JPH02226530A - Method and device for refining of optical disk substrate - Google Patents
Method and device for refining of optical disk substrateInfo
- Publication number
- JPH02226530A JPH02226530A JP1043023A JP4302389A JPH02226530A JP H02226530 A JPH02226530 A JP H02226530A JP 1043023 A JP1043023 A JP 1043023A JP 4302389 A JP4302389 A JP 4302389A JP H02226530 A JPH02226530 A JP H02226530A
- Authority
- JP
- Japan
- Prior art keywords
- fluid
- optical disk
- polycarbonate resin
- disk substrate
- contact
- 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
- 239000000758 substrate Substances 0.000 title claims abstract description 39
- 230000003287 optical effect Effects 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims description 30
- 238000007670 refining Methods 0.000 title abstract description 5
- 239000012535 impurity Substances 0.000 claims abstract description 53
- 239000012530 fluid Substances 0.000 claims abstract description 44
- 239000004431 polycarbonate resin Substances 0.000 claims abstract description 30
- 229920005668 polycarbonate resin Polymers 0.000 claims abstract description 30
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 16
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 13
- 238000000746 purification Methods 0.000 claims description 17
- 239000004417 polycarbonate Substances 0.000 claims description 10
- 238000000926 separation method Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 7
- 229920000515 polycarbonate Polymers 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000011342 resin composition Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 2
- 229920005989 resin Polymers 0.000 abstract description 10
- 239000011347 resin Substances 0.000 abstract description 10
- 238000000465 moulding Methods 0.000 abstract description 8
- 229920000642 polymer Polymers 0.000 abstract description 2
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 12
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 239000002904 solvent Substances 0.000 description 10
- 229920001577 copolymer Polymers 0.000 description 9
- 239000000178 monomer Substances 0.000 description 8
- 239000000654 additive Substances 0.000 description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 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 6
- 150000001875 compounds Chemical class 0.000 description 6
- 238000001125 extrusion Methods 0.000 description 6
- 229920000578 graft copolymer Polymers 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- -1 methanol Chemical class 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000000605 extraction Methods 0.000 description 5
- 239000006082 mold release agent Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- 238000005979 thermal decomposition reaction Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 125000002723 alicyclic group Chemical group 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- VBICKXHEKHSIBG-UHFFFAOYSA-N beta-monoglyceryl stearate Natural products CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 2
- 229920000402 bisphenol A polycarbonate polymer Polymers 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- WOLATMHLPFJRGC-UHFFFAOYSA-N furan-2,5-dione;styrene Chemical compound O=C1OC(=O)C=C1.C=CC1=CC=CC=C1 WOLATMHLPFJRGC-UHFFFAOYSA-N 0.000 description 2
- 229920001519 homopolymer Polymers 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- AJDIZQLSFPQPEY-UHFFFAOYSA-N 1,1,2-Trichlorotrifluoroethane Chemical compound FC(F)(Cl)C(F)(Cl)Cl AJDIZQLSFPQPEY-UHFFFAOYSA-N 0.000 description 1
- QMMJWQMCMRUYTG-UHFFFAOYSA-N 1,2,4,5-tetrachloro-3-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=C(Cl)C(Cl)=CC(Cl)=C1Cl QMMJWQMCMRUYTG-UHFFFAOYSA-N 0.000 description 1
- CQOZJDNCADWEKH-UHFFFAOYSA-N 2-[3,3-bis(2-hydroxyphenyl)propyl]phenol Chemical compound OC1=CC=CC=C1CCC(C=1C(=CC=CC=1)O)C1=CC=CC=C1O CQOZJDNCADWEKH-UHFFFAOYSA-N 0.000 description 1
- FDSYTWVNUJTPMA-UHFFFAOYSA-N 2-[3,9-bis(carboxymethyl)-3,6,9,15-tetrazabicyclo[9.3.1]pentadeca-1(15),11,13-trien-6-yl]acetic acid Chemical compound C1N(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC2=CC=CC1=N2 FDSYTWVNUJTPMA-UHFFFAOYSA-N 0.000 description 1
- WUQYBSRMWWRFQH-UHFFFAOYSA-N 2-prop-1-en-2-ylphenol Chemical compound CC(=C)C1=CC=CC=C1O WUQYBSRMWWRFQH-UHFFFAOYSA-N 0.000 description 1
- PYSRRFNXTXNWCD-UHFFFAOYSA-N 3-(2-phenylethenyl)furan-2,5-dione Chemical compound O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 PYSRRFNXTXNWCD-UHFFFAOYSA-N 0.000 description 1
- PBWGCNFJKNQDGV-UHFFFAOYSA-N 6-phenylimidazo[2,1-b][1,3]thiazol-5-amine Chemical compound N1=C2SC=CN2C(N)=C1C1=CC=CC=C1 PBWGCNFJKNQDGV-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 229930185605 Bisphenol Natural products 0.000 description 1
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- 229920000147 Styrene maleic anhydride Polymers 0.000 description 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229940090958 behenyl behenate Drugs 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- PXBRQCKWGAHEHS-UHFFFAOYSA-N dichlorodifluoromethane Chemical compound FC(F)(Cl)Cl PXBRQCKWGAHEHS-UHFFFAOYSA-N 0.000 description 1
- 235000019404 dichlorodifluoromethane Nutrition 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- RWGFKTVRMDUZSP-UHFFFAOYSA-N isopropyl-benzene Natural products CC(C)C1=CC=CC=C1 RWGFKTVRMDUZSP-UHFFFAOYSA-N 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000001272 nitrous oxide Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- QQVIHTHCMHWDBS-UHFFFAOYSA-N perisophthalic acid Natural products OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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、ポリカーボネート系樹脂製の光ディスク基板
の新規な精製法であり、該基板に含まれる有機性不純物
、無機性不純物、溶媒、添加物、モノマー、オリゴマー
などの不純物を表面から順次除去し、かつ、表面の微細
な機能性の凹凸を損なわない精製法並びにその装置に関
する。[Detailed Description of the Invention] [Industrial Application Field] The present invention is a novel method for purifying an optical disk substrate made of polycarbonate resin, which eliminates organic impurities, inorganic impurities, solvents, and additives contained in the substrate. The present invention relates to a purification method that sequentially removes impurities such as monomers and oligomers from the surface and does not impair fine functional irregularities on the surface, and an apparatus therefor.
