JP2002309106A - Flame-retardant thermoplastic resin composition and flame-retardant resin molding - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a flame-retardant resin composition which does not contain a halogen, phosphorus, antimony and the like, and has sufficient flame retardancy, with controlled generation of a corrosive gas during molding and processing, and with reduced generation of an irritative gas, a corrosive gas and the like on burning. SOLUTION: The resin composition is obtained by blending 100 mass pts. of a thermoplastic resin with at least one material selected from the group consisting of 0.05-50 mass pts. of a swelling clay mineral treated with an organic substance, 0.05-50 mass pts. of a silicon compound, and 0.05-20 mass pts. of a metal compound.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a flame-retardant thermoplastic resin composition and a molded article formed from the flame-retardant thermoplastic resin composition. More specifically, without impairing the moldability and thermal stability of the thermoplastic resin composition, improve the flame retardancy, and halogenated flame retardants such as chlorine and bromine compounds and phosphorus-based flame retardants such as phosphate esters. The present invention relates to a flame-retardant thermoplastic resin composition containing no flame retardant and a molded article.

[0002]

2. Description of the Related Art Along with the tightening of flame-retardant regulations, flame-retardant technology for resins has become an important technology in various fields, especially in OA equipment such as printers and copiers, computers and word processing equipment. Is an important issue. US Underwriters Laboratories (Underwriter L
UL combustion test (U
In order for the resin to be ranked at a high flame retardancy level in L94), it is necessary that the test piece does not drip during the UL burning test, and in order to prevent fire spread in an actual fire, it is necessary to prevent the resin from dropping. This is an important issue.

[0003] Many methods for flame retarding resins have been proposed. For example, as a method for making a thermoplastic resin flame-retardant using a swellable silicate, thermoplastic resin / phosphorous flame retardant /
Method for combining layered silicate (Japanese Patent Laid-Open No. 10-06016)
No. 0) has been proposed. Also, a method of combining a polyolefin resin / organically treated swellable clay mineral / phosphorus flame retardant / metal salt (Japanese Patent Laid-Open No. 11-228748), thermoplastic polyester / halogenated organic flame retardant / antimony oxide A method of combining / organic clay / fluorocarbon (JP-A-11-189710) is known.

Further, as a method for making a cyclic polyolefin-based resin flame-retardant, a method of adding a halogen-based flame retardant such as bis (pentabromophenyl) ethane (Japanese Patent Application Laid-Open No.
JP-A No. 1-140282), a method of adding a phosphorus-based flame retardant such as a phosphate ester and a metal oxide-based flame retardant such as antimony oxide to a resin (Japanese Patent Laid-Open No. 11-106597).

[0005] However, in the case of phosphorus-based flame retardants, in order to impart sufficient flame retardancy to the resin, it may be necessary to add a large amount of the flame retardant, and as a result, the mechanical strength of the obtained molded article decreases, It may be difficult to put into practical use.
There is also concern about environmental pollution due to overnutrition of soil and rivers.

Further, the method using a halogen-based / antimony-based flame retardant has been widely used in the past. However, since a large amount of bromine and chlorine-based compounds are blended, harmful substances containing bromine and chlorine are generated at the time of molding and burning. Gas may be generated, and the generated gas may corrode equipment or generate dioxin harmful to the human body. in addition,
Antimony compounds may cause environmental problems.

[0007]

DISCLOSURE OF THE INVENTION The present invention has been made in view of the above situation, and does not contain halogen, phosphorus, antimony, etc., and has not only sufficient flame retardancy, but also molding An object of the present invention is to provide a flame-retardant resin composition in which the generation of corrosive gas during processing is suppressed and the generation of irritating gas and corrosive gas during combustion is reduced. Another object of the present invention is to provide a molded article obtained by molding a flame-retardant resin composition having such characteristics.

[0008]

According to the present invention, there is provided an organically treated swelling clay in an amount of 0.05 to 50 parts by mass based on 100 parts by mass of a thermoplastic resin. Mineral, at least one compound selected from the group consisting of 0.05 to 50 parts by mass of a silicone compound and 0.05 to 20 parts by mass of a metal oxide. A flame-retardant thermoplastic resin composition is provided.

