JPS63316313A - Polycarbonate for disk substrate - Google Patents
Polycarbonate for disk substrateInfo
- Publication number
- JPS63316313A JPS63316313A JP62150101A JP15010187A JPS63316313A JP S63316313 A JPS63316313 A JP S63316313A JP 62150101 A JP62150101 A JP 62150101A JP 15010187 A JP15010187 A JP 15010187A JP S63316313 A JPS63316313 A JP S63316313A
- Authority
- JP
- Japan
- Prior art keywords
- polycarbonate
- content
- impurities
- methylene chloride
- acetone
- 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.)
- Granted
Links
- 229920000515 polycarbonate Polymers 0.000 title claims abstract description 53
- 239000004417 polycarbonate Substances 0.000 title claims abstract description 53
- 239000000758 substrate Substances 0.000 title claims abstract description 18
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000012535 impurity Substances 0.000 claims abstract description 21
- 229930185605 Bisphenol Natural products 0.000 claims abstract description 12
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical class C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005260 corrosion Methods 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000000465 moulding Methods 0.000 abstract description 4
- 230000003247 decreasing effect Effects 0.000 abstract 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 57
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 20
- 238000000605 extraction Methods 0.000 description 18
- 238000000034 method Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 11
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 239000002904 solvent Substances 0.000 description 8
- 239000010408 film Substances 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 6
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 5
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000012696 Interfacial polycondensation Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000000944 Soxhlet extraction Methods 0.000 description 2
- 229910052771 Terbium Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012788 optical film Substances 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005809 transesterification reaction Methods 0.000 description 2
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- 229920000298 Cellophane Polymers 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 241000287530 Psittaciformes Species 0.000 description 1
- -1 aliphatic ester Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Landscapes
- Magnetic Record Carriers (AREA)
- Optical Record Carriers And Manufacture Thereof (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はディスク基板用ポリカーボネートに関し、詳し
くは不純物の含有量が極めて少な（、ディスク基板の素
材として有用な高純度のポリカーボネートに関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a polycarbonate for disk substrates, and more particularly to a high-purity polycarbonate that has an extremely low content of impurities (and is useful as a material for disk substrates).
〔従来の技術及び発明が解決しようとする問題点〕一般
に、ポリカーボネートは光ディスクや磁気ディスク等の
ディスク基板の素材として利用されている。[Prior art and problems to be solved by the invention] Generally, polycarbonate is used as a material for disk substrates such as optical disks and magnetic disks.
しかし、このポリカーボネートは、ディスク基板として
成形使用するにあたって、■この基板と記録膜との密着
性が不充分である、■記録膜中に存在する鉄、ガリウム
、テルビウム等の金属が徐々に腐食を受ける、あるいは
■成形時に金型が腐食を受けるため、スタンバ−寿命が
短くなる等様々な問題があった。However, when this polycarbonate is molded and used as a disk substrate, the adhesion between the substrate and the recording film is insufficient, and the metals such as iron, gallium, and terbium present in the recording film gradually corrode. There were various problems such as corrosion of the mold during molding, shortening the life of the stand bar.
そこで本発明者らは、ポリカーボネートをディスク基板
として使用するにあたっての上記の如き問題を解消すべ
く種々の検討を重ねたところ、従来のポリカーボネート
、特にホスゲン法によって得られるポリカーボネートに
は、未反応原料や用ｉまた溶媒あるいは低分子量成分が
不純物として含 □有されており、このような不純物
が上述した様々な問題を引き起こす大きな原因になって
いることが判明した。Therefore, the present inventors have conducted various studies to solve the above-mentioned problems when using polycarbonate as a disk substrate, and have found that conventional polycarbonate, especially polycarbonate obtained by the phosgene method, contains unreacted raw materials and It has been found that solvents or low molecular weight components are contained as impurities, and such impurities are a major cause of the various problems mentioned above.