ポリカーボネート樹脂の含有する有機性不純物、無機性
不純物、溶媒、添加物、モノマー、オリゴマーなどの不
純物を除去する方法としては、これまで下記の如き技術
が提案されている。As a method for removing impurities such as organic impurities, inorganic impurities, solvents, additives, monomers, and oligomers contained in polycarbonate resins, the following techniques have been proposed so far.
（１）、ポリカーボネート樹脂粉末をメチレンクロライ
ド／トルエンなどの混合溶媒で抽出する方法（特公昭３
８−１６３４７号公報、同４８−６６２０号等）。(1) A method of extracting polycarbonate resin powder with a mixed solvent such as methylene chloride/toluene (Tokuko Sho 3)
8-16347, 48-6620, etc.).
（２）、ポリカーボネート樹脂溶液を活性炭と接触させ
る方法（特公昭４２−２９１５号公報）。(2) A method of bringing a polycarbonate resin solution into contact with activated carbon (Japanese Patent Publication No. 42-2915).
（３）、ポリカーボネート樹脂溶液をアルカリ水溶液で
抽出する方法（特公昭４２−２９１５号公報）。(3) A method of extracting a polycarbonate resin solution with an alkaline aqueous solution (Japanese Patent Publication No. 42-2915).
（４）、ポリカーボネート樹脂溶融物を高真空下攪拌す
る方法（特公昭４２−１６０７９号公報）。(4) A method of stirring a polycarbonate resin melt under high vacuum (Japanese Patent Publication No. 16079/1983).
しかし、これらの方法は下記のような課題を有する。However, these methods have the following problems.
上記（１）、（２）、（３）の方法は、いずれも精製時
に溶媒を用いるため、溶媒および溶媒中の不純物の残留
が完全には回避できず、かつ精製の適用範囲はポリカー
ボネート樹脂粉末の段階以前に限定され、押出・成形両
過程で熱分解により生成した不純物や、成形後には不要
となり逆に不純物として扱うべき安定剤、離型剤などの
添加物を除去する必要のあるペレットや成形品の精製に
は全く無効である。また、精製効果の点においても、（
１）、（２）の方法は有機性不純物やモノマー、オリゴ
マーの除去には有効であっても、無機性不純物が除去で
きず、（３）の方法では実質的にはモノマーのみの除去
に止まり、部分的な精製に限定される。更に、これらの
方法では、精製後排出される混合溶媒、活性炭、アルカ
リ水溶液の後処理や再生処理が複雑かつ高価となる欠点
を有する。Methods (1), (2), and (3) above all use a solvent during purification, so the solvent and the residual impurities in the solvent cannot be completely avoided, and the scope of purification is limited to polycarbonate resin powder. It is limited to the stage before the extrusion and molding process, and it is necessary to remove impurities generated by thermal decomposition during both extrusion and molding processes, as well as additives such as stabilizers and mold release agents that are unnecessary after molding and should be treated as impurities. It is completely ineffective for refining molded products. In addition, in terms of purification effect, (
Although methods 1) and (2) are effective in removing organic impurities, monomers, and oligomers, they cannot remove inorganic impurities, and method (3) essentially only removes monomers. , limited to partial purification. Furthermore, these methods have the disadvantage that the post-treatment and regeneration treatment of the mixed solvent, activated carbon, and aqueous alkali solution discharged after purification are complicated and expensive.
上記（４）の方法は、溶媒、有機性不純物、モノマーの
除去には有効であるが、無機性不純物やオリゴマーなど
の不揮発性不純物の除去は不能な上、加熱による樹脂の
変質という欠点を持つものであり、同様に成形品に対し
ては無効である。Method (4) above is effective in removing solvents, organic impurities, and monomers, but it is not possible to remove non-volatile impurities such as inorganic impurities and oligomers, and it has the disadvantage of deterioration of the resin due to heating. It is also invalid for molded products.
現在のところ、ポリカーボネート樹脂中の種々の不純物
を１つの処理で高い効率のもと、かつ、目的物品である
成形品から、その形、表面状態を実質的に害することな
く、不純物を除去する方法は全く知られていない。At present, there is no method to remove various impurities from polycarbonate resin in one process with high efficiency and without substantially damaging the shape or surface condition of the molded product. is completely unknown.