In the present invention, an organically treated swellable clay mineral, a silicone compound and a metal oxide are used as the flame retardant. Since these flame retardants are not halogen compounds, they do not contain bromine and chlorine. Therefore, no harmful gas containing bromine and chlorine is generated at the time of molding or burning, and generation of dioxin is suppressed. Further, since these flame retardants are not antimony compounds, there is no concern about environmental problems. Furthermore, since these flame retardants are not phosphorus-based compounds, the resulting molded articles have sufficient mechanical strength. In addition, there is no concern about environmental pollution due to overnutrition of soil and rivers.

As a result, a flame-retardant resin composition which has sufficient flame retardancy, suppresses the generation of corrosive gas during molding, and reduces the generation of irritating gas and corrosive gas during combustion Things can be provided.

[0011]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail.

The thermoplastic resin used in the present invention is not particularly limited as long as it can be melted and molded. For example, polyolefin, polyamide, polycarbonate, polyphenylene oxide,
Examples include polystyrene, acrylonitrile / butadiene / styrene (ABS), polyester, polyacetal, and the like, or a blend thereof, and a copolymer thereof.

The polyolefin is a homopolymer of α-olefin or a copolymer thereof, and specific examples thereof include low density polyethylene, medium density polyethylene, high density polyethylene, polypropylene, polystyrene, polybutene, and poly-4-methyl. Lupentene-1, ethylene-propylene random copolymer, or block copolymer,
Copolymers of ethylene and other copolymerizable monomers are included.

In particular, by using a cyclic olefin resin as the thermoplastic resin, it is possible to obtain a flame-retardant resin composition having a good balance of non-environmental pollution, safety, heat resistance, mechanical properties and moldability. it can.

As the cyclic olefin-based resin, a ring-opened polymer of a norbornene-based monomer or a hydrogenated product thereof, a copolymer of a norbornene-based monomer and an α-olefin, and the like are used. Specific examples of the cyclic olefin repeating unit include norbornene-based monomer repeating units such as norbornene and tetracyclododecene, monocyclic olefin-based monomer repeating units such as cyclopentene and cyclohexene, and cyclopentadiene and cyclohexadiene. And a cyclic conjugated diene repeating unit.

From the viewpoint of heat resistance, the proportion of the cyclic olefin monomer units in the repeating units of the cyclic olefin resin is preferably at least 50 mol%.

As the α-olefin, ethylene, propylene, 1-hexene, 4-methyl-1-pentene, 1
-Octene, 1-butene, 1-pentene and the like.

Commercially available products include cyclic olefin polymers obtained by ring-opening polymerization of a norbornene-based monomer and hydrogenation (Nippon Zeon Co., Ltd.)
(Trade name: ZEONEX), a cyclic olefin polymer having an ester group introduced into a side chain (JSR Corporation)
(Trade name: ARTON), cyclic olefin polymer having a tricyclodecane ring in the main chain obtained by addition polymerization of cyclic olefin and ethylene or propylene (trade name: APEL, manufactured by Mitsui Petrochemical Co., Ltd.) No.

As the polyamide, nylon 4, nylon 6, nylon 6/6, nylon 4/6, nylon 1
2, nylon 6/10 and the like. Examples of the polyester include polyethylene terephthalate and polybutylene terephthalate.

By using a polystyrene resin as the thermoplastic resin, a flame-retardant resin composition having particularly excellent moldability can be obtained.

Further, by using a polypropylene resin as the thermoplastic resin, a flame-retardant resin composition having particularly excellent safety can be obtained.

The organically treated swellable clay compound used in the present invention is preferably a compound in which an organic quaternary onium ion is inserted (intercalated) between layers of the swellable clay compound. An ammonium ion, a phosphonium ion, a sulfonium ion or the like having an aromatic or aromatic hydrocarbon group is preferred.

Since these organically treated swellable clay minerals have a hydrocarbon group in the molecule, they have good compatibility with the resin, and when added to the resin, the transparency is not impaired and the mechanical strength is low. Does not drop.

The swellable clay mineral is not particularly limited as long as it is a clay mineral into which organic ions can be introduced.
Examples include layered silicates such as smectite, vermiculite, halosite, and mica. These may be used alone or in combination of two or more.

