-3 is triphenylcarbonium tetrakis (pentafluorophenyl) borate, and the component B-2 is triphenylboron, tris (3,5-difluorophenyl) boron, tris (pentane). It is preferable to use (fluorophenyl) borate and N, N-dimethylanilinium tetrakis (pentafluorophenyl) borate.

[Component C] Component C is an organoaluminum compound, and is used as needed. Preferred are compounds represented by the following general formula (II),
These compounds can be used alone or in combination of two or more.

[0046]

Embedded image (AlR ⁴ _n X _3-n ) _m (II)

[In the formula, R ⁴ represents an alkyl group having 1 to 20 carbon atoms, preferably 1 to 10 carbon atoms, and X represents a halogen, hydrogen, an alkoxy group or an amino group. n is 1 to 3,
Preferably an integer of 2-3, m is 1-2, preferably 1. ]

Specific compounds include trimethylaluminum, triethylaluminum, trinormal propyl aluminum, trinormal butyl aluminum,
Triisobutylaluminum, trinormal hexyl aluminum, trinormal octyl aluminum, trinormal decyl aluminum, diethyl aluminum monochloride, ethyl aluminum sesquichloride,
Examples thereof include diethylaluminum hydride, diethylaluminum ethoxide, diethylaluminum dimethylamide, diisobutylaluminum hydride, and diisobutylaluminum chloride. Among these, a trialkylaluminum and a dialkylaluminum hydride in which m = 1 and n = 3 are preferable. More preferably, R ⁴ is a trialkyl aluminum having 1 to 8 carbon atoms.

[Preparation of Catalyst] The preparation of the metallocene-based catalyst is carried out in the presence or absence of the monomer to be polymerized in the polymerization vessel or outside the polymerization vessel, using the component A, the component B and the component C used as required. This can be done by contacting in the absence.

The metallocene-based catalyst uses a fine solid as a carrier, and can be used as a solid catalyst. As the solid in the form of fine particles, inorganic porous oxides such as silica and alumina are used as the inorganic compound, and α-olefins such as ethylene, propylene and 1-butene are used as the organic compound, or a polymer formed mainly from styrene. Copolymers or copolymers can be mentioned.

The above-mentioned metallocene catalyst may be one obtained by preliminarily polymerizing in the presence of an olefin. As the olefin used for the prepolymerization, propylene, ethylene, 1-butene, 3-methyl-butene-1, styrene,
Divinylbenzene and the like are used, but a mixture of these and other olefins may be used.

The proportions of component A, component B and component C used in the preparation of the above metallocene catalyst are arbitrary,
In general, the preferred range of the amount used depends on what is selected as the component B.

When component B-1 is used as component B,
The atomic ratio (Al / Me) of the aluminum atom in the aluminum oxy compound of the component B-1 to the transition metal in the component A is 1 to 100,000, more preferably 10 to 10,000, and particularly preferably 50 to 100.
It is preferably within the range of 5,000 to 5,000.

When a Lewis acid of Component B-2 or an ionic compound of Component B-3 is used as Component B, the molar ratio of the transition metal in Component A to Component B-2 or Component B-3 is 0. 1
It is preferably used in the range of from 1000 to 1000, more preferably from 0.5 to 100, especially from 1 to 50.

When the organoaluminum compound of the component C is used, the amount of the organoaluminum compound to be used is 10 moles relative to the component A.
The range is preferably ⁵ or less, more preferably 10 ⁴ or less, and particularly preferably 10 ³ or less.

(Ii) Polymerization The production of an ethylene / α-olefin copolymer using the metallocene catalyst is carried out by mixing and contacting ethylene and α-olefin. The amount ratio of each monomer in the reaction system does not need to be constant over time, and it is convenient to supply each monomer at a constant mixing ratio, and to change the mixing ratio of the supplied monomers over time. Is also possible. Further, any of the monomers can be dividedly added in consideration of the copolymerization reaction ratio.

