JPS6152853B2 - - Google Patents
Info
- Publication number
- JPS6152853B2 JPS6152853B2 JP8298879A JP8298879A JPS6152853B2 JP S6152853 B2 JPS6152853 B2 JP S6152853B2 JP 8298879 A JP8298879 A JP 8298879A JP 8298879 A JP8298879 A JP 8298879A JP S6152853 B2 JPS6152853 B2 JP S6152853B2
- Authority
- JP
- Japan
- Prior art keywords
- ethylene
- crosslinked
- flame
- sheet
- minutes
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 239000000203 mixture Substances 0.000 claims description 14
- 239000003063 flame retardant Substances 0.000 claims description 12
- 229920005672 polyolefin resin Polymers 0.000 claims description 10
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 5
- 238000004132 cross linking Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 5
- 229920001577 copolymer Polymers 0.000 description 4
- 230000000704 physical effect Effects 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 3
- 238000010894 electron beam technology Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- -1 polyethylene Polymers 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- VZNSVWKHKHDGCM-UHFFFAOYSA-N 3,3,4,4,4-pentafluoro-2-methylbutan-2-ol Chemical compound CC(C)(O)C(F)(F)C(F)(F)F VZNSVWKHKHDGCM-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 230000005865 ionizing radiation Effects 0.000 description 2
- 150000001451 organic peroxides Chemical class 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 239000011342 resin composition Substances 0.000 description 2
- UBRWPVTUQDJKCC-UHFFFAOYSA-N 1,3-bis(2-tert-butylperoxypropan-2-yl)benzene Chemical compound CC(C)(C)OOC(C)(C)C1=CC=CC(C(C)(C)OOC(C)(C)C)=C1 UBRWPVTUQDJKCC-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000004604 Blowing Agent Substances 0.000 description 1
- 239000004709 Chlorinated polyethylene Substances 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Natural products C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910000410 antimony oxide Inorganic materials 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- HAISMSJTPGJFIP-UHFFFAOYSA-N butyl 4-tert-butyl-4,5,5-trimethylhexaneperoxoate Chemical compound CCCCOOC(=O)CCC(C)(C(C)(C)C)C(C)(C)C HAISMSJTPGJFIP-UHFFFAOYSA-N 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- 239000012969 di-tertiary-butyl peroxide Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001038 ethylene copolymer Polymers 0.000 description 1
- 229920006226 ethylene-acrylic acid Polymers 0.000 description 1
- 229920006244 ethylene-ethyl acrylate Polymers 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 229920000554 ionomer Polymers 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Chemical class 0.000 description 1
- 239000002184 metal Chemical class 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920005670 poly(ethylene-vinyl chloride) Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Description
本発明は難燃性ポリオレフイン系樹脂架橋組成
物に関する。
近年、ゴム及びプラスチツクの各種材料として
の需要の増大に伴い、難燃性を要求されることが
多くなつた。特に難燃化が最も困難とされる材料
の一つであるポリオレフイン系樹脂架橋組成物の
場合、従来においては、架橋剤、架橋助剤よりな
る架橋系とハロゲン化物及び酸化アンチモンとの
組合わせによる難燃剤とを併用したものが一般的
であり、又、ゴム系架橋組成物の場合は、上記組
合わせの他、更に水酸化アルミニウム、無機充填
剤などを併用したものが最も効果があり、実用化
されている。
しかしながら、上記難燃剤による難燃化の為に
はこれを多量に配合せねばならないことや架橋遅
れによる架橋物の機械的物性の低下、架橋物表面
に難燃剤が滲出して粉を吹く、いわゆるブルーミ
ング現象を生じ、衛生上、外観上好ましいもので
はなかつた。
本発明者らは、上記欠点を改善するために種々
検討した結果、難燃剤兼架橋助剤としてジアリル
テトラブロモフタレートを用い、これをポリオレ
フイン系樹脂に配合することによりブルーミング
性がなく、しかも機械的物性に優れた難燃性架橋
樹脂組成物が得られることを見出し、本発明に至
つたものである。
即ち、本発明は、ポリオレフイン系樹脂にジア
リルテトラブロモフタレートを配合したことを特
徴とする難燃性ポリオレフイン系樹脂架橋組成物
である。
本発明のポリオレフイン系樹脂としては、高圧
法ポリエチレン、中低圧法ポリエチレン等の単独
重合体、エチレンと他の共重合可能な単量体との
共重合体、例えば、エチレン−酢酸ビニル共重合
体、エチレン−塩化ビニル共重合体、エチレン−
スチレン共重合体、エチレン−アクリル酸エチル
共重合体、エチレン−プロピレン共重合体、エチ