本発明者は、従来技術の欠点を改善し、効果的かつ適用
範囲が広い精製方法について鋭意検討を重ねた結果、ポ
リカーボネート樹脂に二酸化炭素の加圧流体を接触させ
ると種々の不純物が極めて効果的に除去される。しかも
、処理条件によっては、成形品の形状、その表面状態を
全く害することなく表面から不純物を除くことが可能で
あることを見出した。さらに検討を進めた結果、サブミ
クロンオーダーの機能性凹凸を表面に有する光ディスク
基板においても条件を選択することにより有効な精製が
できることを見出し、本発明に至った。As a result of extensive research into purification methods that are effective and have a wide range of applications, the inventors of the present invention have discovered that various impurities can be removed extremely effectively by contacting polycarbonate resin with a pressurized fluid of carbon dioxide. will be removed. Moreover, it has been found that, depending on the processing conditions, it is possible to remove impurities from the surface of the molded product without damaging its shape or surface condition at all. As a result of further investigation, it was discovered that effective purification can be achieved by selecting conditions even for optical disk substrates having submicron-order functional irregularities on the surface, leading to the present invention.
すなわち、本発明は、ポリカーボネート樹脂、ポリカー
ボネート樹脂を主体とする樹脂組成物及びポリカーボネ
ート系共重合体からなる群より選択されたポリカーボネ
ート系樹脂製の光ディスク基板を二酸化炭素が７０重量
％以上の組成を有する温度 ３０〜１００℃、圧力 １
０〜２００ ｋｇ／ｃｎｌの流体と接触させることを特
徴とする光ディスク基板の精製法、曲びに温度制御用の
熱媒ジャケット、光ディスク基板を保持した補助具の投
入・取り出し口、及び二酸化炭素が７０重量％以上の組
成を有する流体の導入・排出口を少なくとも備えた接触
処理槽（１）、接触に使用した該流体の減圧弁（２）、
減圧された該流体から不純物を除く不純物分離槽（３）
、該流体の圧縮機（４）、圧縮された該流体を所定温度
にする熱交換機（５）および不純物除去用のフィルター
（６）並びにこれらの間を結ぶ流体管を少なくとも備え
てなるポリカーボネート系樹脂製光ディスク基板の精製
装置である。That is, the present invention provides an optical disc substrate made of a polycarbonate resin selected from the group consisting of a polycarbonate resin, a resin composition mainly composed of a polycarbonate resin, and a polycarbonate copolymer, and having a composition containing carbon dioxide in an amount of 70% by weight or more. Temperature: 30-100℃, Pressure: 1
A method for purifying an optical disk substrate characterized by bringing it into contact with a fluid of 0 to 200 kg/cnl, a heating medium jacket for bending and temperature control, an input/output port for an auxiliary tool holding an optical disk substrate, and a carbon dioxide concentration of 70 kg/cnl. a contact treatment tank (1) equipped with at least an inlet/outlet for a fluid having a composition of % by weight or more; a pressure reducing valve (2) for the fluid used for contact;
Impurity separation tank (3) for removing impurities from the reduced pressure fluid
A polycarbonate resin comprising at least a compressor (4) for the fluid, a heat exchanger (5) for bringing the compressed fluid to a predetermined temperature, a filter (6) for removing impurities, and a fluid pipe connecting these. This is a refining device for manufacturing optical disk substrates.
以下、本発明の構成について説明する。The configuration of the present invention will be explained below.
本発明の精製に使用する二酸化炭素を７０重量％以上の
組成を有する温度３０〜１００℃、圧力 １０〜２００
ｋｇ／ｃｎｆ以上の流体（以下、本流体という）とは
、二酸化炭素単独又はこれに一種以上のその他の化合物
を配合してなるものである。配合するその他化合物は、
主に除去対象とする不純物の特性に応じて適宜選択する
ものであるが、抽出条件を緩和する為の希釈用としても
適宜使用される。ここに３０重量％以下の量で併用する
化合物としては、臨界温度が３００℃以下、臨界圧力が
１００ｋｇ／ｃｎｆ以下の化合物が好ましく、具体的に
はフロン−１２、ｎ−ブタン、亜酸化窒素、二酸化硫黄
、メタノール、エタ＞ニル、ジエチルエーテルなどが挙
げられる。無機性不純物を特に効果的に除去したい場合
にはメタノールなどの極性化合物を、有機性不純物や添
加物を特に効果的に除去したい場合にはｎ−ブタンなど
の無極性乃至低極性化合物を配合する。また、希釈には
、窒素ガスなどを適宜使用する。Carbon dioxide used in the purification of the present invention has a composition of 70% by weight or more. Temperature: 30-100°C, pressure: 10-200°C.
The fluid of kg/cnf or more (hereinafter referred to as the main fluid) is carbon dioxide alone or a mixture of carbon dioxide and one or more other compounds. Other compounds to be blended are:
It is selected as appropriate depending on the characteristics of the impurity to be removed, but it is also used as appropriate for dilution to ease the extraction conditions. As the compound to be used together in an amount of 30% by weight or less, a compound having a critical temperature of 300° C. or less and a critical pressure of 100 kg/cnf or less is preferable, and specifically, Freon-12, n-butane, nitrous oxide, Examples include sulfur dioxide, methanol, ethanyl, diethyl ether, and the like. If you want to remove inorganic impurities particularly effectively, use a polar compound such as methanol, and if you want to remove organic impurities or additives particularly effectively, use a non-polar or low polar compound such as n-butane. . Further, nitrogen gas or the like is appropriately used for dilution.