As the polymerization mode, any mode can be adopted as long as the catalyst component and each monomer are in efficient contact. Specifically, a slurry method using an inert solvent, a bulk method using a monomer itself as a solvent without substantially using an inert solvent, a solution polymerization method, or a method in which each monomer is substantially gasified without using a substantially liquid solvent A gas phase method or the like for maintaining the shape can be employed.

The present invention is also applicable to continuous polymerization and batch polymerization. In the case of slurry polymerization, hexane, heptane, pentane, cyclohexane, benzene,
A single or mixture of a saturated aliphatic or aromatic hydrocarbon such as toluene can be used.

The polymerization conditions are as follows: the polymerization temperature is -78 ° C.
The temperature is 160 ° C., preferably 0 ° C. to 150 ° C. At that time, hydrogen can be used as a molecular weight regulator in an auxiliary manner. The polymerization pressure is 0 to 90 kg / cm ² · G, preferably 0 to 60 kg / cm ² · G, particularly preferably 1 to 60 kg / cm ² · G.
50 kg / cm ² · G is appropriate.

The ethylene / α-olefin copolymer of the present invention satisfies the condition that Tem by DSC is 120 ° C. or less, preferably 90% by weight or more, in addition to the conditions of DSC, the elution amount at 80 ° C. or less by TREF is 90% by weight or more. As long as it is obtained by a method using any catalyst, it is particularly preferable to satisfy the conditions of DSC and TREF, and to use ethylene and C6 to C10 using the above-described metallocene catalyst. And obtained by copolymerizing α-olefin of the formula (1). The ethylene / α-olefin copolymer obtained by using such a metallocene-based catalyst is clearly distinguished from, for example, an ethylene / α-olefin copolymer obtained by a Ziegler-type catalyst using a titanium compound.

That is, in the ethylene / α-olefin copolymer obtained by the Ziegler-type catalyst using a titanium compound, the monomer constituting the copolymer is the same as the copolymer of the present invention, and the density and MFR Even when the values of the two coincide, the Tem by DSC is higher than 120 ° C., and the elution amount at 80 ° C. or lower by TREF is less than 90% by weight. On the other hand, the ethylene / α-olefin copolymer obtained by the above-mentioned metallocene-based catalyst has a high content of a copolymer component in the copolymer, and has a narrow molecular weight distribution despite the fact that the copolymer as a whole has many branches. It is a polymer with a uniform composition, and the Tem by DSC becomes 120 ° C. or less,
In addition, the elution amount at 80 ° C. or less by TREF is also 90% by weight or more.

As described above, the Tem by DSC is 120
℃ or less, preferably further 80 ℃ by TREF
The resin composition of the present invention, wherein the following elution amount is 90% by weight or more, more preferably an ethylene / α-olefin copolymer which is polymerized using a metallocene catalyst and satisfies the above conditions, is used as a resin component. It is a resin material which is superior in flexibility and high in strength as compared with an ethylene / α-olefin copolymer obtained by a Ziegler catalyst using a conventional titanium compound which does not satisfy such conditions. Also, compared to a copolymer of ethylene and an α-olefin having 4 or less carbon atoms obtained by a vanadium-based catalyst or the like, since it is a resin material having high strength, an inorganic filler can be blended at a high concentration, Sound insulation, which is important as a backing material, can be enhanced.

For this reason, when the resin composition of the present invention is used as a backing material for carpets, it has excellent strength, excellent flexibility, a high concentration of inorganic filler, and excellent sound insulation. It will be. This is mainly due to
This is considered to be due to the difference in the ethylene / α-olefin copolymer used as the resin component.