レン−プロピレン−ジエン共重合体など、エチレ
ンとアクリル酸のナトリウム、カリウムなどの金
属塩との共重合体であるエチレン−アクリル酸ア
イオノマー、エチレンに他の原子または原子団が
結合した重合体、例えば、塩素化ポリエチレンな
どがあり、これら樹脂の単独、またはこれらの混
合物あるいは実質的な主成分が上記樹脂である他
のポリマー（例えば、SBR、NBRなど）との混
合物が用いられる。
本発明に用いるジアリルテトラブロモフタレー
ト（以下DATBPと略記する）は、融点約110℃
を有する白色粉末状であり、パーオキサイドによ
り重合可能な化合物である。
上記DATBPの配合量は、ポリオレフイン系樹
脂100重量部に対して、DATBP1〜100重量部の
範囲が適当である。
DATBP量が１重量部未満では難燃剤として、
又架橋助剤としての効果が小さく実用性がない。
また100重量部をこえる場合は、ポリオレフイン
系樹脂の熱可塑的性質が失なわれ、硬くなつて成
形性も悪化し、更に価格面での経済性も損なわれ
るため好ましくない。
本発明の組成物には、その他に安定剤、充填
剤、可塑剤、滑剤、顔料、酸化防止剤、発泡剤、
他種難燃剤などがその使用目的に応じて添加でき
る。混合の方法としては、ロール、ニーダー、バ
ンバリーミキサーなどの通常の混合機が利用され
る。本発明の組成物の架橋は有機過酸化物による
方法あるいは電離性放射線を照射する方法によつ
て行なわれる。
有機過酸化物としては、ジクミルパ−オキサイ
ド、ジ−タ−シヤリ−ブチルパ−オキサイド、
１・３−ビス（タ−シヤリ−ブチルパ−オキシイ
ソプロピル）ベンゼン、４・４−ジ−タ−シヤリ
−ブチルパ−オキシバレリン酸−ｎ−ブチルエス
テル、１・１−ジ−タ−シヤリ−ブチルパ−オキ
シ−３・３・５−トリ−メチルシクロヘキサン、
α・α′−ビス（タ−シヤリ−ブチルパ−オキ
シ）−Ｐ−ジ−イソプロピルベンゼン、２・５−
ジメチル−２・５−ジ（タ−シヤリ−ブチルパ−
オキシ）ヘキシン−３などがあり、樹脂成分100
重量部に対して１〜15重量部の範囲で用いられ
る。架橋条件は、温度140〜200℃、時間１〜30分
間の範囲が適当である。
電離性放射線架橋の場合は、高エネルギー線と
してα線、β線、γ線、Ｘ線、加速化された陽子
線、電子線、中性子線などがあるが、一般的には
高エネルギー電子線照射機が使用され、組成物を
混合、成形した後、１〜50Mradの線量を照射さ
せることによつて架橋が行なわれる。
本発明の組成物は、電線被覆、ホース、型製
品、建材などの各種材料として利用される。
以下実施例によつて本発明を説明する。
実施例１〜３、比較例１〜２
表１に示す各配合物を８インチロールにて80〜
90℃で約15分間混練し、シート化した。これを
170℃、100Kg/cm2で15分間プレスし、約２mmの架
橋シートを得た。
得られた架橋シートを以下の方法によつて物性
テストを行ない、その結果を表１に示した。
引張試験：JISK6302に準ずる。
圧縮永久歪：120℃で72時間、25％圧縮後の歪
率。
ブルーミング試験：−５℃×20時間→80℃×20時
間の寒熱を２回繰り返した後の表面状態観察。
（評価）
〇 全くブルームなし。これを更に室温で２週
間放置後においても全くブルームなし。
× 寒熱１回後に既に多量にブルームしてい
る。
The present invention relates to a flame-retardant polyolefin resin crosslinked composition. In recent years, with the increase in demand for various materials such as rubber and plastic, flame retardancy has been increasingly required. Particularly in the case of crosslinked polyolefin resin compositions, which are one of the most difficult materials to make flame retardant, the conventional method is to combine a crosslinking system consisting of a crosslinking agent and a crosslinking aid with halides and antimony oxide. It is common to use flame retardants in combination, and in the case of rubber-based crosslinked compositions, in addition to the above combinations, aluminum hydroxide, inorganic fillers, etc. are the most effective and practically has been made into However, in order to achieve flame retardancy using the above-mentioned flame retardants, a large amount of the flame retardant must be blended, the mechanical properties of the cross-linked product deteriorate due to delayed cross-linking, and the flame retardant oozes out onto the surface of the cross-linked product, resulting in the formation of powder. A blooming phenomenon occurred, which was not desirable in terms of hygiene and appearance. As a result of various studies in order to improve the above-mentioned drawbacks, the present inventors have found that by using diallyltetrabromophthalate as a flame retardant and crosslinking aid, and blending this into a polyolefin resin, there is no blooming property, and the mechanical strength is improved. It was discovered that a flame-retardant crosslinked resin composition with excellent physical properties can be obtained, leading to the present invention. That is, the present invention is a flame-retardant polyolefin-based resin crosslinked composition characterized by blending diallytetrabromophthalate with a polyolefin-based resin. The polyolefin resin of the present invention includes homopolymers such as high-pressure polyethylene and medium-low pressure polyethylene, copolymers of ethylene and other copolymerizable monomers, such as ethylene-vinyl acetate copolymers, Ethylene-vinyl chloride copolymer, ethylene-
