JPH06155466A - Method of drying aromatic polycarbonate granule - Google Patents
Method of drying aromatic polycarbonate granuleInfo
- Publication number
- JPH06155466A JPH06155466A JP31012492A JP31012492A JPH06155466A JP H06155466 A JPH06155466 A JP H06155466A JP 31012492 A JP31012492 A JP 31012492A JP 31012492 A JP31012492 A JP 31012492A JP H06155466 A JPH06155466 A JP H06155466A
- Authority
- JP
- Japan
- Prior art keywords
- solvent
- aromatic polycarbonate
- powder
- amount
- drying
- 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
- 239000004417 polycarbonate Substances 0.000 title claims abstract description 41
- 125000003118 aryl group Chemical group 0.000 title claims abstract description 40
- 229920000515 polycarbonate Polymers 0.000 title claims abstract description 40
- 239000008187 granular material Substances 0.000 title claims abstract description 31
- 238000001035 drying Methods 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims description 17
- 239000002904 solvent Substances 0.000 claims abstract description 53
- 239000000843 powder Substances 0.000 claims description 50
- 230000002542 deteriorative effect Effects 0.000 abstract description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 36
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 21
- 239000002245 particle Substances 0.000 description 19
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 17
- 239000013557 residual solvent Substances 0.000 description 15
- 238000003756 stirring Methods 0.000 description 8
- 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
- 238000011156 evaluation Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- -1 diaryl carbonate Chemical compound 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 230000020169 heat generation Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- XGIAHMUOCFHQTI-UHFFFAOYSA-N Cl.Cl.Cl.Cl.CC Chemical compound Cl.Cl.Cl.Cl.CC XGIAHMUOCFHQTI-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- 125000001118 alkylidene group Chemical group 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- MIMDHDXOBDPUQW-UHFFFAOYSA-N dioctyl decanedioate Chemical compound CCCCCCCCOC(=O)CCCCCCCCC(=O)OCCCCCCCC MIMDHDXOBDPUQW-UHFFFAOYSA-N 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、貧溶媒や非溶媒が残留
する芳香族ポリカーボネート粉粒体を乾燥する方法に関
する。更に詳しくは、貧溶媒や非溶媒が残留する芳香族
ポリカーボネート粉粒体を、分子量低下や色相悪化を生
じることなく、また異物を増加させることなく乾燥する
方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for drying an aromatic polycarbonate powder granule containing a residual poor solvent or non-solvent. More specifically, the present invention relates to a method for drying an aromatic polycarbonate powder or granular material in which a poor solvent or a non-solvent remains, without causing a decrease in molecular weight or deterioration in hue, and without increasing foreign matter.
【０００２】[0002]
【従来の技術】芳香族ポリカーボネートは、通常二価フ
ェノールのアルカリ水溶液とホスゲンを塩化メチレンの
ようなハロゲン含有良溶媒の存在下反応させる所謂溶液
法により製造され、得られる芳香族ポリカーボネートの
溶媒溶液から溶媒を除去し、乾燥工程を経て粉粒体とし
て得られる。こうして得られる芳香族ポリカーボネート
粉粒体には相当量の溶媒が残留し、用途によってはこの
残留溶媒のハロゲンが悪影響を及ぼすため、残留溶媒を
充分に除去する必要がある。しかしながら、この残留溶
媒は通常の乾燥で充分に除去することは困難である。Aromatic polycarbonates are usually produced by a so-called solution method in which an alkaline aqueous solution of a dihydric phenol and phosgene are reacted in the presence of a halogen-containing good solvent such as methylene chloride. The solvent is removed and a drying step is performed to obtain a powder. A considerable amount of the solvent remains in the aromatic polycarbonate powder thus obtained, and the halogen of the residual solvent exerts an adverse effect depending on the application. Therefore, it is necessary to sufficiently remove the residual solvent. However, it is difficult to sufficiently remove this residual solvent by ordinary drying.
【０００３】残留溶媒の充分に少ない芳香族ポリカーボ
ネートの製造法として、芳香族ポリカーボネートの溶媒
溶液、溶媒が残留している芳香族ポリカーボネート粉粒
体又は溶媒が残留している芳香族ポリカーボネート粉粒
体のスラリー等に、貧溶媒や非溶媒を添加混合した後脱
液し、乾燥する方法が知られている。また、貧溶媒であ
るアセトン等によって芳香族ポリカーボネート粉粒体か
ら不純物を抽出除去する方法（特開昭６３−２７８９２
９号公報、特開昭６４−６０２０号公報）が提案されて
いる。かかる方法は、芳香族ポリカーボネート中に残留
する有機溶媒、未反応の二価フェノール、低分子量重合
体、四塩化炭素等の不純物を著しく低減できる優れた方
法である。As a method for producing an aromatic polycarbonate having a sufficiently small residual solvent, a solvent solution of an aromatic polycarbonate, an aromatic polycarbonate powder in which a solvent remains, or an aromatic polycarbonate powder in which a solvent remains is used. A method is known in which a poor solvent or a non-solvent is added to and mixed with a slurry or the like, followed by deliquoring and drying. Further, a method of extracting and removing impurities from the aromatic polycarbonate powder particles by using a poor solvent such as acetone (JP-A-63-27892).
