JPH03294314A - Methacrylic resin for optical information recording medium - Google Patents
Methacrylic resin for optical information recording mediumInfo
- Publication number
- JPH03294314A JPH03294314A JP2096857A JP9685790A JPH03294314A JP H03294314 A JPH03294314 A JP H03294314A JP 2096857 A JP2096857 A JP 2096857A JP 9685790 A JP9685790 A JP 9685790A JP H03294314 A JPH03294314 A JP H03294314A
- Authority
- JP
- Japan
- Prior art keywords
- methyl methacrylate
- information recording
- methacrylic resin
- optical information
- resin
- 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.)
- Pending
Links
- 230000003287 optical effect Effects 0.000 title claims abstract description 19
- 239000000113 methacrylic resin Substances 0.000 title claims abstract description 13
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical group COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229920001577 copolymer Polymers 0.000 claims abstract description 14
- KBLWLMPSVYBVDK-UHFFFAOYSA-N cyclohexyl prop-2-enoate Chemical group C=CC(=O)OC1CCCCC1 KBLWLMPSVYBVDK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011347 resin Substances 0.000 abstract description 7
- 229920005989 resin Polymers 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 3
- 239000012778 molding material Substances 0.000 description 8
- 238000001746 injection moulding Methods 0.000 description 6
- 238000000465 moulding Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 3
- 238000010557 suspension polymerization reaction Methods 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000012662 bulk polymerization Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000005395 methacrylic acid group Chemical group 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 1
- KZCOBXFFBQJQHH-UHFFFAOYSA-N octane-1-thiol Chemical compound CCCCCCCCS KZCOBXFFBQJQHH-UHFFFAOYSA-N 0.000 description 1
- 239000008188 pellet 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
- 239000002685 polymerization catalyst Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はビデオディスク等の光学式情報記録体用メタク
リル樹脂に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a methacrylic resin for optical information recording media such as video discs.
メタクリル樹脂は成形性がよく、透明性に優れ、有用な
光学特性を示すため、種々の光学機器用途に使用できる
ことは知られておシ、最近はそのすぐれた性質を生かし
、ビデオディスク等の光学式情報記録体用基板として使
用されている。Methacrylic resin has good moldability, excellent transparency, and exhibits useful optical properties, so it is known that it can be used in a variety of optical equipment applications. It is used as a substrate for type information recording bodies.
光学式情報記録体用基板としては、光学歪が小さく、優
几た耐熱性と成形性を併せ持った樹脂材料が要求される
上、近年、ビデオディスクの需要拡大により、市場では
射出成形におけるディスクの生産性向上、即ち成形サイ
クルの短縮ができることが強く望まれている。Substrates for optical information recording media require resin materials with low optical distortion, excellent heat resistance, and moldability.In recent years, with the increasing demand for video discs, the market has become increasingly popular for injection molding discs. It is strongly desired to improve productivity, that is, to shorten the molding cycle.
光学式情報記録体用メタクリル樹脂としては、メチルメ
タクリレートとエチルアクリレート(特開昭57−12
5208号)が提案さ几ている。As methacrylic resins for optical information recording media, methyl methacrylate and ethyl acrylate (JP-A-57-12
No. 5208) has been proposed.
しかしながら、メチルメタクリレ−トドエチルアクリレ
ートを用いた場合、流動性を向上させると光学歪は減少
するが、耐熱性や機械的強度が低下するという欠点が表
面化してくるため、成形生産性を向上させることは困難
であった。However, when using methyl methacrylate-doethyl acrylate, improving fluidity reduces optical distortion, but disadvantages such as a decrease in heat resistance and mechanical strength become apparent, so it is necessary to improve molding productivity. It was difficult to do so.
現在、光学式情報記録体用基板、4!にビデオディスク
、オーディオディスクは、主に射出成形により製造され
ているが、その生産性を考慮した場合、樹脂の耐熱性及
び流動性により、その成形サイクルが決定されている。Currently, there are 4 optical information recording substrates! Video discs and audio discs are mainly manufactured by injection molding, but when considering productivity, the molding cycle is determined by the heat resistance and fluidity of the resin.