Copolymers of ethylene and metal salts of acrylic acid such as sodium and potassium, such as styrene copolymers, ethylene-ethyl acrylate copolymers, ethylene-propylene copolymers, and ethylene-propylene-diene copolymers. There are ethylene-acrylic acid ionomers, polymers in which ethylene is bonded to other atoms or atomic groups, such as chlorinated polyethylene, and these resins alone or in mixtures, or in which the substantial main component is the above resin. (e.g., SBR, NBR, etc.). Diallyltetrabromophthalate (hereinafter abbreviated as DATBP) used in the present invention has a melting point of approximately 110°C.
It is a white powdery compound that can be polymerized with peroxide. The appropriate amount of DATBP to be blended is in the range of 1 to 100 parts by weight based on 100 parts by weight of the polyolefin resin. When the amount of DATBP is less than 1 part by weight, it is used as a flame retardant.
Moreover, its effect as a crosslinking aid is small and is not practical.
If the amount exceeds 100 parts by weight, the polyolefin resin loses its thermoplastic properties, becomes hard, deteriorates moldability, and is also unfavorable in terms of cost efficiency. In addition, the composition of the present invention includes stabilizers, fillers, plasticizers, lubricants, pigments, antioxidants, blowing agents,
Other types of flame retardants can be added depending on the purpose of use. As a mixing method, a conventional mixer such as a roll, kneader, or Banbury mixer is used. Crosslinking of the composition of the present invention is carried out by a method using an organic peroxide or by irradiation with ionizing radiation. Examples of organic peroxides include dicumyl peroxide, di-tertiary butyl peroxide,
1,3-bis(tert-butylperoxyisopropyl)benzene, 4,4-di-tert-butyl peroxyvaleric acid-n-butyl ester, 1,1-di-tert-butyl peroxyisopropyl Oxy-3,3,5-tri-methylcyclohexane,
α・α′-bis(tertiary-butylperoxy)-P-di-isopropylbenzene, 2,5-
Dimethyl-2,5-di(tertiary-butylper-)
Oxy)Hexine-3 etc., resin component 100
It is used in a range of 1 to 15 parts by weight. Suitable crosslinking conditions are a temperature of 140 to 200°C and a time of 1 to 30 minutes. In the case of ionizing radiation crosslinking, high-energy rays include α-rays, β-rays, γ-rays, X-rays, accelerated proton beams, electron beams, and neutron beams, but generally high-energy electron beam irradiation is used. After mixing and shaping the composition using a machine, crosslinking is carried out by irradiation with a dose of 1 to 50 Mrad. The composition of the present invention is used as various materials such as electric wire coatings, hoses, molded products, and building materials. The present invention will be explained below with reference to Examples. Examples 1 to 3, Comparative Examples 1 to 2 Each of the formulations shown in Table 1 was rolled for 80~
The mixture was kneaded at 90°C for about 15 minutes to form a sheet. this
Pressing was carried out at 170° C. and 100 kg/cm 2 for 15 minutes to obtain a crosslinked sheet of approximately 2 mm. The obtained crosslinked sheet was subjected to physical property tests according to the following method, and the results are shown in Table 1. Tensile test: According to JISK6302. Compression set: Strain rate after 25% compression at 120℃ for 72 hours. Blooming test: Observation of surface condition after repeated heating and cooling at -5°C for 20 hours and then at 80°C for 20 hours. (Evaluation) 〇 No bloom at all. There was no bloom at all even after this was left at room temperature for two weeks. × A large amount of bloom has already occurred after one cold and fever.