本流体の接触による不純物の抽出或いは精製は、本流体
の接触面（表面）から順次内部に向かって進行し、圧力
の上昇、温度の上昇により急速となるので、ポリカーボ
ネート系樹脂製光ディスク基板の素材によって、適宜、
条件を選択するものであり、通常、接触時間は１〜２４
０分の範囲から選択される。又、１０〜７５．▽２ｋｇ
／ ｃｎｆであるガス状の二酸化炭素で処理した後、圧
カフ５．２ ｋｇ／ｃｎｆ以上に上げて超臨界二酸化炭
素で処理する等の多段階処理を適宜適用することも好ま
しい態様である。Extraction or purification of impurities due to contact with the fluid proceeds from the contact surface (surface) of the fluid toward the inside, and becomes rapid due to increases in pressure and temperature. As appropriate,
The conditions are selected, and the contact time is usually 1 to 24
Selected from a range of 0 minutes. Also, 10-75. ▽2kg
It is also a preferable embodiment to appropriately apply a multi-stage treatment such as treatment with gaseous carbon dioxide of /cnf, then increasing the cuff pressure to 5.2 kg/cnf or higher and treatment with supercritical carbon dioxide.
本発明の光ディスク基板用のポリカーボネート系樹脂と
しては、ホモ−或いはコーポリカーボネート樹脂、ポリ
カーボネート樹脂組成物（ＰＣＴロイ）、ポリカーボネ
ート樹脂とビニル系樹脂とのグラフト共重合体が挙げら
れ、光学的に均質な素材であれば、特に限定されない。Examples of the polycarbonate resin for the optical disk substrate of the present invention include homo- or copolycarbonate resins, polycarbonate resin compositions (PCT Roy), and graft copolymers of polycarbonate resin and vinyl resin. There are no particular limitations as long as it is a material.
ここに、ホモ−或いはコーポリカーボネート樹脂とは、
下記一般式（１）で表される構成単位を２０以上有する
脂肪族、脂環族または芳香族ポリカーボネート樹脂（＝
ＰＣ）であり、特にＰＣとしては芳香族ポリカーボネー
トが好ましい。Here, homo- or copolycarbonate resin is
Aliphatic, alicyclic or aromatic polycarbonate resin (=
PC), and aromatic polycarbonate is particularly preferred as PC.
一般式（１） ： −０−Ｒ−０−Ｃ（＝Ｏ）−▽▽
▽▽・・・ （１）（式中のＲは、２価の脂肪族、脂環
族または芳香族ヒドロキシ化合物残基であ
る。）
又、ポリカーボネート樹脂組成物としては、該ＰＣＣジ
シクロヘキサンジメタノールテレフタル酸／イソフタル
酸共重合体（＝ＰＣＴＡ） 、シクロヘキサンジメタツ
ール／エチレングリコール／テレフタル酸共重合体（＝
ＰＣＴＧ）などのポリエステル樹脂（＝ＰＥＳ）との樹
脂組成物；該ＰＣとスチレンを主体とするスチレン／無
水マレイン酸共重合体、スチレン／マレイミド共重合体
、スチレン／無水マレイン酸／マレイミド共重合体およ
びスチレン／（メタ）アクリル酸エステル共重合体（＝
ＭＳ）との樹脂組成物が挙げられる。ポリカーボネート
系共重合体とは該ＰＣとＰＳ、スチレンを主体とするス
チレン／無水マレイン酸共重合体、スチレン／マレイミ
ド共重合体、スチレン／無水マレイン酸／マレイミド共
重合体、およびＭＳとのグラフト共重合体が挙げられ、
特にホモ−或いはコーポリカーボネート樹脂、ポリカー
ボネート系のグラフト共重合体が挙げられる。General formula (1): -0-R-0-C(=O)-▽▽
▽▽... (1) (R in the formula is a divalent aliphatic, alicyclic or aromatic hydroxy compound residue.) In addition, as the polycarbonate resin composition, the PCC dicyclohexanedimethanol Terephthalic acid/isophthalic acid copolymer (=PCTA), cyclohexane dimetatool/ethylene glycol/terephthalic acid copolymer (=
Resin compositions with polyester resins (=PES) such as PCTG); styrene/maleic anhydride copolymers, styrene/maleimide copolymers, and styrene/maleic anhydride/maleimide copolymers mainly composed of PC and styrene. and styrene/(meth)acrylate copolymer (=
Examples include resin compositions with MS). Polycarbonate copolymers include PC and PS, styrene/maleic anhydride copolymers mainly containing styrene, styrene/maleimide copolymers, styrene/maleic anhydride/maleimide copolymers, and graft copolymers with MS. Examples include polymers,
In particular, homo- or copolycarbonate resins and polycarbonate-based graft copolymers are mentioned.
上記ポリカーボネート系樹脂中に含まれる有機性不純物
、無機性不純物、溶媒、添加物、モノマー、オリゴマー
としては、反応に使用する溶媒、触媒、未反応モノマー
、反応副生物など、反応時に原料、溶媒、反応容器材質
などから生成する不純物、更に押出、成形等のために使
用する安定剤、離型剤などが挙げられる。Organic impurities, inorganic impurities, solvents, additives, monomers, and oligomers contained in the polycarbonate resin include solvents used in the reaction, catalysts, unreacted monomers, reaction by-products, raw materials, solvents, etc. Examples include impurities generated from the reaction vessel material, stabilizers used for extrusion, molding, etc., mold release agents, and the like.