〔問題点を解決するための手段］
本発明者らは、このような知見′に基いてさらに研究を
続けたところ、これら不純物を含有するポリカーボネー
トをアセトン等の有機溶剤で処理すると、不純物含量が
極めて少なく高純度のポリカーボネートとなり、これが
上述した問題をすべて解消し、ディスク基板として非常
にすぐれた性能を発揮することを見出した。[Means for Solving the Problems] Based on these findings, the present inventors continued their research and found that when polycarbonate containing these impurities is treated with an organic solvent such as acetone, the impurity content can be reduced. It has been found that the polycarbonate has a very low content and has high purity, which solves all of the above-mentioned problems and exhibits extremely excellent performance as a disk substrate.
本発明はかかる過程を経て完成したものであり、その要
旨は不純物の含有量が低分子量成分３重量％以下、未反
応ビスフェノール類２０ｐｐａ＋以下および塩化メチレ
ン２０ｐｐｍ以下であることを特徴とするディスク基板
用ポリカーボネートである。The present invention was completed through such a process, and its gist is a disk substrate characterized in that the content of impurities is 3% by weight or less of low molecular weight components, 20ppa+ or less of unreacted bisphenols, and 20ppm or less of methylene chloride. It is polycarbonate.
本発明のポリカーボネートは、従来のポリカーボネート
に比べて不純物の含有量が少なく、純度の高いものであ
る。一般に、従来のポリカーボネートには様々な不純物
が含有されているが、特に低分子量成分（ポリカーボネ
ートオリゴマーなど）や未反応ビスフェノール類（ビス
フェノールＡなど）あるいは溶媒として用いた塩化メチ
レンが多く、またこれらの不純物はポリカーボネートを
ディスク基板に用いたときに、前述した如き種々の問題
を引き起こす。The polycarbonate of the present invention has a lower content of impurities and higher purity than conventional polycarbonates. In general, conventional polycarbonate contains various impurities, especially low molecular weight components (polycarbonate oligomers, etc.), unreacted bisphenols (bisphenol A, etc.), and methylene chloride used as a solvent. When polycarbonate is used as a disk substrate, it causes various problems as described above.
本発明のポリカーボネートは、上述した不純物の含有量
はいずれも少なく、低分子量成分は３重量％以下、好ま
しくは２重量％以下であり、未反応ビスフェノール類は
２０ｐｐｍ以下、好ましくは１０ｐｐｍ以下であって、
また塩化メチレンは２０ｐｐＩ１１以下、好ましくは１
５ｐｐｍ以下である。The polycarbonate of the present invention has a low content of all of the above-mentioned impurities, with low molecular weight components being 3% by weight or less, preferably 2% by weight or less, and unreacted bisphenols being 20ppm or less, preferably 10ppm or less. ,
Furthermore, methylene chloride is 20ppI11 or less, preferably 1
It is 5 ppm or less.
ここで、低分子量成分が３重量％を越えたり、あるいは
未反応ビスフェノール類が２０ｐｐｍを越えると、ディ
スク基板と記録膜との接着性が低下する。さらに、塩化
メチレンが２０ｐｐｍを越えると、記録膜が腐食を受け
やすくなり、また成形時に金型が腐食を受けるためスタ
ンパ−寿命も短くなる。なお、上記低分子量成分の含有
量は、対象とするポリカーボネートをアセトンを溶媒と
してソックスレー抽出された成分の割合を意味する。Here, if the low molecular weight component exceeds 3% by weight or the unreacted bisphenol exceeds 20 ppm, the adhesion between the disk substrate and the recording film decreases. Furthermore, if methylene chloride exceeds 20 ppm, the recording film is susceptible to corrosion, and the mold is also corroded during molding, resulting in a shortened stamper life. In addition, the content of the low molecular weight component mentioned above means the proportion of the component obtained by Soxhlet extraction of the target polycarbonate using acetone as a solvent.
本発明のポリカーボネートは、様々な手法によって得る
ことが可能であるが、通常は各種方法で得られた不純物
を含有する粉末状ポリカーボネートをアセトン等の有機
溶媒で抽出処理することによって得られる。The polycarbonate of the present invention can be obtained by various methods, but is usually obtained by extracting powdered polycarbonate containing impurities obtained by various methods with an organic solvent such as acetone.