(2) Inorganic Filler As the inorganic filler which is an essential component of the present invention, a filler used for rubber and plastic can be used. This filler is, for example, as described in the section "VI. Reinforcing Materials and Fillers" of "Rubber Industry Handbook (New Edition)" (Japan Rubber Association, second edition of 1979). . Specific examples include calcium carbonates, clays, silicas, aluminas, talcs, barium sulfate, calcium sulfate, zinc white, aluminum hydroxide, magnesium hydroxide, and carbon black. Among these, calcium carbonates Is most preferred.

If necessary, the above filler may be used after being treated with a surface treating agent (such as a silane coupling agent or an organic titanate).

(3) Other Components In the resin composition of the present invention, if necessary, a phenolic antioxidant, a phosphorus antioxidant, a sulfur antioxidant, a neutralizing agent, a light stabilizer, an ultraviolet ray The above-mentioned effects (characteristics) that the composition of the present invention has additives such as an absorbent, a lubricant, an antistatic agent, a metal deactivator, an antibacterial and fungicide, an optical brightener band, a flame retardant, and a coloring agent May be added as long as is not impaired.

The resin composition of the present invention may contain other resin components than the above-mentioned ethylene / α-olefin copolymer. Other resin components that can be blended include high-pressure low-density polyethylene, atactic polypropylene, ethylene-vinyl acetate copolymer, ethylene-
An acrylic acid copolymer, an ethylene-methyl acrylate copolymer, and the like can be given. When such another resin component is blended, its blending amount is usually about 1 to 30% by weight based on the amount of the ethylene-α-olefin copolymer.

(4) Resin Composition (a) Composition Ratio The content of the inorganic filler in the resin composition of the present invention is as follows:
Preferably 30% by weight or more, more preferably 50% by weight
That is all. If the amount of the inorganic filler is less than 30% by weight, the mass per unit area of the obtained backing material is low, and the sound insulating effect is not good.

The upper limit of the content of the inorganic filler is not particularly limited, but is preferably 75% by weight or less, more preferably 70% by weight or less, in consideration of the balance with flexibility. If the amount of the inorganic filler is too large, the moldability becomes poor. A particularly preferred content of the inorganic filler is 60 to 70% by weight.

The amounts of the components such as antioxidants used as necessary are appropriately selected according to the known standards according to the purpose.

(B) Density The density of the resin composition of the present invention is preferably 1.20 g /
cm ³ or more. If the density of the entire resin composition is lower than the above range, the rigidity is low, and the shape retention after heat molding is inferior.

(C) Preparation of Resin Composition In general, the resin composition of the present invention is prepared by mixing the above-mentioned ethylene / α-olefin copolymer with an inorganic filler and other optional components used if necessary. It can be prepared by melting and kneading.

Mixing, melting and kneading are usually carried out using a Henschel mixer, a super mixer, a V-blender, a tumbler mixer, a ribbon blender, a Banbury mixer,
It can be carried out by a kneader blender, a single-screw or twin-screw kneading extruder, and among them, it is preferable to perform mixing or melt kneading by a single-screw or twin-screw kneading extruder. After compounding, it can be extruded with an extruder or the like, and can be formed into powder, pellets, film, sheet, or the like, if necessary.

In the present invention, as a preferred method of blending the inorganic filler with the ethylene / α-olefin copolymer, a coagulant (binder) having compatibility with the ethylene / α-olefin copolymer and an inorganic filler are used. There is a method in which an inorganic filler mixture comprising a filler and containing the inorganic filler in a high concentration of 70% by weight or more is prepared in advance and mixed with an ethylene / α-olefin copolymer.

As the coagulant, wax, atactic polypropylene, petroleum resin, melt index of about 30
The above-mentioned ethylene-vinyl acetate copolymer, rosin or rosin derivative, terpene resin, asphalt and the like can be mentioned. These are used alone or as a mixture of two or more. Among them, it is preferable to select from the group consisting of wax, atactic polypropylene, and petroleum resin.

As the wax, paraffin wax,
Examples include microcrystalline wax and polyethylene wax. Examples of the petroleum resin include aliphatic, alicyclic, and aromatic hydrocarbons and mixtures thereof.