射出成形における生産性向上のためには、光学歪が小さ
く優れ九透明性や機械的強度を損なうことなく、樹脂の
流動性を陶土させ、更に射出成形時にお行る冷却時間短
縮の目的で耐熱性を向上させる必要があるが、既存の成
形材料では耐熱性を向上させると、流動性の低下や機械
的強度の低下を伴う問題点を有しているのが現状である
。In order to improve productivity in injection molding, it is necessary to improve the fluidity of the resin without compromising transparency or mechanical strength, and to reduce the cooling time during injection molding. Although it is necessary to improve the heat resistance of existing molding materials, the current problem is that improving the heat resistance of existing molding materials causes problems such as a decrease in fluidity and a decrease in mechanical strength.
本発明者らはこのような現状に鑑み、光学式情報記録体
用成形材料としてのメタクリル樹脂に着目して種々検討
したところ、上述の問題点のない光学式情報記録体用基
板が生産性よく製造することができることを見出し本発
明に到達した。In view of the current situation, the present inventors conducted various studies focusing on methacrylic resin as a molding material for optical information recording media, and found that a substrate for optical information recording media that does not have the above-mentioned problems can be produced with high productivity. The present invention was achieved by discovering that it can be manufactured.
即ち、本発明はメチルメタクリレート単位80〜995
重量4とシクロヘキシルアクリレートI15〜20重量
憾との共重合体であることを特徴とする光学式情報記録
体用メタクリル樹脂である。That is, the present invention has 80 to 995 methyl methacrylate units.
This methacrylic resin for optical information recording media is characterized by being a copolymer of 4 in weight and 15 to 20 in weight of cyclohexyl acrylate I.
本発明のメタクリル樹脂において共重合比率がこの範囲
外では、成形物の耐熱性及び量産時の生産性を併せもつ
ことができない。即ち、メチルメタクリレート単位が9
9.5重量鴫を越えると、樹脂の成形流動性を維持する
ために分子量を低くしなければならず、その結果、機械
的強度が低下する。一方、シクロヘキシルアクリレート
単位が20重f4を越えると耐熱性の著しく劣ったもの
と表り好ましくない。If the copolymerization ratio of the methacrylic resin of the present invention is outside this range, the molded product will not have both heat resistance and productivity during mass production. That is, the number of methyl methacrylate units is 9.
If the weight exceeds 9.5, the molecular weight must be lowered to maintain molding fluidity of the resin, resulting in a decrease in mechanical strength. On the other hand, if the number of cyclohexyl acrylate units exceeds 20 f4, the heat resistance will be extremely poor, which is not preferable.
また、本発明のメタクリル樹脂のメルトフローレートは
、五8TM−Dj23Bに基づき、荷重五akgで測定
した値で(15〜501F/10分の範囲にあるのが好
ましい。メルトフローレートがCL5f/1o分よシ小
さいと金型からの情報の転写性が劣り、尚且つ、成形物
の光学歪が大きくなりやすい。一方、50?/10分よ
り大きいと機械的強度が低下する傾向にある。Further, the melt flow rate of the methacrylic resin of the present invention is a value measured at a load of 5 kg based on 58TM-Dj23B (preferably in the range of 15 to 501F/10 minutes.The melt flow rate is CL5f/1o If the distance is too small, the transferability of information from the mold will be poor, and the optical distortion of the molded product will tend to increase.On the other hand, if it is larger than 50?/10 minutes, the mechanical strength will tend to decrease.
更に、本発明のメタクリル樹脂の熱変形温度は、成形時
及び使用時の熱変形防止のために、187M−D648
に基づき荷重1a56k11で測定した値で70℃以上
であることが好ましい。Furthermore, the heat distortion temperature of the methacrylic resin of the present invention is 187M-D648 in order to prevent heat distortion during molding and use.
It is preferable that the temperature is 70°C or higher as measured under a load of 1a56k11.