【表】【table】
【表】
実施例４〜５、比較例３〜４
表２に示す各配合物を８インチロールにて110
〜120℃で10分間混練し、シート化した。実施例
４及び比較例３は、上記シートを170℃、100Kg/
cm2で15分間プレスし、厚み約２mmの架橋シートと
した。
実施例５及び比較例４は、上記混練シートを
100℃、100Kg/cm2で５分間プレスして厚み約２mm
とした後、冷却して取出し、三菱電機社製電子線
照射機で400KEV、10ｍＡの条件下、10Mradを
照射して架橋を行なつた。
上記各架橋シートを実施例１〜３と同様に物性
テストを行ない、その結果を表２に示した。[Table] Examples 4 to 5, Comparative Examples 3 to 4 Each formulation shown in Table 2 was rolled on an 8-inch roll to
The mixture was kneaded at ~120°C for 10 minutes and formed into a sheet. In Example 4 and Comparative Example 3, the above sheet was heated at 170℃ and 100Kg/
cm 2 for 15 minutes to form a crosslinked sheet with a thickness of about 2 mm. In Example 5 and Comparative Example 4, the above kneading sheet was
Press at 100℃ and 100Kg/cm 2 for 5 minutes to a thickness of approximately 2mm.
After that, it was cooled, taken out, and cross-linked by irradiation of 10 Mrad using an electron beam irradiation machine manufactured by Mitsubishi Electric under conditions of 400 KEV and 10 mA. The physical properties of each of the crosslinked sheets described above were tested in the same manner as in Examples 1 to 3, and the results are shown in Table 2.
【表】【table】
【表】
実施例６、比較例５
表３に示す各配合物を８インチロールにて80℃
℃で15分間混練し、シート化した。これを170
℃、100Kg/cm2で15分間プレスし、厚み約２mmの架
橋シートとした。架橋シートの物性テストを実施
例１〜３と同様に行ない、その結果を表３に示し
た。[Table] Example 6, Comparative Example 5 Each compound shown in Table 3 was rolled at 80°C using an 8-inch roll.
The mixture was kneaded at ℃ for 15 minutes to form a sheet. This is 170
It was pressed for 15 minutes at 100 kg/cm 2 at 100° C. to form a crosslinked sheet with a thickness of about 2 mm. The physical properties of the crosslinked sheet were tested in the same manner as in Examples 1 to 3, and the results are shown in Table 3.
【表】【table】
Claims (1)
モフタレートを配合したことを特徴とする難燃性
ポリオレフイン系樹脂架橋組成物。1. A flame-retardant polyolefin resin crosslinked composition characterized by blending diallytetrabromophthalate with a polyolefin resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8298879A JPS565841A (en) | 1979-06-29 | 1979-06-29 | Crosslinked composition of flame-retardant polyolefin-based resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8298879A JPS565841A (en) | 1979-06-29 | 1979-06-29 | Crosslinked composition of flame-retardant polyolefin-based resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS565841A JPS565841A (en) | 1981-01-21 |
| JPS6152853B2 true JPS6152853B2 (en) | 1986-11-14 |
Family
ID=13789590
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8298879A Granted JPS565841A (en) | 1979-06-29 | 1979-06-29 | Crosslinked composition of flame-retardant polyolefin-based resin |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS565841A (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0611823B2 (en) * | 1983-09-22 | 1994-02-16 | 昭和電工株式会社 | Polypropylene resin material |
| JPS60168740A (en) * | 1984-02-13 | 1985-09-02 | Showa Denko Kk | Polypropylene composition |
| JPH0735606B2 (en) * | 1984-12-28 | 1995-04-19 | 東レ株式会社 | Method for manufacturing polyester thermal shrinkage difference mixed yarn |
| JP2692513B2 (en) * | 1992-11-10 | 1997-12-17 | 東レ株式会社 | Method and apparatus for producing polyester fiber |
-
1979
- 1979-06-29 JP JP8298879A patent/JPS565841A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS565841A (en) | 1981-01-21 |
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