The inorganic filler mixture can be formed into flakes, granules or pellets in advance, and can be easily extruded by simply dry blending with an ethylene / α-olefin copolymer.

The method for preparing a resin composition using the above inorganic filler mixture is preferably an ethylene / α-olefin copolymer: inorganic filler mixture = 15 to 60:85.
~ 40 (weight ratio), more preferably 20 ~ 30: 80 ~
The two can be mixed at a ratio of 70 (weight ratio), and can be performed using a melt kneading device such as a Banbury mixer, an intensive mixer, or a twin screw extruder.

(5) Carpet backing As a method of backing a carpet substrate using the resin composition of the present invention, immediately after the preparation of the resin composition, the resin composition is extruded into a film or sheet and directly onto the carpet substrate. There is a method of backing. Alternatively, the resin composition prepared in powder form in advance may be evenly sprayed on the back surface of the carpet base material, and then heat-fused for backing.

After extruding the resin composition formed into pellets into a film or sheet by an extruder or the like, the film or sheet can be backed to a carpet substrate. The film or sheet is
The backing process can be performed by heating or bonding together with a carpet substrate using an adhesive.

Specifically, for example, using a well-known extrusion coating apparatus, the resin composition is melt-extruded into a sheet shape from a T-die of an extruder, combined with the back surface of the carpet, and further backed by compression and cooling with a cooling roll and a press roll. A method of backing, or a method in which the resin composition previously formed into a sheet shape is heated together with a carpet backside and heated by a heater or the like to melt the resin composition, and further pressed and cooled with a press roll to back the resin composition. A method in which the resin composition is melt-kneaded using a calendering apparatus, the amount of application is adjusted with a metering roll, and the backing is backed by calendering in which the carpet is backed with a nip roll.

[0082] In addition to the backing on the carpet base material, a woven fabric, a nonwoven fabric, a plastic film, paper, felt and the like can be further laminated if necessary. The resin composition of the present invention is also excellent in adhesiveness to a laminate such as felt.

The carpet base material to which the resin composition of the present invention can be used as a backing material is a woven carpet, a knitted carpet, a tufted carpet of loop or cut pile, a needle punched carpet having a nonwoven fabric provided with a backing material, etc. It can be preferably used for tufted carpet for vehicles.

[0084]

EXAMPLES Hereinafter, the present invention will be described specifically with reference to examples, but the present invention is not limited to these examples. In addition, the measurement of the physical properties in the following Examples and Comparative Examples was performed by the following methods.

(1) MFR; JIS-K7210 (19
(0 ° C., 2.16 kg load). (2) Density: measured according to JIS-K7112. (3) Extrapolated melting end temperature (Tem); JIS-K712
1 was measured. (4) Tensile breaking strength and tensile breaking elongation; JIS-K71
13 was measured. (5) Vicat softening point temperature: Measured according to JIS-K7206.

(6) Bending test: A state in which a sheet having a thickness of 2 mm was bent at 180 degrees was visually observed and evaluated according to the following criteria. ：: Some small cracks may occur. Δ: Many cracks were observed, but no break was observed. X: The film was broken from the fold.

(7) Thread pulling strength: One end of the cut pile was pulled with a spring gauge, and the strength (kg / piece) at the time of thread pulling was measured. (8) Olsen bending stiffness: measured according to JIS-K7106.

(9) Measurement of elution amount by TREF: The elution amount measurement by TREF in the present invention was performed as follows. The measurement was carried out using a cloth separation apparatus (CFC T150A, manufactured by Mitsubishi Chemical Corporation) as a measurement apparatus according to the measurement method in the attached operation manual. This cross-separation apparatus includes a temperature-rise elution separation (TREF) mechanism that separates a sample by using a difference in dissolution temperature, and a size exclusion chromatograph (SEC) that further separates the separated fraction according to a molecular size. Is a device connected online.