ここに、本発明の精製により除去される不純物を、現在
商業的生産の大部分を占める界面重合法ビスフェノール
Ａホモポリカーボネート樹脂の場合について例示すると
、有機性不純物としては原料ビスフェノールＡの不純物
として含まれるクマロン化合物、トリフエノールなど、
押出・成形両過程で熱分解によって精製含有されるイソ
プロペニルフェノールとそのダイマーなど、および全て
の製造工程を通じて混入したオイル分などが挙げられ、
これは総量として樹脂中に０．０１ｗｔ％内外含まれて
おり、従来技術では除去が困難な難溶性、難揮発性の中
性乃至弱酸性の有機性不純物である。無機性不純物の例
としては、通常の製造・精製時の残留物や添加した無機
酸エステル系安定剤が押出・成形時に熱分解して生成或
いは樹脂の取り扱い時等に周囲環境からの混入により含
有されるＮａ”、 （’１−． ＰＯ４３−、▽ＳＯ３
”−などが挙げられる。Here, the impurities removed by the purification of the present invention are exemplified in the case of interfacially polymerized bisphenol A homopolycarbonate resin, which currently accounts for the majority of commercial production. Examples of organic impurities include impurities in the raw material bisphenol A. coumaron compounds, triphenol, etc.
These include isopropenylphenol and its dimer, which are purified by thermal decomposition during both extrusion and molding processes, and oils that are mixed in throughout all manufacturing processes.
This is contained in the resin in a total amount of about 0.01 wt%, and is a slightly soluble, slightly volatile, neutral to weakly acidic organic impurity that is difficult to remove using conventional techniques. Examples of inorganic impurities include residues from normal manufacturing and refining, added inorganic acid ester stabilizers that are generated by thermal decomposition during extrusion and molding, or those that are mixed in from the surrounding environment during resin handling. Na", ('1-. PO43-, ▽SO3
”- etc.
除去可能な溶媒としては、通常の製造時や加工時に使用
したものが残留して含有されてくる溶媒でメチレンクロ
ライド、クロロホルム、四塩化炭素、トルエン、シクロ
ヘキサン、ヘプタン、アセトン、イソプロピルアルコー
ル、ベンゼンなどが挙げられる。又、除去可能な添加物
としては、ペンタエリスリチル−テトラキス［３−▽（
３，５−ジー ｔ−フチルー４−ヒドロキシフェニル）
プロピオネート］ （商品名；イルガノックス１０１０
）などの酸化防止剤、ブチルステアレート、ステアリン
酸モノグリセリド、シリコンオイルなどの離型剤などが
挙げられる。更に、除去可能なモノマーとしては製造時
の残留や押出・成形・加工時の熱分解、加水分解によっ
て生成し含有されるビスフェノールＡ、末端停止剤のフ
ェノールやｐ−ｔ−ブチルフェノールなどがあり、オリ
ゴマーとしては重合度が１０以下の低重合成分が除去可
能であるが、除去効率は重合度が低いもの程高くなり、
特に重合度３以下のオリゴマーが効果的に除去される。Solvents that can be removed include those that remain after being used during normal manufacturing and processing, such as methylene chloride, chloroform, carbon tetrachloride, toluene, cyclohexane, heptane, acetone, isopropyl alcohol, and benzene. Can be mentioned. In addition, as a removable additive, pentaerythrityl-tetrakis [3-▽(
3,5-di-t-phthyl-4-hydroxyphenyl)
Propionate] (Product name: Irganox 1010
), mold release agents such as butyl stearate, stearic acid monoglyceride, silicone oil, etc. Furthermore, monomers that can be removed include bisphenol A, which is generated and contained during manufacturing, thermal decomposition during extrusion, molding, and processing, and hydrolysis, and end-stopping agents such as phenol and pt-butylphenol. It is possible to remove low polymerization components with a degree of polymerization of 10 or less, but the removal efficiency increases as the degree of polymerization decreases.
In particular, oligomers with a degree of polymerization of 3 or less are effectively removed.
なお、本発明の精製により除去が困難乃至不可能な不純
物としてはＣａａ （ＰＯ４） ２１口ａＳＯ，などの
難溶性の塩類や金属単体の微細片などが挙げられるが、
これらは種類が限定され、かつポーリカーボネート系樹
脂中に混入することは極めて稀なものである。Note that impurities that are difficult or impossible to remove by the purification of the present invention include poorly soluble salts such as Caa (PO4) 21-aSO, and fine particles of simple metals.
These are limited in type and are extremely rarely mixed into polycarbonate resins.
本発明の光ディスク基板の精製法は、本基板を抽出或い
は接触用の圧力容器（以下、接触処理槽という）に入れ
、これに本発明の上記した流体を導入して接触させる方
法によるバッチ方式；又は本基板の投入部と取り出し部
とを設けた接触処理槽を有する装置を用い、投入部に本
基板を入れ、該供給部に本流体を満たした後、接触槽本
体中に導入し、所定時間後、取り出し部に導き、該取り
出し部から本流体を排出した後に精製された基板を取り
出す半連続式などによる。The method for purifying an optical disk substrate of the present invention is a batch method in which the substrate is placed in a pressure vessel for extraction or contact (hereinafter referred to as a contact treatment tank), and the above-described fluid of the present invention is introduced into the vessel and brought into contact with it; Alternatively, using a device having a contact treatment tank with an input section and an output section for the substrate, put the substrate into the input section and fill the supply section with the fluid, then introduce it into the contact tank main body and perform the specified treatment. After a period of time, the purified substrate is guided to a take-out part, and the purified substrate is taken out after discharging the main fluid from the take-out part, such as in a semi-continuous manner.
上記方法により精製され取り出された本基板は、通常、
必要に応じて１００℃以下の温度で常圧又は真空下に加
熱して、使用した流体を除去する。This substrate purified and extracted by the above method is usually
If necessary, the used fluid is removed by heating at a temperature of 100° C. or less under normal pressure or vacuum.