この不純物を含有する粉末状ポリカーボネートを製造す
る方法としては、特に制限はないが、通常はホスゲン法
、特にビスフェノールＡ等のビスフェノール類とホスゲ
ンを原料とし、塩化メチレンを溶媒とする界面重縮合法
、とりわけ連続界面重縮合法をあげることができる。そ
のほか、エステル交換法やホスゲン法のうちのピリジン
を溶媒とする所謂ピリジン重合法をあげることもできる
。There are no particular restrictions on the method for producing powdered polycarbonate containing impurities, but usually the phosgene method, especially the interfacial polycondensation method using bisphenols such as bisphenol A and phosgene as raw materials and methylene chloride as a solvent; In particular, mention may be made of the continuous interfacial polycondensation method. In addition, among the transesterification method and the phosgene method, the so-called pyridine polymerization method using pyridine as a solvent can also be mentioned.
上記の粉末状ポリカーボネートとは、厳密な意味での粉
末状のものに限定するわけではなく、フレーク状等のも
のをも包含する。つまり、ホスゲン法やエステル交換法
で得られた粉末状１粒状。The above-mentioned powdery polycarbonate is not limited to powdery polycarbonate in a strict sense, but also includes flaky polycarbonate and the like. In other words, it is a single grain of powder obtained by the phosgene method or transesterification method.
フレーク状等のポリカーボネートであって、ペレット化
する前のものすべてを包含する。It includes all types of polycarbonate in the form of flakes, etc., before being pelletized.
たとえば、上述の連続界面重縮合により得られる粉末状
ポリカーボネートは、通常はフレーク状であって、不純
物としてポリカーボネートのオリゴマー等の低分子量成
分を４〜８重景％、ビスフェノールＡ等の未反応ビスフ
ェノール類を７０〜１５０ｐｐ−および溶媒として用い
た塩化メチレンを５０〜１５０ｐｐｍ程度含有している
。For example, the powdered polycarbonate obtained by the above-mentioned continuous interfacial polycondensation is usually in the form of flakes, and contains 4 to 8 weight percent of low molecular weight components such as polycarbonate oligomers as impurities, and unreacted bisphenols such as bisphenol A. It contains about 70 to 150 ppm of methylene chloride used as a solvent and about 50 to 150 ppm of methylene chloride.
本発明のポリカーボネートは、このような不純物を含有
する粉末状ポリカーボネートを、アセトン、メチルエチ
ルケトンなどのケトン類、トルエン、キシレンなどのポ
リカーボネートに対しては弱い沈澱効果があるとされて
いる有機溶媒にて抽出処理することによって得られる。The polycarbonate of the present invention is obtained by extracting powdered polycarbonate containing such impurities with an organic solvent that is said to have a weak precipitation effect on polycarbonate, such as ketones such as acetone and methyl ethyl ketone, and toluene and xylene. Obtained by processing.
抽出処理にあたっては、上記有機溶媒を粉末状ポリカー
ボネートの０．５〜２０倍量の範囲で使用し、温度を４
０°Ｃ以上、用いる有機溶媒の沸点以下の範囲に設定す
ることが好ましい、なお、この抽出処理は、通常は常圧
下で行うが、加圧下で行うことも可能である。また、抽
出処理に使用する有機溶媒としては、特にアセトンが好
適である。In the extraction process, the above organic solvent was used in an amount of 0.5 to 20 times the amount of powdered polycarbonate, and the temperature was adjusted to 4.
It is preferable to set the temperature in a range of 0° C. or higher and lower than the boiling point of the organic solvent used. Note that this extraction treatment is usually performed under normal pressure, but it can also be performed under increased pressure. Furthermore, acetone is particularly suitable as the organic solvent used in the extraction process.
〔実施例〕
次に、本発明を実施例および比較例によりさらに詳しく
説明する。[Example] Next, the present invention will be explained in more detail with reference to Examples and Comparative Examples.