熱変形温度が70℃より低い場合には成形体の耐熱性が
劣り、特に成形時及び使用時の熱変形が大きくな)好ま
しくない。より好ましくは80℃以上である。If the heat deformation temperature is lower than 70° C., the heat resistance of the molded product will be poor, and in particular, the heat deformation during molding and use will be large (unpreferably). More preferably, the temperature is 80°C or higher.
上記したような条件を満足するメタクリル樹脂を使用す
ることにより、従来より本生産性向上可能な光学歪の小
さい優れた透明性、機械強度を有する成形体を得ること
ができる。By using a methacrylic resin that satisfies the above-mentioned conditions, it is possible to obtain a molded article having excellent transparency and mechanical strength with small optical distortion, which can improve productivity compared to conventional molded articles.
本発明の成形材料の製造は、懸濁重合、塊状重合、溶液
重合葬のアクリル樹脂製造の公知の方法を用いることが
できる。本発明の共重合体には必要に応じて、安定剤、
離型剤、滑剤、可塑剤、染料等を添加することも可能で
ある。The molding material of the present invention can be produced using known methods for producing acrylic resins such as suspension polymerization, bulk polymerization, and solution polymerization. The copolymer of the present invention may optionally contain a stabilizer,
It is also possible to add release agents, lubricants, plasticizers, dyes, etc.
このようKして得らnた本発明の成形材料は、射出成形
、圧縮成形いずれ本適用することができる。The molding material of the present invention thus obtained can be applied to either injection molding or compression molding.
以下、実施例によシ本発明を具体的に説明する。なお、
各特性値の測定は次の方法で行った。Hereinafter, the present invention will be specifically explained using examples. In addition,
Measurement of each characteristic value was performed by the following method.
■ 熱変形温度(EDT )
187M−D648に準じて荷重1a56に9で測定し
た。(2) Heat distortion temperature (EDT) Measured at a load of 1a56 to 9 according to 187M-D648.
■ メルトフローレート(MPR)
ムSTM−D1258に準じて荷重五8kgで測定した
。(2) Melt flow rate (MPR) Measured under a load of 58 kg according to STM-D1258.
■ 引張強度、引張伸度
日清樹脂社製P8−60 Mによりダンベルム型試験片
を射出成形し、A S T M−D658に準じて測定
した。(2) Tensile strength and tensile elongation Dumbbell-shaped test pieces were injection molded using P8-60M manufactured by Nisshin Jushi Co., Ltd., and measured according to ASTM-D658.
■ 光線透過率
各機製作所社製M−200ダイナメルタによ)φ300
−のディスク(1,2■t)を射出成形(シリンダー温
度260℃)により作製し、中心より7exaの地点の
透過率を島津製作所社製UV−160Aにより500〜
900nmの領域で測定した。■ Light transmittance (by M-200 Dynamelta manufactured by Kakaki Seisakusho Co., Ltd.) φ300
- A disk (1,2 t) was produced by injection molding (cylinder temperature 260°C), and the transmittance at a point 7exa from the center was measured at 500 ~ 500 using UV-160A manufactured by Shimadzu Corporation.
Measurement was performed in the 900 nm region.
■ 複屈折(retaraatlon)上記ディスク成
形品の中心より73の地点の複屈折(retaraat
ion)を偏光顕微鏡(Nikon。■ Birefringence (retaraatlon) Birefringence (retaraatlon) at a point 73 from the center of the disc molded product.
ion) using a polarizing microscope (Nikon).
OF、TlPEl0T−POL、 BF、NARMOM
T 00MPEN5ATOR−使用波長546 nm、
lsingle pass ) Kよ)測定した。OF, TlPEl0T-POL, BF, NARMOM
T 00MPEN5ATOR-Used wavelength 546 nm,
lsingle pass) K) was measured.
また、実施例の「4」、「部」はそれぞれ「重量部」、
「重量部」を示すものである。In addition, "4" and "parts" in Examples are "parts by weight", respectively.
It indicates "parts by weight."