また、使用した流体は、接触処理槽、或いは投入、取り
出し部から分離器に移し、溶解している不純物の大部分
を分離した上で廃棄または循環使用するが、循環使用す
る場合には、圧力変化によるガス／液分離、活性炭吸着
などにより精製処理するが、特に、不純物の少ない光デ
ィスク基板などの成形品の場合には吸着精製処理を行う
ことが好ましい。In addition, the used fluid is transferred from the contact treatment tank or input/output section to a separator to separate most of the dissolved impurities before being disposed of or recycled. Purification treatment is performed by gas/liquid separation due to change, activated carbon adsorption, etc., but it is particularly preferable to perform adsorption purification treatment in the case of molded products such as optical disk substrates with few impurities.
以上の説明した本発明の精製工程の一例を添付の図面に
より説明する。An example of the purification process of the present invention explained above will be explained with reference to the attached drawings.
第１図は、以下の単位装置を組み合わせてなるものであ
り、それぞれ、
（１）、接触処理槽 ：
本流体と光ディスク基板とを所定の条件で接触処理する
接触処理槽（１）であり、通常、温度制御用の熱媒ジャ
ケットＱｌ）を備え、光ディスク基板が互いに接触しな
いように保持する処理用補助具の保持とその投入口Ｑノ
・取り出し口Ｑ４）及び必要に応じて、投入・取り出し
用の隔離室（即ち、投入部０３と取り出し部α５１＞を
持ち、本流体を導入する導入管α０と排出する排出管面
、並びに必要に応じて投入・取り出し部（隔離室）にも
接触処理槽からの導入管と排出管（Ｉｇｌとを備えたも
のである。FIG. 1 shows a combination of the following unit devices: (1) Contact treatment tank: A contact treatment tank (1) for contact treatment of the main fluid and the optical disk substrate under predetermined conditions; Normally, it is equipped with a heat medium jacket Ql) for temperature control, and holds a processing auxiliary tool that holds the optical disk substrates so that they do not come into contact with each other. It has an isolation chamber (i.e., an input section 03 and an extraction section α51), and contact treatment is applied to the introduction pipe α0 for introducing the main fluid and the discharge pipe surface for discharging the fluid, as well as the input/extraction section (isolation chamber) as necessary. It is equipped with an inlet pipe and an outlet pipe (Igl) from the tank.
（２）、減圧弁 ：
処理に使用した本流体から＠量の抽出不純物を除（ため
に下記の不純物分離槽（３）に導入するに先立って、減
圧する。不純物分離槽の入口に取りつけてもよい。(2), Pressure reducing valve: To remove the amount of extracted impurities from the main fluid used for processing, reduce the pressure before introducing it into the impurity separation tank (3) below. Installed at the inlet of the impurity separation tank. Good too.
（３）、不純物分離槽 ：
処理操作に使用した本流体を減圧してガス／液分離、又
は活性炭等の吸着剤との接触処理をして、抽出された不
純物を取り除くものであり、通常、内部に活性炭層を有
する。連続運転する場合には複数の不純物分離槽を設け
るのが好ましい。(3) Impurity separation tank: The main fluid used in the treatment operation is depressurized to perform gas/liquid separation or contact treatment with an adsorbent such as activated carbon to remove extracted impurities. Has an activated carbon layer inside. In the case of continuous operation, it is preferable to provide a plurality of impurity separation tanks.
（４）、圧縮機 ：
本発明の通常の操作においては、ピストン式の圧縮機を
使用する。(4) Compressor: In normal operation of the present invention, a piston type compressor is used.
（５）、熱交換器 ：
接触処理槽への本流体を導入温度を制御するために用い
る。(5) Heat exchanger: Used to control the temperature at which the main fluid is introduced into the contact treatment tank.
（６）、フィルター 二
本流体中に固形の不純物等があると、ディスク表面を汚
染する恐れがあるので、接触処理槽（１）に導入する本
流体は予めフィルターを通過させ精製する。(6) Filter Two solid impurities in the fluid may contaminate the disk surface, so the fluid introduced into the contact treatment tank (1) is purified by passing it through a filter in advance.
（７）、配管 ：
本流体を、接触処理槽（１）→減圧弁（２）→不純物分
離槽（３）→圧縮機（４）→熱交換器（５）→フィルタ
ー（５）→接触処理槽（１）とするために、さらに投入
・取り出し部への導入・排出に使用するものであり、特
にゴミの発生のないものを選択するのが好ましい。(7), Piping: This fluid is transferred to contact treatment tank (1) → pressure reducing valve (2) → impurity separation tank (3) → compressor (4) → heat exchanger (5) → filter (5) → contact treatment In order to make the tank (1), it is also used for introduction to and discharge from the loading/unloading section, and it is particularly preferable to select a tank that does not generate dust.
（８）、その他補助装置 ：
二酸化炭素などの本流体をストックするため補助タンク
（８）、本流体を供給する供給部などを適宜用いる。(8) Other auxiliary equipment: Use an auxiliary tank (8) to stock the main fluid such as carbon dioxide, a supply section for supplying the main fluid, etc. as appropriate.
からなるものである。It consists of
以下、実施例、比較例により本発明を具体的に説明する
が、本発明はこれに限定されるものではない。EXAMPLES Hereinafter, the present invention will be specifically explained with reference to Examples and Comparative Examples, but the present invention is not limited thereto.