実施例１
低分子量成分４重量％、未反応ビスフェノールＡ１００
ｐｐｍおよび塩化メチレン１１００ｐｐを含有するフレ
ーク状のポリカーボネート１００ｋｇに、アセトン２２
５ｋｇを加えて５０°Ｃで１時間撹拌して接触処理（抽
出処理）を行った。Example 1 4% by weight of low molecular weight components, 100 unreacted bisphenol A
100 kg of polycarbonate flakes containing 1100 ppm of methylene chloride and 22 kg of acetone
A contact treatment (extraction treatment) was performed by adding 5 kg of the mixture and stirring at 50°C for 1 hour.
その後、アセトンを除去し、１２０″Ｃ１３０〜１ｍ１
ｇの減圧下で２０時間乾燥した。得られたフレーク状の
ポリカーボネート中の不純物含量は第１表の通りであっ
た。Then remove the acetone and add 120″C130~1m1
The mixture was dried for 20 hours under a reduced pressure of 100 g. The impurity content in the obtained flaky polycarbonate was as shown in Table 1.
次に、このフレーク状のポリカーボネートにリン系酸化
防止剤４ｐｐｍ（リン換算）および脂肪族エステル２０
０ｐｐｍを添加した後に、押出機でベレット化し、射出
成形機で直径１３ＣＩのディスク基板を成形した。この
際、ディスクの射出成形で５０００シヨツト後の金型鏡
面のくもり度合いを目視観察して、これをスタンパ−寿
命として評価した。結果を第１表に示す。Next, 4 ppm of phosphorous antioxidant (in terms of phosphorus) and 20 ppm of aliphatic ester were added to this flaky polycarbonate.
After adding 0 ppm, it was pelletized using an extruder and molded into a disk substrate with a diameter of 13 CI using an injection molding machine. At this time, the degree of cloudiness of the mirror surface of the mold after 5,000 shots of disk injection molding was visually observed, and this was evaluated as the stamper life. The results are shown in Table 1.
厚さ８００人の酸化珪素（Ｓｉｎ、）Ｊｔ！／厚さ１０
００人の金属（Ｔｂ、 Ｆｅ、 Ｃｏ）７０１／厚さ８
００人の酸化珪素（Ｓｉｎ工）層の三層構造からなる光
磁気膜を、スパッタリング法により上記ディスク基板上
に形成した。得られた光ディスクの性能を、下記の如く
接着性（光磁気膜と基板との接着性）および腐食性のテ
ストを行うことにより評価した。Silicon oxide (Sin,) Jt with a thickness of 800 people! /thickness 10
00 metals (Tb, Fe, Co) 701/thickness 8
A magneto-optical film having a three-layer structure of 0.0000000 silicon oxide (Sin) layers was formed on the disk substrate by sputtering. The performance of the obtained optical disc was evaluated by conducting adhesiveness (adhesion between the magneto-optical film and the substrate) and corrosiveness tests as described below.
結果を第１表に示す。The results are shown in Table 1.
遣１血±入上
上記光ディスクを、温度９０℃、相対湿度９０％の雰囲
気下に１００時間放置後、セロハンテープによるゴバン
目ピンホールテストを行い、次式に基いて接着性を表示
した。After leaving the above optical disc in an atmosphere with a temperature of 90° C. and a relative humidity of 90% for 100 hours, a pinhole test using cellophane tape was performed, and the adhesion was expressed based on the following formula.
上記光ディスクを、温度６０℃、相対湿度９０％の雰囲
気下に３００時間放置後、光学顕微鏡にて１０００倍で
２５０μｍＸ２００μｍの視野中におけるピンホール腐
食の数を測定した。After the optical disk was left in an atmosphere of 60° C. and 90% relative humidity for 300 hours, the number of pinhole corrosion in a field of view of 250 μm×200 μm was measured at 1000 times using an optical microscope.
実施例２
実施例１において、アセトンによる抽出処理をアセトン
の沸点（約５６．５℃）で行ったこと以外は、実施例１
と同様の操作を行った。結果を第１表に示す。Example 2 Example 1 except that the extraction treatment with acetone was performed at the boiling point of acetone (approximately 56.5°C).
The same operation was performed. The results are shown in Table 1.
