JP2004285150A5

JP2004285150A5 -

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Publication number: JP2004285150A5
Application number: JP2003077498A
Authority: JP
Filing date: 2003-03-20
Publication date: 2006-05-11
Anticipated expiration: 2023-03-20

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参考例１：共重合体（Ｃ）の合成
（Ｃ−１）
容量が５リットルで、バッフルおよびファウドラ型撹拌翼を備えたステンレス製オートクレーブに、メタクリル酸メチル／アクリルアミド共重合体系懸濁剤（以下の方法で調整した。メタクリル酸メチル２０重量部、アクリルアミド８０重量部、過硫酸カリウム０．３重量部、イオン交換水１５００重量部を反応器中に仕込み反応器中を窒素ガスで置換しながら７０℃に保つ。反応は単量体が完全に、重合体に転化するまで続け、メタクリル酸メチルとアクリルアミド共重合体の水溶液として得る。得られた水溶液を懸濁剤として使用した。）０．０５部をイオン交換水１６５部に溶解した溶液を供給し、４００ｒｐｍで撹拌し、系内を窒素ガスで置換した。次に、下記混合物質を反応系を撹拌しながら添加し、７０℃に昇温した。内温が７０℃に達した時点を重合開始として、１８０分間保ち、重合を終了した。以降、通常の方法に従い、反応系の冷却、ポリマーの分離、洗浄、乾燥を行い、ビーズ状の共重合体（Ｃ−１）を得た。この共重合体（Ｃ−１）の重合率は９８重量％であり、重量平均分子量は１１万であった。
メタクリル酸２７重量部
メタクリル酸メチル７３重量部
ｔ−ドデシルメルカプタン１．２重量部
２，２’−アゾビスイソブチロニトリル０．４重量部。 Reference Example 1: Synthesis of copolymer (C) (C-1)
In a stainless steel autoclave having a capacity of 5 liters and equipped with a baffle and a Faudra type stirring blade, a methyl methacrylate / acrylamide copolymer suspension (prepared by the following method: 20 parts by weight of methyl methacrylate, 80 parts by weight of acrylamide) , 0.3 parts by weight of potassium persulfate and 1500 parts by weight of ion-exchanged water were charged into a reactor, and the temperature of the reactor was maintained at 70 ° C. while replacing the reactor with nitrogen gas. To obtain an aqueous solution of methyl methacrylate and acrylamide copolymer. The obtained aqueous solution was used as a suspending agent.) A solution in which 0.05 part was dissolved in 165 parts of ion-exchanged water was supplied, and the solution was supplied at 400 rpm. After stirring, the inside of the system was replaced with nitrogen gas. Next, the following mixture was added while stirring the reaction system, and the temperature was raised to 70 ° C. The time when the internal temperature reached 70 ° C. was defined as the start of polymerization, and was maintained for 180 minutes to complete the polymerization. Thereafter, the reaction system was cooled, the polymer was separated, washed, and dried according to a usual method, to obtain a bead-like copolymer (C-1). The polymerization rate of the copolymer (C-1) was 98% by weight, and the weight average molecular weight was 110,000.
27 parts by weight of methacrylic acid 73 parts by weight of methyl methacrylate 1.2 parts by weight of t-dodecyl mercaptan 0.4 parts by weight of 2,2'-azobisisobutyronitrile

〔実施例７〜１２〕
参考例（１）で得られた共重合体（Ｃ）および可塑剤（Ｂ）を表２に示した配合比でドライブレンドし、スクリュー回転数１００ｒｐｍ、原料供給量５ｋｇ／ｈ、シリンダ温度３００℃に設定したベント付き２軸押出機（ＴＥＸ３０（日本製鋼社製、Ｌ／Ｄ＝４４．５）に供して、ペレット状の熱可塑性樹脂組成物を得た。
次いで、１００℃で３時間乾燥したペレットを射出成形機（名機製作所社製Ｍ−５０ＡII−ＳＪ）に供して、各試験片を成形した。成形条件は成形温度：ガラス転移温度＋１５０℃、金型温度：８０℃、射出速度：９０ｃｍ³／秒、射出時間：１０秒、冷却時間：３０秒、成形圧力：金型に樹脂が全て充填される圧力（成形下限圧力）＋１ＭＰａで行った。
各種特性評価結果を表２に示す。 [Examples 7 to 12]
The copolymer (C) and the plasticizer (B) obtained in Reference Example (1) were dry-blended at the compounding ratio shown in Table 2 , screw rotation speed 100 rpm, raw material supply amount 5 kg / h, cylinder temperature 300 ° C. Was applied to a twin screw extruder with a vent (TEX30 (manufactured by Nippon Steel Corporation, L / D = 44.5)) to obtain a pellet-shaped thermoplastic resin composition.
Next, the pellets dried at 100 ° C. for 3 hours were supplied to an injection molding machine (M-50AII-SJ, manufactured by Meiki Seisakusho) to form each test piece. The molding conditions were as follows: molding temperature: glass transition temperature + 150 ° C., mold temperature: 80 ° C., injection speed: 90 cm ³ / sec, injection time: 10 seconds, cooling time: 30 seconds, molding pressure: the mold was completely filled with resin. Pressure (forming lower pressure limit) + 1 MPa.
Table 2 shows the results of various characteristic evaluations.