JP2005082716A5 - - Google Patents
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- JP2005082716A5 JP2005082716A5 JP2003316967A JP2003316967A JP2005082716A5 JP 2005082716 A5 JP2005082716 A5 JP 2005082716A5 JP 2003316967 A JP2003316967 A JP 2003316967A JP 2003316967 A JP2003316967 A JP 2003316967A JP 2005082716 A5 JP2005082716 A5 JP 2005082716A5
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Description
本発明の要旨は、メタクリル酸メチル単位８８〜１００質量％と、炭素数が１〜８のアクリル酸アルキルエステル単位０〜１２質量％とを含むメタクリル系重合体であって、その重合体末端に結合せず硫黄化学発光検出器付ガスクロマトグラフィで求められる未反応メルカプタンを除く硫黄系化合物中の全硫黄濃度が５ｐｐｍ以下であり、且つ重合体末端の結合硫黄量Ｘ（質量％）が、下記式（１）の範囲内にあるメタクリル系重合体にある。 The gist of the present invention is a methacrylic polymer containing 88 to 100% by mass of methyl methacrylate units and 0 to 12% by mass of acrylic acid alkyl ester units having 1 to 8 carbon atoms. The total sulfur concentration in the sulfur-based compound excluding unreacted mercaptan determined by gas chromatography with sulfur chemiluminescence detector without binding is 5 ppm or less, and the bound sulfur amount X (mass%) at the polymer terminal is expressed by the following formula: It exists in the methacrylic polymer which exists in the range of (1).
本発明のメタクリル系重合体は、その重合体末端に結合せず硫黄化学発光検出器付ガスクロマトグラフィで求められる未反応メルカプタンを除く硫黄系化合物中の全硫黄濃度が５ｐｐｍ以下である。５ｐｐｍ以下であると、その成形品が黄帯色することなく無色透明性に優れた材料となる。３ｐｐｍ以下であることが好ましく、低い方がより好ましい。なお、本発明における「ｐｐｍ」は「（質量）ｐｐｍ」を意味する。 The methacrylic polymer of the present invention has a total sulfur concentration of 5 ppm or less in the sulfur-based compound excluding unreacted mercaptan which is not bonded to the polymer terminal and is determined by gas chromatography with a sulfur chemiluminescence detector. When the content is 5 ppm or less, the molded product is a material excellent in colorless transparency without yellowing. It is preferably 3 ppm or less, and more preferably lower. In the present invention, “ppm” means “(mass) ppm”.
本発明における重合体末端に結合せず硫黄化学発光検出器付ガスクロマトグラフィで求められる未反応メルカプタンを除く硫黄系化合物中の全硫黄濃度とは、メタクリル系重合体をアセトンやクロロホルム等の良溶媒に溶解後、メタノールやｎ−ヘキサン等の貧溶媒にてポリマーを再沈・除去した際に貧溶媒に抽出され、その貧溶媒において硫黄化学発光検出器付ガスクロマトグラフィで検出される成分を指す。 In the present invention, the total sulfur concentration in the sulfur-based compound excluding unreacted mercaptan that is not bonded to the polymer terminal and is determined by gas chromatography with a sulfur chemiluminescence detector is a good solvent such as acetone or chloroform. After dissolution, when the polymer is reprecipitated and removed with a poor solvent such as methanol or n-hexane, it is extracted into the poor solvent and is detected in the poor solvent by gas chromatography with a sulfur chemiluminescence detector.
得られたメタクリル系重合体の重合体末端に結合せず硫黄化学発光検出器付ガスクロマトグラフィで求められる未反応メルカプタンを除く硫黄系化合物中の全硫黄濃度を５ｐｐｍ以下とする方法としては、連続塊状重合法や連続溶液重合法において、未反応の重合性原料を含む揮発性成分と重合体とを含む反応液から、未反応の重合性原料を含む揮発性成分を脱揮押出機や薄膜蒸発器によって脱揮する際に低温で脱揮する方法、高温で脱揮された重合体や他の製造方法で重合された重合体を良溶媒で再溶解後、貧溶媒を用いて再沈する方法が挙げられる。工業的に大量生産する場合には、低温で脱揮する方法が好ましい。
As a method of adjusting the total sulfur concentration in the sulfur-based compound excluding unreacted mercaptan, which is not bonded to the polymer end of the obtained methacrylic polymer and determined by gas chromatography with a sulfur chemiluminescence detector, to 5 ppm or less, a continuous mass In a polymerization method or continuous solution polymerization method, a volatile component containing an unreacted polymerizable material is removed from a reaction solution containing a volatile component containing an unreacted polymerizable material and a polymer, and a devolatilizing extruder or thin film evaporator. The method of devolatilizing at a low temperature when devolatilized by the method, the method of reprecipitation using a poor solvent after re-dissolving the polymer devolatilized at a high temperature and the polymer polymerized by other production methods with a good solvent Can be mentioned. For industrial mass production, a method of devolatilization at a low temperature is preferred.
Claims (1)
７５（質量％）≦（Ｘ／３２）×Ｍｎ≦１００（質量％） （１）
（式中、Ｍｎはメタクリル系重合体の数平均分子量を表す。） A methacrylic polymer containing 88 to 100% by mass of methyl methacrylate units and 0 to 12% by mass of an alkyl acrylate unit having 1 to 8 carbon atoms, and is not bonded to the polymer terminal and sulfur chemiluminescence The total sulfur concentration in the sulfur-based compound excluding unreacted mercaptan determined by gas chromatography with a detector is 5 ppm or less, and the bound sulfur amount X (mass%) at the polymer terminal is within the range of the following formula (1). Methacrylic polymer in
75 (mass%) ≦ (X / 32) × Mn ≦ 100 (mass%) (1)
(In the formula, Mn represents the number average molecular weight of the methacrylic polymer.)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2003316967A JP2005082716A (en) | 2003-09-09 | 2003-09-09 | Methacrylic polymer and its manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2003316967A JP2005082716A (en) | 2003-09-09 | 2003-09-09 | Methacrylic polymer and its manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2005082716A JP2005082716A (en) | 2005-03-31 |
| JP2005082716A5 true JP2005082716A5 (en) | 2006-10-26 |
Family
ID=34416701
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2003316967A Pending JP2005082716A (en) | 2003-09-09 | 2003-09-09 | Methacrylic polymer and its manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2005082716A (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW200617125A (en) * | 2004-09-27 | 2006-06-01 | Hitachi Chemical Co Ltd | Photocurable resin composition |
| JP2006117897A (en) * | 2004-09-27 | 2006-05-11 | Hitachi Chem Co Ltd | Photocurable resin composition for coating or adhesive |
| CN101765488B (en) | 2007-08-21 | 2016-05-25 | 株式会社日本触媒 | The manufacture method of acrylic resin pellet and the manufacture method of film |
| KR101482561B1 (en) | 2008-04-25 | 2015-01-16 | 주식회사 동진쎄미켐 | A producing method for acryl polymer |
| WO2013161266A1 (en) | 2012-04-27 | 2013-10-31 | 株式会社クラレ | (meth) acrylic resin composition |
| IN2014DN11140A (en) * | 2012-06-29 | 2015-09-25 | Kuraray Co | |
| US9771438B2 (en) * | 2012-06-29 | 2017-09-26 | Kuraray Co., Ltd. | Methacrylic resin composition, its molded product, and method of producing the composition |
-
2003
- 2003-09-09 JP JP2003316967A patent/JP2005082716A/en active Pending
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