実施例３
実施例１において、アセトンによる抽出処理をアセトン
の沸点（約５６．５℃）で３０分間行ったこと以外は、
実施例１と同様の操作を行った。結果を第１表に示す。Example 3 In Example 1, except that the extraction treatment with acetone was performed for 30 minutes at the boiling point of acetone (approximately 56.5°C),
The same operation as in Example 1 was performed. The results are shown in Table 1.
実施例４
実施例１において、抽出処理をアセトンの代わりにトル
エンを使用して抽出処理を２回行い、トルエンを除去後
、４０時間減圧下で乾燥したこと以外は、実施例１と同
様の操作を行った。結果を第１表に示す。Example 4 The same procedure as in Example 1 was performed, except that the extraction treatment was performed twice using toluene instead of acetone, and after removing toluene, it was dried under reduced pressure for 40 hours. I did it. The results are shown in Table 1.
実施例５
実施例１において、抽出処理をアセトンの代わりにメチ
ルエチルケトンを使用して抽出処理を行い、メチルエチ
ルケトンを除去後、４０時間減圧下で乾燥したこと以外
は、実施例１と同様の操作を行った。結果を第１表に示
す。Example 5 The same operation as in Example 1 was carried out, except that the extraction treatment was performed using methyl ethyl ketone instead of acetone, and after removing methyl ethyl ketone, it was dried under reduced pressure for 40 hours. Ta. The results are shown in Table 1.
比較例１
実施例１において、アセトンによる抽出処理を行わなか
ったこと以外は、実施例１と同様の操作を行った。結果
を第１表に示す。Comparative Example 1 The same operation as in Example 1 was performed except that the extraction treatment with acetone was not performed. The results are shown in Table 1.
比較例２
実施例１において、アセトンによる抽出処理をアセトン
１００ｋｇを用いて２５℃で行ったこと以外は、実施例
１と同様の操作を行った。結果を第１表に示す。Comparative Example 2 The same operation as in Example 1 was performed except that the extraction treatment with acetone was performed at 25° C. using 100 kg of acetone. The results are shown in Table 1.
比較例３
実施例１において、ポリカーボネートとして低分子量成
分２重量％、未反応ビスフェノールＡＩ００ｐｐｍおよ
び塩化メチレン１１００ｐｐを含有するフレーク状ポリ
カーボネートを用いたこと及びアセトンによる抽出処理
を行わなかったこと以外は、実施例１と同様の操作を行
った。結果を第１表に示す。Comparative Example 3 Example 1 except that a flaky polycarbonate containing 2% by weight of low molecular weight components, 00 ppm of unreacted bisphenol AI, and 1100 ppm of methylene chloride was used as the polycarbonate, and that the extraction treatment with acetone was not performed. The same operation as in 1 was performed. The results are shown in Table 1.
比較例４
実施例１において、ポリカーボネートとして低分子量成
分４重量％、未反応ビスフェノールＡｉｏｐｐ−および
塩化メチレン１０ｐｐｍを含有するフレーク状ポリカー
ボネートを用いたこと及びアセトンによる抽出処理を行
わなかったこと以外は、実施例１と同様の操作を行った
。結果を第１表に示す。Comparative Example 4 In Example 1, except that flaky polycarbonate containing 4% by weight of low molecular weight components, unreacted bisphenol Aiopp- and 10 ppm of methylene chloride was used as the polycarbonate, and the extraction treatment with acetone was not performed. The same operation as in Example 1 was performed. The results are shown in Table 1.
比較例５
実施例１において、ポリカーボネートとして低分子量成
分２重量％、未反応ビスフェノールＡ１０ｐｐｍおよび
塩化メチレン１１００ｐｐ＋を含有するフレーク状ポリ
カーボネートを用いたこと及びアセトンによる抽出処理
を行わなかったこと以外は、実施例１と同様の操作を行
った。結果を第１表に示す。Comparative Example 5 Example 1 except that a flaky polycarbonate containing 2% by weight of low molecular weight components, 10 ppm of unreacted bisphenol A, and 1100 pp+ of methylene chloride was used as the polycarbonate, and that the extraction treatment with acetone was not performed. The same operation as in 1 was performed. The results are shown in Table 1.