Among these swellable clay minerals, smectite has an appropriate charge density between layers, and can easily introduce various organic cations, and can increase the amount of the introduced organic cations. Therefore, it is preferable because the dispersibility of the clay mineral is improved and the flame retardancy can be effectively exhibited.
In particular, among the clay minerals of smectite, montmorillonite and hectorite exhibit the maximum flame retardancy.

The average particle diameter of the organically treated swellable clay mineral is 0.1 μm from the viewpoint of improving dispersibility and accompanying fire retardancy and mechanical properties during burning of the thermoplastic resin composition. It is preferably in the range of not less than 300 μm and not more than 300 μm. When the particle size is 0.1 μm or more, dust generated when the particles are dispersed in the material can be suppressed, and good workability can be realized. If the particle size is 300 μm or less,
Sufficient mechanical strength of the molded product can be realized.

As a commercially available organically treated swellable clay compound, an organic bentonite (trade name) obtained by subjecting montmorillonite, which is a typical example of a smectite clay mineral, to an organic modification is available from Toyohyun Yoko Co., Ltd. : Esven series, product name: Organite series). In addition, there is a product obtained by subjecting montmorillonite to ion exchange treatment with a quaternary alkylammonium ion, such as Cloisite 6A (trade name) manufactured by Southern Clay Product.

The amount of the organically treated swellable clay mineral is 0.05 parts by mass or more with respect to 100 parts by mass of the thermoplastic resin composition, from the viewpoint of achieving sufficient flame retardancy. 1 part by mass or more is more preferable, and 1 part by mass or more is further preferable. On the other hand, it is 50 parts by mass or less, and more preferably 30 parts by mass or less. When the amount is 50 parts by mass or less, sufficient fluidity during molding of the thermoplastic resin composition can be ensured, and the appearance and mechanical strength of the obtained molded article can be improved.

As the silicone compound used in the present invention, a (meth) acrylic group-containing polysilicone is preferred because it reacts at the time of combustion (high temperature) and exhibits flame retardancy.

More specifically, the repeating structural unit (M unit) represented by the general formula (I) is from 10 mol parts to 75 mol parts and the repeating structural unit (D
Unit), 80 mol parts or less of the repeating structural unit (T unit) represented by the general formula (III), and 15 repeating units (Q unit) of the general formula (IV).
Polysilicones containing at least one of the following molar parts are preferred.

[0031]

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[0032]

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[0033]

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[0034]

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In the formula, R ^{1 to} R ^{6 each} represent an alkyl group having 1 to 14 carbon atoms, a substituted alkyl group having 1 to 14 carbon atoms,
14, selected from an organic functional group consisting of an alkoxyl group, an aryl group and a (meth) acryl group;
At least one of the organic functional groups (R) in the repeating structural unit contained in the polysilicone is a (meth) acryl group. The bond between Si is Si-O-Si.

Examples of the alkyl group include a methyl group, an ethyl group, a propyl group and a butyl group; examples of the substituted alkyl group include a trifluoropropyl group; Examples of the aryl group include a phenyl group, a tolyl group, and a naphthyl group; and the term (meth) acryl group refer to an acryl group and / or a methacryl group.

When the polysilicone contains a T unit and / or a Q unit, the polysilicone is crosslinked. If necessary, the crosslinked silicone can be used.

Further, the silicone compound used in the present invention is composed of M units, D units, T units and Q units, wherein the T units occupy not more than 80 mol% of the total siloxane units, and the Q units are siloxane units. It is preferred that it accounts for 15 mol% or less of the whole unit from the viewpoint of moldability and flame retardancy.

In addition, it is preferred from the viewpoint of flame retardancy that 10 mol% or more of the organic functional groups (R) in the silicone compound are aryl groups such as phenyl groups. In addition,
Examples of commercially available (meth) acrylic group-containing polysilicones include DC4-7081 (trade name) manufactured by Dow Corning Toray Silicone Co., Ltd.