実施例 １
分子量１６．０００のビスフェノールＡポリカーボネー
トホモポリマーを射出成形して、片面にラセン状のグル
ープを持つ厚み１．２＋ｒｕｎ、直径１３０ ｍｍの光
ディスク基板を得た。Example 1 A bisphenol A polycarbonate homopolymer having a molecular weight of 16,000 was injection molded to obtain an optical disk substrate having a thickness of 1.2+run and a diameter of 130 mm and having helical groups on one side.
この基板中には、メチレンクロライド（ＭＣ） ２０ｐ
ｐｍ、未反応ビスフェノール（ＢＰＡ） ５０ｐｐｒ
ｎ、ＣＰイオン０．５ｐｐｍが含まれ、また、離型剤で
あるステアリン酸モノグリセリドが ０．０４％含有さ
れていた。In this substrate, methylene chloride (MC) 20p
pm, unreacted bisphenol (BPA) 50ppr
It contained 0.5 ppm of n, CP ions, and 0.04% of stearic acid monoglyceride as a mold release agent.
この基板をＣＯ２１００ｗｔ％の流体を用い、温度４５
℃、圧力１００ｋｇ／ｃｄにて５分間接触処理した。This substrate was coated at a temperature of 45% using a fluid containing 100 wt% CO2.
The contact treatment was carried out at a temperature of 100 kg/cd at a temperature of 100 kg/cd for 5 minutes.
接触処理後、基板をクリーン環境下で常圧１００℃にて
１時間乾燥した後、この基板上に光磁化膜であるＴｂ／
Ｐｅ／Ｃｏ合金をスパッタリングにより蒸着し、さらに
その上に光硬化型のアクリル樹脂をコートした後、紫外
線で硬化させた。After the contact treatment, the substrate was dried in a clean environment at normal pressure of 100°C for 1 hour, and then a photomagnetic film of Tb/
A Pe/Co alloy was deposited by sputtering, and a photocurable acrylic resin was coated thereon, followed by curing with ultraviolet light.
この光ディスクを８０℃、９０％Ｒ１１で３００時間放
置し、この光ディスクの全面に３０−以上の疵欠点が何
個存在するかを調べた結果を第１表に示した。This optical disc was left at 80° C. and 90% R11 for 300 hours, and the number of defects of 30 or more on the entire surface of this optical disc was investigated. The results are shown in Table 1.
光ディスクの疵欠点検査は、日本電子光学側性、自動疵
検査装置Ｉ型を使用した。The optical disc was inspected for defects using an automatic defect inspection device type I manufactured by Nippon Denshi Optical Co., Ltd.
比較例 １
実施例１において、Ｃ０２流体による接触処理に代えて
、光ディスク基板を水洗した後、ｔＰＡとフロン１１３
の蒸気浴洗浄を行なう他は全く同様にした。Comparative Example 1 In Example 1, instead of the contact treatment with C02 fluid, after washing the optical disk substrate with water, tPA and Freon 113 were used.
The procedure was exactly the same except that the steam bath cleaning was performed.
結果を第１表に示した。The results are shown in Table 1.
第１表（疵欠点数／枚）
実施例 ２
末端停止剤として不飽和ビニル化合物を使用してなるビ
スフェノールＡポリカーボネートホモポリマーに、スチ
レン及び無水マレイン酸をグラフト重合させ、ポリカー
ボネート／スチレン−無水マレイン酸グラフト共重合体
を製造した。このグラフト共重合体のガラス転移温度は
１４３℃であった。Table 1 (Number of defects/sheet) Example 2 Styrene and maleic anhydride were graft-polymerized to a bisphenol A polycarbonate homopolymer using an unsaturated vinyl compound as a terminal capper to form polycarbonate/styrene-maleic anhydride. A graft copolymer was produced. The glass transition temperature of this graft copolymer was 143°C.
このグラフト共重合体を射出成形して、片面にラセン状
のグループを持つ厚み１，２画、直径１３０ｍｍの光デ
ィスク基板を得た。This graft copolymer was injection molded to obtain an optical disk substrate having a helical group on one side and having a thickness of 1 or 2 strokes and a diameter of 130 mm.
この基板中には、ＭＣ１５ｐｐｍ、 ＣＩ−イオンＯ，
！５ｐｐｍが含まれ、又、離型剤であるベヘニルベヘネ
ートが０．２％含有されていた。In this substrate, MC15ppm, CI-ion O,
! It contained 5 ppm, and also contained 0.2% of behenyl behenate, which is a mold release agent.
この基板を第２表に示したＣ０２、これにジエチルエー
テル（以下、Ｅｔ２０と記す）、又は窒素ガス（以下、
Ｎ２と記す）を配合してなる本発明の流体を用いて、第
２表に記載の条件にてそれぞれ接触処理した。その後は
実施例１と全く同様とした。This substrate is treated with C02 shown in Table 2, diethyl ether (hereinafter referred to as Et20), or nitrogen gas (hereinafter referred to as Et20).
Contact treatment was carried out under the conditions listed in Table 2 using the fluid of the present invention containing N2). After that, the procedure was exactly the same as in Example 1.
結果を第２表に示した。The results are shown in Table 2.
ポリカーボネート系樹脂は、情報記録ディスクヘの利用
が図られているが、樹脂に含まれる種々な微量の不純物
や添加剤が表面に現れ、記録膜の劣化を促進し、信頼性
、安全性を損なうため、その除去や低減に多くの努力が
払われている。Polycarbonate resin is being used for information recording disks, but trace amounts of various impurities and additives contained in the resin appear on the surface, accelerating the deterioration of the recording film and impairing reliability and safety. , many efforts are being made to eliminate or reduce it.