比較例６
実施例１において、抽出処理をアセトンの代わりにヘキ
サンを用いたこと及び処理温度を４０°Ｃとしたこと以
外は、実施例１と同様の操作を行った。結果を第１表に
示す。Comparative Example 6 The same operation as in Example 1 was performed except that hexane was used instead of acetone for the extraction treatment and the treatment temperature was 40°C. The results are shown in Table 1.
比較例７
実施例１において、抽出処理をアセトンの代わりにメタ
ノールを用いたこと及び処理温度を４０°Ｃとしたこと
以外は、実施例１と同様の操作を行った。結果を第１表
に示す。Comparative Example 7 The same operation as in Example 1 was performed except that methanol was used instead of acetone for the extraction treatment and the treatment temperature was 40°C. The results are shown in Table 1.
比較例８
実施例１において、ポリカーボネートとして低分子量成
分４重量％、未反応ビスフェノールＡ１０ｐｐｍおよび
塩化メチレン１０ｐｐｍを含有するフレーク状ポリカー
ボネートを用いたこと及びアセトンによる抽出処理を行
わなかったこと以外は、実施例１と同様の操作を行った
。結果を第１表に示す。Comparative Example 8 Example 1 except that flaky polycarbonate containing 4% by weight of low molecular weight components, 10 ppm of unreacted bisphenol A, and 10 ppm of methylene chloride was used as the polycarbonate, and that the extraction treatment with acetone was not performed. The same operation as in 1 was performed. The results are shown in Table 1.
比較例９
実施例１において、ポリカーボネートとして低分子量成
分１．５重量％、未反応ビスフェノールＡ１０ｐｐ−お
よび塩化メチレン４０ｐｐｍを含有するフレーク状ポリ
カーボネートを用いたこと及びアセトンによる抽出処理
を行わなかったこと以外は、実施例１と同様の操作を行
った。結果を第１表に示す。Comparative Example 9 In Example 1, except that flaky polycarbonate containing 1.5% by weight of low molecular weight components, 10 ppm of unreacted bisphenol A, and 40 ppm of methylene chloride was used as the polycarbonate, and the extraction treatment with acetone was not performed. , the same operation as in Example 1 was performed. The results are shown in Table 1.
比較例１０
実施例１において、ポリカーボネートとして低分子量成
分１．５重量％、′未反応ビスフェノールＡ３０ｐｐｍ
＋および塩化メチレン１０ｐｐｍを含有するフレーク状
ポリカーボネートを用いたこと及びアセトンによる抽出
処理を行わなかったこと以外は、実施例１と同様の操作
を行った。結果を第１表に示す。Comparative Example 10 In Example 1, 1.5% by weight of low molecular weight component as polycarbonate, 30 ppm of unreacted bisphenol A
The same operation as in Example 1 was performed, except that flaky polycarbonate containing + and 10 ppm of methylene chloride was used, and the extraction treatment with acetone was not performed. The results are shown in Table 1.
＊ 第１表中で、得られたポリカーボネート中の不純物
含量は、次の如く分析定量されたものである。* In Table 1, the content of impurities in the obtained polycarbonate was analyzed and determined as follows.
成分ヱ１底公
アセトンを溶媒としてソックスレー抽出された成分であ
る。即ち、試料であるポリカーボネートを粉砕して１０
０メツシユの金網を通過したちの１５ｇを円筒濾紙胤８
４（２８ｘ１００鵡）に採取し、これを３００Ｉ１１の
アセトンを用いて、３〜４分に１回（２０ｍ／回）の還
流量で８時間還流させて抽出した。その後、３００１１
１のアセトンを蒸発させた後の残渣物を秤量し、これを
低分子量成分とした。Ingredient (1) This is a component extracted using Soxhlet using acetone as a solvent. That is, a sample of polycarbonate was ground to 10
Transfer 15 g of the material that passed through the wire mesh of 0 mesh to 8 thimble filter paper seeds.