The addition amount of the silicone compound is set to 0.05 parts by mass or more, more preferably 0.1 parts by mass or more, from the viewpoint of achieving sufficient flame retardancy with respect to 100 parts by mass of the thermoplastic resin. 1 part by mass or more is more preferable. 5
0 parts by mass or less, and more preferably 30 parts by mass or less.
When the amount is 50 parts by mass or less, sufficient fluidity during molding of the thermoplastic resin composition can be ensured, and the appearance and mechanical strength of the obtained molded article can be improved.

The metal oxide used in the present invention includes:
For example, magnesium oxide, aluminum oxide, silicon oxide, calcium oxide, titanium oxide, vanadium oxide,
Examples include chromium oxide, manganese oxide, iron oxide, cobalt oxide, nickel oxide, copper oxide, and zinc oxide. These may be used alone or in combination of two or more.

The compounding amount of the metal oxide is selected from thermoplastic resin 10
From the viewpoint of realizing sufficient flame retardancy with respect to 0 parts by mass,
The content is 0.05 parts by mass or more, and more preferably 0.1 parts by mass or more. On the other hand, it is 20 parts by mass or less, more preferably 10 parts by mass or less. When the amount is 20 parts by mass or less, sufficient fluidity during molding of the thermoplastic resin composition can be secured, and the appearance and mechanical strength of the obtained molded article can be improved.

Although the metal oxide is effective when used alone, it is more effective to use the metal oxide in combination with a swelling clay mineral or a silicone compound which has been treated organically, if the metal oxide has sufficient flame retardancy and mechanical properties. Can be compatible. More preferably, all of the organically treated swellable clay mineral, silicone compound and metal oxide are used in combination.

When a plurality of flame retardants are used, the total amount of the flame retardants is preferably 0.1 part by mass or more from the viewpoint of realizing sufficient flame retardancy with respect to 100 parts by mass of the thermoplastic resin. Further, the amount is preferably 50 parts by mass or less. When the amount is 50 parts by mass or less, sufficient fluidity during molding of the thermoplastic resin composition can be ensured, and the appearance and mechanical strength of the obtained molded article can be improved.

Polytetrafluoroethylene having a fibril-forming ability is used as an agent for preventing dripping of the molten resin during combustion from 0.01 to 100 parts by mass of the thermoplastic resin.
You may mix | blend 5 mass parts. When the amount is 0.01 parts by mass or more, dripping is sufficiently prevented, and when the amount is 5 parts by mass or less, sufficient mechanical strength of the obtained molded body can be secured.

Examples of the polytetrafluoroethylene having the fibril type performance include Teflon 6-J (trade name) manufactured by Mitsui DuPont Fluorochemicals Co., Ltd .;
03, polyflon F201, polyflon MPA, polyflon FA-100 (trade name); CD036 (trade name) manufactured by Asahi ICI Fluoropolymers Co., Ltd .; and Algoflon F5 (trade name) manufactured by Montefluos Corporation. These polytetrafluoroethylenes may be used alone or in combination of two or more.

In order to improve weather resistance and the like,
An ultraviolet absorber or the like can be added. Further, an antistatic agent may be used for the purpose of preventing dust adhesion and generation of static electricity. In addition, for example, a pigment or dye for coloring, an antiblocking agent, a natural oil, a synthetic oil, a wax, or the like may be added. These compounding agents may be used alone or in combination of two or more kinds, and the compounding amount is selected within a range not to impair the object of the present invention.

The flame-retardant resin composition can be produced, for example, by dry blending each component with a tumbler, melt-mixing with a Banbury mixer, a kneader, a twin-screw extruder, or the like, and cutting into pellets. The flame-retardant resin composition thus obtained is then formed into a tube or sheet by extrusion molding or the like; into a film or the like by inflation or T-die molding; or by injection molding or compression molding or the like. It can be processed into size and shape. The obtained molded article has excellent flame retardancy in addition to the fact that the resin is hardly carbonized and hardly deteriorated.

Although the specific use of the molded article of the present invention is not particularly limited, for example, the use of flame-retardant materials such as copier exterior materials, printer exterior materials, personal computer exterior materials, electric appliances, furniture, and home appliances. Can be used for all.

[0050]

EXAMPLES The present invention will be described below in more detail with reference to Examples and Comparative Examples, but the present invention is not limited to the following Examples.