実施例1〜3
メチルメタクリレートとシクロヘキシルアクリレートを
第1表に示す割合の単量体混合物100部に、n−オク
チルメルカプタンの(135部を溶解し、重合触媒とし
てラウロイルパーオキサイドα44部、離型剤としてス
テアリルアルコールα1部、懸濁重合分散剤としてメタ
クリル酸メチルと3−メタクリロイルオキシプロパルス
ルホン酸カリウムの共重合体α01部、硫酸す) IJ
ウムIIL15部、分散媒として水145部を攪はん機
、温度針付きガラス製フラスコ重合装置に混入し、80
℃で重合させ同温がピークに達した後95℃で30分間
保持後冷却し′、濾過、水洗、乾燥することにより、ビ
ーズ状ポリマーを得た。得られたポリマーを、田辺プラ
スチックス機械製40m押出機にて240℃で混練しペ
レット化した。得られたベレットを用いて各種の評価を
したところ、第1表の結果を得た。尚、光線透過率は何
れの実施例に於いても500〜900 nmの波長領械
で914以上であ抄、又複屈折(retardatio
n)は何れも20部m以下と良好であった。Examples 1 to 3 135 parts of n-octyl mercaptan was dissolved in 100 parts of a monomer mixture of methyl methacrylate and cyclohexyl acrylate in the proportions shown in Table 1, 44 parts of lauroyl peroxide α as a polymerization catalyst, and a mold release agent. 1 part of stearyl alcohol as a suspension polymerization dispersant, 01 part of a copolymer of methyl methacrylate and potassium 3-methacryloyloxypropalsulfonate as a suspension polymerization dispersant, and sulfuric acid (IJ)
15 parts of UmIIL and 145 parts of water as a dispersion medium were mixed into a glass flask polymerization apparatus equipped with a stirrer and a temperature needle.
The polymer was polymerized at 95°C, and after reaching a peak temperature, it was kept at 95°C for 30 minutes, cooled, filtered, washed with water, and dried to obtain bead-like polymers. The obtained polymer was kneaded and pelletized at 240° C. using a 40 m extruder manufactured by Tanabe Plastics Machinery. Various evaluations were conducted using the obtained pellets, and the results shown in Table 1 were obtained. In addition, in any of the examples, the light transmittance is 914 or more in the wavelength range of 500 to 900 nm, and the birefringence (retardation) is 914 or more.
n) was 20 parts m or less, which was good.
比較例1〜4
メチルメタクリレートとエチルアクリレートを第1表に
示す割合から成る混合物100部を使用した以外は実施
例1と全く同様に実施したと、こる第1表の結果を得た
。尚、シクロヘキシルアクリレートを30部、メチルメ
タクリレートを70部を共重合し得られたポリマー(比
較例3)は、押し出し賦形時において耐熱性が非常に低
いため、ペレット化することが出来なく実用性に欠ける
ものであシ、メチルメタクリレート100部を重合し得
られたポリマー(比較例4)は、MPRが22.、5
f 710分であり、実施例2、比較例1とほぼ同等の
流動性であるが・引張強度が各個の半分以下であシ実用
性に欠けることがわかる。Comparative Examples 1 to 4 The results shown in Table 1 were obtained in exactly the same manner as in Example 1, except that 100 parts of a mixture of methyl methacrylate and ethyl acrylate in the proportions shown in Table 1 was used. In addition, the polymer obtained by copolymerizing 30 parts of cyclohexyl acrylate and 70 parts of methyl methacrylate (Comparative Example 3) has very low heat resistance during extrusion shaping, so it cannot be pelletized and is not practical. However, the polymer obtained by polymerizing 100 parts of methyl methacrylate (Comparative Example 4) had an MPR of 22. ,5
f 710 minutes, and the fluidity is almost the same as that of Example 2 and Comparative Example 1. However, the tensile strength is less than half of each, indicating that it lacks practicality.