4 (28 x 100 parrots), and extracted with 300 I11 acetone by refluxing for 8 hours at a reflux rate of once every 3 to 4 minutes (20 m/time). Then 30011
The residue after evaporating the acetone in Step 1 was weighed and used as a low molecular weight component.
ビスフェノールＡ
上述の低分子量成分をアセトンを溶媒としてソックスレ
ー抽出を行った後、液体クロマトグラフィーにより定量
したものである。Bisphenol A The above-mentioned low molecular weight component was subjected to Soxhlet extraction using acetone as a solvent, and then quantified by liquid chromatography.
塩化基土にヱ
１．２−ジクロロエタンに試料であるポリカーボネート
を溶解し、ガスクロマトグラフィー（ＦＩＤ）により定
量したものである。A polycarbonate sample was dissolved in 1,2-dichloroethane in a chloride base, and the amount was determined by gas chromatography (FID).
本発明のポリカーボネートは、不純物ｐ含有量が極めて
少なく高品質のものであって、光ディスクや磁気ディス
ク等のディスク基板に使用したときに、記録膜との密着
性がよく、しかも記録膜を腐食させるおそれもなく、ま
た成形時に金型が腐食を受けないためスタンパ−寿命も
長い。The polycarbonate of the present invention is of high quality with extremely low impurity p content, and when used for disk substrates such as optical disks and magnetic disks, it has good adhesion to the recording film and does not corrode the recording film. There is no fear, and since the mold is not corroded during molding, the life of the stamper is long.
したがって、本発明のポリカーボネートは、優れた性能
を有するディスク基板の素材として実用上極めて価値の
高いものであり、その幅広い利用が期待される。Therefore, the polycarbonate of the present invention has extremely high practical value as a material for disc substrates having excellent performance, and its wide use is expected.
Claims (1)
反応ビスフェノール類２０ｐｐｍ以下および塩化メチレ
ン２０ｐｐｍ以下であることを特徴とするディスク基板
用ポリカーボネート。(1) A polycarbonate for a disk substrate, characterized in that the content of impurities is 3% by weight or less of low molecular weight components, 20ppm or less of unreacted bisphenols, and 20ppm or less of methylene chloride.
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62150101A JPH07108938B2 (en) | 1987-06-18 | 1987-06-18 | Disc substrate made of polycarbonate |
| US07/191,604 US4880896A (en) | 1987-05-30 | 1988-05-09 | Polycarbonate for disc substrate having low bisphenol content |
| EP88108453A EP0293769B1 (en) | 1987-05-30 | 1988-05-27 | Polycarbonate for disc substrate |
| DE3855023T DE3855023T2 (en) | 1987-05-30 | 1988-05-27 | Polycarbonate for plate substrates |
| KR1019880006371A KR950000069B1 (en) | 1987-05-30 | 1988-05-30 | Polycarbonate for disc substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62150101A JPH07108938B2 (en) | 1987-06-18 | 1987-06-18 | Disc substrate made of polycarbonate |
Related Child Applications (3)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5064897A Division JPH0794544B2 (en) | 1993-03-24 | 1993-03-24 | Disc substrate made of polycarbonate |
| JP5064898A Division JPH0794543B2 (en) | 1993-03-24 | 1993-03-24 | Disc substrate made of polycarbonate |
| JP33550697A Division JP3253905B2 (en) | 1997-12-05 | 1997-12-05 | Polycarbonate for disk substrates |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63316313A true JPS63316313A (en) | 1988-12-23 |
| JPH07108938B2 JPH07108938B2 (en) | 1995-11-22 |
Family
ID=15489528
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62150101A Expired - Lifetime JPH07108938B2 (en) | 1987-05-30 | 1987-06-18 | Disc substrate made of polycarbonate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07108938B2 (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6431690A (en) * | 1987-07-29 | 1989-02-01 | Mitsubishi Gas Chemical Co | Polycarbonate molding material for optical disk |
| JPH06100682A (en) * | 1993-03-24 | 1994-04-12 | Idemitsu Petrochem Co Ltd | Polycarbonate for disk base |