Unless otherwise specified, “parts” and “%” represent “parts by mass” and “% by mass”, respectively.
Commercially available high-purity reagents were used.

(Evaluation of Flame Retardancy) A corn calorimeter (product name: CONE3, 100 mm × 100 mm × 3 mm) was applied to a plate-like test piece in accordance with ASTM E1354.
Irradiation of radiant heat of 30 kW / m ² by ATLAS Co., Ltd., the maximum heat generation rate PHRR (combustion per unit area and unit time of sample, unit: kW /
m ² ) and the total heating value THR (MJ / m ² ) were measured to evaluate its flame retardancy. The smaller these values are, the more the combustion is suppressed.

(Examples 1 to 12, Comparative Example 1) Flame-retardant cyclic olefin resin compositions were obtained at the compounding ratios shown in Table 1. That is, 100 parts of cyclic polyolefin (trade name: ZEONEX E48R, manufactured by Zeon Corporation) and organic bentonate (trade name: Cloisite 6A, manufactured by Toyojun Yoko Co., Ltd.) as an organically treated swellable clay mineral.
And a silicone compound (manufactured by Dow Corning Toray Silicone Co., Ltd., trade name: DC 4-7081), and copper (I) oxide (manufactured by Soekawa Riken Co., Ltd., cuprous oxide, Cu)
₂ O) and titanium oxide (manufactured by Ishihara Sangyo Co., Ltd., trade name:
TTO-51 (C), TiO ₂ ) and a twin screw extruder (manufactured by Nippon Steel Works, Ltd., product name: TE) at the compounding ratio shown in Table 1.
X30α) and melt-mixed at a cylinder temperature of 280 ° C. to obtain resin pellets having each composition.

The obtained pellets were subjected to an injection molding machine (manufactured by FANUC Co., Ltd., product name: ROBOSHOT α-150).
Was injection-molded at a cylinder temperature of 280 ° C. and a mold temperature of 80 ° C. to obtain a plate-shaped test piece of 100 mm × 100 mm × 3 mm.

The flame retardancy was evaluated using the obtained test pieces, and the results are shown in Table 1.

[0056]

[Table 1]

When Examples 1 to 3 and Comparative Example 1 are compared,
It can be seen that when the organically treated swelling clay mineral is added, the maximum heat release rate PHRR is greatly reduced, and the calorific value THR also tends to be reduced.

In Examples 1 to 3, the dispersibility of the organically treated swellable clay mineral in the cyclic olefin resin was good, so that the obtained 3 mm thick test piece was transparent.

Further, from the results of Examples 4 to 8, it can be seen that when a silicone compound and / or a metal oxide is added to a system to which an organically treated swelling clay mineral is added, flame retardancy is further improved. You.

In addition, it can be seen from the results of Examples 9 to 11 that the addition of the silicone compound significantly reduces the maximum heat generation rate PHRR. Also, the results of Example 12 show that the addition of a metal oxide to a system to which a silicone compound has been added improves flame retardancy.

The compositions of Examples 1 to 12 had good productivity and moldability, and also had sufficient mechanical properties such as impact resistance.

As described above, the moldability and impact resistance are impaired by adding one or more additives selected from organically treated swellable clay minerals, silicone compounds and metal oxides to the cyclic olefin resin. It has been found that high flame retardancy can be realized without any problem. Further, since the obtained flame-retardant cyclic olefin resin composition does not contain a flame retardant composed of chlorine, bromine and a phosphorus compound, there is no fear of generating harmful gas containing bromine and chlorine caused by the flame retardant during combustion. It also proved to have excellent performance in terms of environmental protection.

(Examples 13 to 22, Comparative Examples 2 to 6) Table 2
The flame-retardant thermoplastic resin composition was obtained at the compounding ratio shown in Table 1. Examples of the thermoplastic resin include polypropylene (PP, manufactured by Idemitsu Petrochemical Co., Ltd., trade name: Idemitsu Polypro J-2003G),
Polystyrene (PS, manufactured by Idemitsu Petrochemical Co., Ltd., trade name:
Idemitsu Styrol IT41), polycarbonate (PC,
Nippon GE Plastics Co., Ltd., trade name: Lexan 141R), modified polyphenylene ether (PPO, Japan GE Plastics Co., Ltd., trade name: Noryl 11)
5), polyamide (nylon 6, made by Unitika, trade name:
A1025) was used.