実施例1〜3及び比較例1〜2よりMFRとHDTの関
係は、第1図の様になり例えばMFRが209/10m
1nの成形材料を得ようとする場合、シクロヘキシルア
クリレートとメチルメタクリレートの共重合体は、メチ
ルメタクリレートとエチルアクリレートとの共重合体よ
り本HDTで約4℃向上が認められる。また、HDTが
85℃の成形材料を得ようとする場合、メチルメタクリ
レ−トドシクロヘキシルアクリレートとの共重合体はメ
チルメタクリレ−トドエチルアクリレートの共重合体よ
りも、MFR約13t / 10 minの向上が認め
られ、メチルメタクリレートとシクロヘキシルアクリレ
ートの共重合体はメチルメタクリレートとエチルアクリ
レートの共重合体よりも、その成形性は生産性の意味に
おいて良好であるといえる。From Examples 1 to 3 and Comparative Examples 1 to 2, the relationship between MFR and HDT is as shown in Figure 1. For example, when MFR is 209/10m
When trying to obtain a 1N molding material, the HDT of the copolymer of cyclohexyl acrylate and methyl methacrylate is about 4° C. higher than that of the copolymer of methyl methacrylate and ethyl acrylate. Furthermore, when trying to obtain a molding material with an HDT of 85°C, a copolymer of methyl methacrylate docyclohexyl acrylate has a MFR of about 13 t/10 min compared to a copolymer of methyl methacrylate doethyl acrylate. Improvement was observed, and it can be said that the copolymer of methyl methacrylate and cyclohexyl acrylate has better moldability than the copolymer of methyl methacrylate and ethyl acrylate in terms of productivity.
本発明の光学式情報記録体用メタクリル樹脂成形材料は
、メタクリル樹脂本来の持つ優れた光学的性質を維持し
たまま耐熱性に優れ、良流動性で生産性にも優れた成形
材料として光学式情報記録体用基材として好適に使用す
ることができ、工業上優れた効果を奏する。The methacrylic resin molding material for optical information recording media of the present invention has excellent heat resistance, good flowability, and excellent productivity while maintaining the excellent optical properties inherent to methacrylic resin. It can be suitably used as a base material for recording bodies, and has excellent industrial effects.
第1図は、本発明のメチルメタクリレート/シクロヘキ
シルアクリレート共重合体と従来のメチルメータリレー
ト/エチルアクリレート共重合体の熱賛形温度とメルト
フローレートトノ関係を示す図である。
第
図
MFR[g/10mLn]FIG. 1 is a diagram showing the relationship between temperature and melt flow rate of the methyl methacrylate/cyclohexyl acrylate copolymer of the present invention and a conventional methyl methacrylate/ethyl acrylate copolymer. Figure MFR [g/10mLn]
Claims (1)
ロヘキシルアクリレート20〜0.5重量%との共重合
体から成る光学式情報記録体用メタクリル樹脂。A methacrylic resin for optical information recording media comprising a copolymer of 80 to 99.5% by weight of methyl methacrylate units and 20 to 0.5% by weight of cyclohexyl acrylate.
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2096857A JPH03294314A (en) | 1990-04-12 | 1990-04-12 | Methacrylic resin for optical information recording medium |
KR1019910701419A KR920702857A (en) | 1990-02-23 | 1991-02-22 | Methacrylate resin molding materials for optical information recording media |
PCT/JP1991/000225 WO1991013105A1 (en) | 1990-02-23 | 1991-02-22 | Methacrylic resin molding material for optical information recording medium |
EP19910904333 EP0470260A4 (en) | 1990-02-23 | 1991-02-22 | Methacrylic resin molding material for optical information recording medium |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2096857A JPH03294314A (en) | 1990-04-12 | 1990-04-12 | Methacrylic resin for optical information recording medium |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH03294314A true JPH03294314A (en) | 1991-12-25 |
Family
ID=14176144
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2096857A Pending JPH03294314A (en) | 1990-02-23 | 1990-04-12 | Methacrylic resin for optical information recording medium |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH03294314A (en) |
-
1990
- 1990-04-12 JP JP2096857A patent/JPH03294314A/en active Pending
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