First, the sample to be measured (ethylene / α
-Olefin copolymer) using a solvent (o-dichlorobenzene) to give a concentration of 4 mg / ml.
It was melted at ℃ and injected into a sample loop in the measuring device. The following measurements were performed automatically according to the set conditions.

The sample solution held in the sample loop is separated using a TREF column (inside diameter of 4 m filled with glass beads as an inert carrier) by utilizing the difference in dissolution temperature.
m, 150mm length stainless steel column attached to the device)
Was injected 0.4 ml. The sample was cooled at a rate of 1 ° C./min from 140 ° C. to 0 ° C. and coated on the inert carrier. At this time, from the high crystal component (the one that is easy to crystallize) to the low crystal component (the one that hardly crystallizes)
The polymer layer is formed on the surface of the inert carrier in this order. TR
After maintaining the EF column at 0 ° C. for an additional 30 minutes, 2 ml of the component dissolved at a temperature of 0 ° C. was added at a flow rate of 1 ml / min.
From REF column to SEC column (Showa Denko KK,
AD80M · S, 3 tubes). While fractionation by molecular size was being performed by SEC, the temperature of the TREF column was raised to the next elution temperature (5 ° C.) and maintained at that temperature for about 30 minutes. The measurement of each elution section by SEC was performed at intervals of 39 minutes. The following temperature is used as the elution temperature,
The temperature was raised stepwise.

Elution temperature (° C.): 0, 5, 10, 15, 2
0, 25, 30, 35, 40, 45, 49, 52, 5
5,58,61,64,67,70,73,76,7
9,82,85,88,91,94,97,100,1
02,120,140 ° C.

For the solution separated by the molecular size in the SEC column, the absorbance in proportion to the concentration of the polymer was measured with an infrared spectrophotometer attached to the apparatus (wavelength 3.42 μm).
m, detection by stretching vibration of methylene) to obtain chromatograms for each elution temperature category. Using built-in data processing software,
A baseline of the chromatogram of each elution temperature section obtained by the above measurement was drawn and subjected to arithmetic processing. The area of each chromatogram was integrated and an integrated elution curve was calculated. From the integrated elution curve, the area ratio of the elution amount at 80 ° C. or less to the total area was determined.

[0093]

Example 1 As an ethylene / α-olefin copolymer, “Kernel KE027” (manufactured by Nippon Polychem Co., Ltd.)
Ethylene hexene obtained with a metallocene catalyst
1 copolymer: MFR 16.5 g / 10 min, density: 0.8
98 g / cm ³ ), 20% by weight, and an inorganic filler “Calpet” (trade name, manufactured by Nitto Powder Chemical Co., Ltd., calcium carbonate 80)
A mixture of 80% by weight) and a width of 1.6% at a resin temperature of 240 ° C. using an extrusion laminator of a 115 mmφ extruder.
Extrusion coating at a laminating speed of 4 m / min on the back of a tufted carpet of
Backing was performed at a thickness of kg / m ² to obtain a desired sound insulating carpet. Separately, only the backing resin composition 2
A pressed sheet having a thickness of mm was formed, and the physical properties of the sheet were measured. Table 1 shows the results.

[0094]

Embodiment 2 In Embodiment 1, the kernel KE027
Was changed to an ethylene-hexene-1 copolymer (MFR: 16.5 g / 10 min, density: 0.885 g / cm ³ ) obtained by using a metallocene catalyst, in the same manner as in Example 1, except that And a press sheet. Table 1 shows the results.

[0095]

Example 3 Sound insulation was performed in the same manner as in Example 1 except that the mixing ratio in the backing resin composition was changed so that the kernel KE027 was 25% by weight and the carpet was 75% by weight. A carpet and a press sheet were obtained. Table 1 shows the results.