An organic bentonite (Souther) was used as an organically treated swellable clay mineral in 100 parts of the resin.
n Clay Product Inc. Product name:
Cloisite 6A) and a silicone powder having a methacryl group as a silicone compound (manufactured by Dow Corning Toray Silicone Co., Ltd., trade name: DC 4-70)
81) and copper oxide (I) (cuprous oxide, Cu ₂ O, manufactured by Soegawa Rikagaku Co., Ltd.) as a metal oxide in the number shown in Table 2. The obtained mixture is subjected to a twin-screw extruder (Co., Ltd.)
It was melt-kneaded using Nippon Steel Works, product name: TEX30α) to obtain resin pellets having each composition.

The obtained pellets were subjected to an injection molding machine (manufactured by FANUC CORPORATION, product name: ROBOSHOT α-150).
Injection molding using 100mm x 100mm x 3mm
A plate-shaped test piece was obtained.

The cylinder temperature during melt-kneading and injection molding and the mold temperature during injection molding were as follows: Thermoplastic resin cylinder temperature (° C.) Mold temperature (° C.) PP 220 60 PS 200 50 PC 260 80 PPE 280 80 Nylon 6 250 60.

The flame retardancy was evaluated using the obtained test pieces, and the results are shown in Table 2.

[0068]

[Table 2]

As shown in Table 2, the thermoplastic resin to which the organically treated swelling clay mineral and the silicone compound were added (Examples 13 to 22) were not added (Comparative Examples 2 to 22).
It can be seen that the maximum heat generation rate PHRR is significantly reduced as compared with 6). Further, it can be seen that the addition of cuprous oxide further improves the flame retardancy.

[0070]

According to the present invention, a thermoplastic resin composition obtained by blending a swellable clay mineral organically treated with a thermoplastic resin, a silicone compound and a metal oxide can be used without impairing impact resistance and moldability. With high flame retardancy, chlorine, bromine,
Since it does not contain a flame retardant composed of a phosphorus compound, there is no concern about generation of harmful gases including bromine and chlorine caused by the flame retardant during combustion, and it also has excellent performance in terms of environmental protection.

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Claims (11)

[Claims] [Claim 1] With respect to 100 parts by mass of a thermoplastic resin,
0.05 to 50 parts by weight of an organically treated swellable clay mineral, 0.05 to 50 parts by weight of a silicone compound, and 0.05 to 20 parts by weight of a metal oxide A flame-retardant thermoplastic resin composition comprising at least one compound selected from the group consisting of: 2. The flame-retardant thermoplastic resin composition according to claim 1, wherein the thermoplastic resin is an olefin resin. 3. The flame-retardant thermoplastic resin composition according to claim 2, wherein the olefin resin is a cyclic olefin resin. 4. The flame-retardant thermoplastic resin composition according to claim 2, wherein the olefin resin is a polystyrene resin. 5. The flame-retardant thermoplastic resin composition according to claim 2, wherein the olefin resin is a polypropylene resin. 6. The swellable clay mineral that has been organically treated,
The flame-retardant thermoplastic resin composition according to any one of claims 1 to 5, wherein the composition is a swellable clay mineral having organic onium ions inserted between layers. 7. The flame-retardant thermoplastic resin composition according to claim 1, wherein the swellable clay mineral is smectite. 8. The flame-retardant thermoplastic resin composition according to claim 7, wherein the smectite is at least one of montmorillonite and hectorite. 9. The flame-retardant thermoplastic resin composition according to claim 1, wherein the silicone compound is a (meth) acrylic group-containing polysilicone. 10. The metal oxide includes magnesium oxide, aluminum oxide, silicon oxide, calcium oxide,
10. At least one member selected from the group consisting of titanium oxide, vanadium oxide, chromium oxide, manganese oxide, iron oxide, cobalt oxide, nickel oxide, copper oxide and zinc oxide. The flame-retardant thermoplastic resin composition according to the above. 11. A flame-retardant resin molded product obtained by molding the flame-retardant thermoplastic resin composition according to claim 1 into a predetermined shape.