| JPH06100683A (en) * | 1993-03-24 | 1994-04-12 | Idemitsu Petrochem Co Ltd | Polycarbonate for disk base |
| US5747632A (en) * | 1995-11-27 | 1998-05-05 | Mitsubishi Gas Chemical Company, Inc. | Polycarbonate resin with high flowability and process for producing the same |
| US5969084A (en) * | 1997-04-14 | 1999-10-19 | Mitsubishi Gas Chemical Company | Process for producing polycarbonate resin with high flowability |
| WO2000011086A1 (en) * | 1998-08-18 | 2000-03-02 | Teijin Chemicals, Ltd. | Optical polycarbonate resin molding material and optical disk substrate |
| JP2002069219A (en) * | 2000-08-31 | 2002-03-08 | Teijin Chem Ltd | Polycarbonate resin composition molded product |
| US7307114B2 (en) | 2003-05-07 | 2007-12-11 | Asahi Kasei Chemicals Corporation | Polycarbonate resin composition for use in the production of a substrate for an optical information medium |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54138097A (en) * | 1978-04-19 | 1979-10-26 | Mitsubishi Chem Ind Ltd | Method of washing a polycarbonate solution in an organic solvent |
| JPS5521773A (en) * | 1978-08-01 | 1980-02-16 | Kubota Ltd | Combined harvester |
| JPS56131654A (en) * | 1978-08-28 | 1981-10-15 | Discovision Ass | Polymer plastic composition for making video disc |
| US4529791A (en) * | 1981-01-28 | 1985-07-16 | The Dow Chemical Company | Interfacial polycarbonate preparation by adding additional solvent |
| JPS60169445A (en) * | 1983-12-27 | 1985-09-02 | ゼネラル・エレクトリツク・カンパニイ | Improved manufacture of aromatic carbonate |
| JPS6121136A (en) * | 1984-07-07 | 1986-01-29 | バイエル・アクチエンゲゼルシヤフト | Method of removing undesirable components, particularly low molecular weight components from solid polymer |
| JPS61289555A (en) * | 1985-06-14 | 1986-12-19 | Matsushita Electric Ind Co Ltd | Optical disk |
| JPS61291545A (en) * | 1985-06-18 | 1986-12-22 | Daicel Chem Ind Ltd | Production of carbonic acid ester |
| JPS6231801A (en) * | 1985-08-02 | 1987-02-10 | Teijin Chem Ltd | Optical molding |
| JPS6250801A (en) * | 1985-08-30 | 1987-03-05 | Teijin Chem Ltd | Molding for optical purpose |
| JPS6271902A (en) * | 1985-09-26 | 1987-04-02 | Teijin Chem Ltd | Molding for optical article |
| JPS6377932A (en) * | 1986-09-20 | 1988-04-08 | Sony Corp | Optical information recording medium |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6431690A (en) * | 1987-07-29 | 1989-02-01 | Mitsubishi Gas Chemical Co | Polycarbonate molding material for optical disk |
| JPH06100682A (en) * | 1993-03-24 | 1994-04-12 | Idemitsu Petrochem Co Ltd | Polycarbonate for disk base |
| JPH06100683A (en) * | 1993-03-24 | 1994-04-12 | Idemitsu Petrochem Co Ltd | Polycarbonate for disk base |
| US5747632A (en) * | 1995-11-27 | 1998-05-05 | Mitsubishi Gas Chemical Company, Inc. | Polycarbonate resin with high flowability and process for producing the same |
| US5969084A (en) * | 1997-04-14 | 1999-10-19 | Mitsubishi Gas Chemical Company | Process for producing polycarbonate resin with high flowability |
| WO2000011086A1 (en) * | 1998-08-18 | 2000-03-02 | Teijin Chemicals, Ltd. | Optical polycarbonate resin molding material and optical disk substrate |
| JP2002069219A (en) * | 2000-08-31 | 2002-03-08 | Teijin Chem Ltd | Polycarbonate resin composition molded product |
| US7307114B2 (en) | 2003-05-07 | 2007-12-11 | Asahi Kasei Chemicals Corporation | Polycarbonate resin composition for use in the production of a substrate for an optical information medium |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07108938B2 (en) | 1995-11-22 |
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