[0096]

[Comparative Example 1] In Example 1, the kernel KE027
Was converted to a high-pressure method ethylene-vinyl acetate copolymer (vinyl acetate content: 28% by weight, MFR: 15 g / 10 min, density:
Except for changing to 0.950 g / cm ³ ), a sound insulating carpet and a press sheet were obtained in the same manner as in Example 1. Table 1 shows the results.

[0097]

Comparative Example 2 In Example 3, the kernel KE027
With a high-pressure method ethylene / vinyl acetate copolymer (vinyl acetate content: 28% by weight, MFR: 15 g / 10 min, density:
Except for changing to 0.950 g / cm ³ ), a sound insulating carpet and a press sheet were obtained in the same manner as in Example 1. Table 1 shows the results.

[0098]

Comparative Example 3 In Example 3, the kernel KE027
Was prepared using an ethylene / butene-1 copolymer (MFR: 8 g / 10 min, density: 0.922 g /
cm ³ ), except that a sound insulating carpet and a press sheet were obtained in the same manner as in Example 1. Table 1 shows the results.

[0099]

Comparative Example 4 In Example 3, the kernel KE027
Of ethylene-butene-1 produced with a vanadium-based catalyst
Copolymer (MFR: 18 g / 10 min, density: 0.89 g)
/ Cm ^Three) Except that the sound insulation was performed in the same manner as in Example 1.
A carpet and a press sheet were obtained. The results are shown in Table 1.
You.

[0100]

[Table 1]

Examples 1 to 3 using the resin composition of the present invention
Shows a remarkably high tensile elongation as compared with Comparative Examples 1 to 4, and is excellent in flexibility. In addition, flexibility,
It can be seen that the thread removal strength and heat resistance are also remarkably excellent.

[0102]

The resin composition of the present invention can be blended with an inorganic filler at a higher concentration than conventional products, so that it has high sound insulation performance, and has flexibility, flexibility, impact resistance, and heat resistance. It has excellent properties and thread removal strength, and is useful as a sound insulating carpet backing material for vehicles.

──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI Theme coat ゛ (Reference) D06M 17/00 D06M 17/00 C

Claims (6)

[Claims] 1. A resin composition comprising an ethylene / α-olefin copolymer and an inorganic filler as essential components, wherein said ethylene / α-olefin copolymer is obtained by differential scanning calorimetry (DSC). Measured temperature range -10 to 170
A resin composition for sound insulating carpet backing for vehicles, which has an extrapolated melting end temperature (Tem) at 120 ° C or lower. 2. The resin composition according to claim 1, wherein the content of the inorganic filler in the resin composition is 30% by weight or more, and the density of the resin composition is 1.20 g / cm ³ or more. The resin composition for a sound insulating carpet backing for vehicles according to the above. 3. The ethylene / α-olefin copolymer is a copolymer of ethylene and an α-olefin having 5 to 12 carbon atoms, and has a density of 0.870 to 0.910 g /
The resin composition for sound-insulating carpet backing for vehicles according to claim 1, wherein the resin composition has a melt flow rate of ³ to 100 g / 10 min in cm ³ . 4. The amount of the ethylene / α-olefin copolymer eluted at a temperature of 80 ° C. or less by temperature rising elution fractionation (TREF) is 90% by weight or more based on the total amount of the ethylene / α-olefin copolymer. The resin composition for sound-insulating carpet backing for vehicles according to any one of claims 1 to 3, characterized in that: 5. The ethylene / α-olefin copolymer is obtained by copolymerizing ethylene and α-olefin using a metallocene-based catalyst as a polymerization catalyst. The resin composition for a sound insulating carpet backing for vehicles according to any one of claims 1 to 4. 6. An ethylene / α-olefin copolymer comprising 15 to 60% by weight of a coagulant and an inorganic filler which are compatible with the ethylene / α-olefin copolymer. 6. The resin composition for sound-insulating carpet backing for vehicles according to claim 1, wherein the resin composition is obtained by mixing 40 to 85% by weight of an inorganic filler mixture containing 70% by weight or more of an agent. .