本発明の方法は、サブミクロンオーダーの表面凹凸を有
する光ディスク基板の表面の凹凸を保持して表面層の不
純物等を除くことができるものであり、その結果、表面
層の不純物が特に原因となる光ディスクの記録膜の密着
性や性能劣化を大幅に解消したものである。The method of the present invention can maintain the surface irregularities of an optical disk substrate having submicron-order surface irregularities and remove impurities in the surface layer, and as a result, impurities in the surface layer can be particularly caused. This significantly eliminates the problem of adhesion and performance deterioration in the recording film of optical discs.
第１図は本発明の光ディスク基板の精製法を実施するた
めの装置のフローを示すものであり、図中の番号はそれ
ぞれ、（１）：接触処理槽、（２）：減圧弁、（３）：
不純物分離槽、（４）：圧縮機、（５）：熱交換器、（
６）：フィルター、（７）：配管、（８）：補助タンク
、ａυ：熱媒ジャケット、ａＳ ：投入口、α３二投入
部、α◇：取り出し口、α９：取り出し部、ａＯ：導入
管、α″ｔ）：排出管、α９＝排出管を示す。
特許出願人 三菱瓦斯化学株式会社
代理人（９０７０）弁理士 小月 貞文第１図
（１）：接触処理槽
減圧弁FIG. 1 shows the flow of an apparatus for carrying out the optical disk substrate purification method of the present invention, and the numbers in the figure are (1): contact treatment tank, (2): pressure reducing valve, (3). ):
Impurity separation tank, (4): Compressor, (5): Heat exchanger, (
6): Filter, (7): Piping, (8): Auxiliary tank, aυ: Heat medium jacket, aS: Inlet, α32 input part, α◇: Outlet port, α9: Outlet part, aO: Inlet pipe, α″t): discharge pipe, α9 = discharge pipe. Patent applicant Mitsubishi Gas Chemical Co., Ltd. Agent (9070) Patent attorney Sadafumi Kozuki Figure 1 (1): Contact treatment tank pressure reducing valve
Claims (1)
とする樹脂組成物及びポリカーボネート系共重合体から
なる群より選択されたポリカーボネート系樹脂製の光デ
ィスク基板を二酸化炭素が７０重量％以上の組成を有す
る温度３０〜１００℃、圧力１０〜２００ｋｇ／ｃｍ＾
２の流体と接触させることを特徴とする光ディスク基板
の精製法。 ２ポリカーボネート系樹脂性光ディスク基板の洗浄精製
装置であって、温度制御用の熱媒ジャケット、光ディス
ク基板を保持した補助具の投入・取り出し口、及び二酸
化炭素が７０重量％以上の組成を有する流体の導入・排
出口を少なくとも備えた接触処理槽（１）、接触に使用
した該流体の減圧弁（２）、減圧された該流体から不純
物を除く不純物分離槽（３）、該流体の圧縮機（４）、
圧縮された該流体を所定温度にする熱交換機（５）およ
び不純物除去用のフィルター（６）並びにこれらの間を
結ぶ流体管を少なくとも備えてなる光ディスク基板の精
製装置。[Scope of Claims] 1. An optical disk substrate made of a polycarbonate resin selected from the group consisting of polycarbonate resin, a resin composition mainly composed of polycarbonate resin, and a polycarbonate copolymer with a composition containing carbon dioxide at 70% by weight or more. Temperature 30~100℃, pressure 10~200kg/cm^
2. A method for purifying an optical disk substrate, which comprises bringing it into contact with a fluid. 2. A cleaning and purifying device for polycarbonate resin optical disk substrates, which includes a heating medium jacket for temperature control, an input/output port for an auxiliary tool holding an optical disk substrate, and a fluid containing 70% by weight or more of carbon dioxide. A contact treatment tank (1) equipped with at least an inlet/outlet port, a pressure reducing valve (2) for the fluid used for contact, an impurity separation tank (3) for removing impurities from the reduced pressure fluid, and a compressor for the fluid ( 4),
An optical disc substrate purification device comprising at least a heat exchanger (5) for bringing the compressed fluid to a predetermined temperature, a filter (6) for removing impurities, and a fluid pipe connecting these.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1043023A JPH02226530A (en) | 1989-02-27 | 1989-02-27 | Method and device for refining of optical disk substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1043023A JPH02226530A (en) | 1989-02-27 | 1989-02-27 | Method and device for refining of optical disk substrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02226530A true JPH02226530A (en) | 1990-09-10 |
Family
ID=12652359
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1043023A Pending JPH02226530A (en) | 1989-02-27 | 1989-02-27 | Method and device for refining of optical disk substrate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02226530A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001158827A (en) * | 1999-09-21 | 2001-06-12 | Daicel Chem Ind Ltd | Method for modifying surface of plastic molding product and surface-modified plastic molding product |
| US6786790B2 (en) | 2001-04-05 | 2004-09-07 | Matsushita Electric Industrial Co., Ltd. | Method and apparatus for manufacturing optical resin substrate, method and apparatus for manufacturing liquid crystal display element using it, and liquid crystal display device using it |
-
1989
- 1989-02-27 JP JP1043023A patent/JPH02226530A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001158827A (en) * | 1999-09-21 | 2001-06-12 | Daicel Chem Ind Ltd | Method for modifying surface of plastic molding product and surface-modified plastic molding product |
| US6786790B2 (en) | 2001-04-05 | 2004-09-07 | Matsushita Electric Industrial Co., Ltd. | Method and apparatus for manufacturing optical resin substrate, method and apparatus for manufacturing liquid crystal display element using it, and liquid crystal display device using it |
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