No. 9, JP-A No. 64-6020) have been proposed. This method is an excellent method that can significantly reduce impurities such as an organic solvent, unreacted dihydric phenol, low molecular weight polymer and carbon tetrachloride remaining in the aromatic polycarbonate.
【０００４】しかしながら、これらの方法で得られる芳
香族ポリカーボネート粉粒体には、使用した貧溶媒や非
溶媒が相当量残留し、この粉粒体を通常使用されている
二軸型押出乾燥機、パドルドライヤー、ジャケット付き
ナウターミキサー等の翼型乾燥機で乾燥すると、微粉が
多量発生し、巾広い粒度分布の粉粒体になり、押出性や
取扱性が悪化する。また、微粉が多量に発生することに
より、乾燥機等のベントに微粉が渡り、運転上トラブル
が発生する。However, in the aromatic polycarbonate powder particles obtained by these methods, a considerable amount of the poor solvent or non-solvent used remains, and the powder or particles are usually used in the twin-screw extruder / dryer. When it is dried with a blade dryer such as a paddle dryer or a Nauta mixer with a jacket, a large amount of fine powder is generated, and a powder having a wide particle size distribution is formed, resulting in poor extrudability and handleability. Further, since a large amount of fine powder is generated, the fine powder spreads to a vent of a dryer or the like, which causes a trouble in operation.
【０００５】翼型乾燥機は内部発熱により温度上昇の効
率化を図っており、極めて効率のよい乾燥機であり、芳
香族ポリカーボネート粉粒体の乾燥機として多用されて
いるが、かかる乾燥機により貧溶媒や非溶媒が相当量残
留する芳香族ポリカーボネート粉粒体を乾燥すると、生
産量変更等による残留溶媒量の変動や負荷の変動等によ
り温度制御が困難になり、壁面等への融着による分子量
の低下、製品の色相の悪化、製品中の残留溶媒量の変動
等の問題が発生する。また、負荷による機器の摩耗等に
よって発生する異物量の増大や機器のトラブル等の問題
も発生する。[0005] The blade type dryer is an extremely efficient dryer, which is designed to increase the efficiency of temperature rise due to internal heat generation, and is widely used as a dryer for aromatic polycarbonate powders. When aromatic polycarbonate powder granules containing a considerable amount of poor solvent or non-solvent are dried, temperature control becomes difficult due to changes in the amount of residual solvent due to changes in production volume, changes in load, etc. There are problems such as a decrease in molecular weight, deterioration of product hue, and variation in the amount of residual solvent in the product. In addition, problems such as an increase in the amount of foreign matter generated due to wear of the device due to load and trouble of the device also occur.
【０００６】[0006]
【発明が解決しようとする課題】本発明は、芳香族ポリ
カーボネート粉粒体に残留する貧溶媒や非溶媒を、分子
量低下や色相悪化を生じることなく、また異物を増加さ
せることなく効率よく除去し得る乾燥方法を提供するこ
とを目的とする。DISCLOSURE OF THE INVENTION The present invention efficiently removes a poor solvent or a non-solvent remaining in an aromatic polycarbonate powder, without lowering the molecular weight or deteriorating the hue, and without increasing foreign matter. It is intended to provide a drying method for obtaining the same.
【０００７】本発明者は、上記目的を達成せんとして種
々検討した結果、貧溶媒や非溶媒が残留する芳香族ポリ
カーボネート粉粒体を乾燥するに際し、残留溶媒量が特
定の量になるまでの間非翼型乾燥機により乾燥すれば、
分子量低下や色相悪化を生じることなく、また異物を増
加させることなく、しかも粒径を殆ど変化させることな
く効率よく残留溶媒を除去し得ることを見出し、本発明
を完成した。As a result of various investigations aimed at achieving the above-mentioned object, the present inventor has found that when drying an aromatic polycarbonate powder or granular material in which a poor solvent or a non-solvent remains, until the amount of residual solvent reaches a specific amount. If you dry with a non-wing dryer,
The present invention has been completed by finding that the residual solvent can be efficiently removed without lowering the molecular weight or deteriorating the hue, increasing the amount of foreign substances, and hardly changing the particle size.
【０００８】[0008]
【課題を解決するための手段】本発明は、貧溶媒や非溶
媒が５〜５５重量％残留する芳香族ポリカーボネート粉
粒体を、該溶媒の残留量が少くとも５重量％未満になる
までは非翼型乾燥機で乾燥することを特徴とする芳香族
ポリカーボネート粉粒体の乾燥方法である。According to the present invention, an aromatic polycarbonate powder containing 5 to 55% by weight of a poor solvent or a non-solvent remains until the residual amount of the solvent is at least less than 5% by weight. A method for drying aromatic polycarbonate powder granules, which comprises drying with a non-blade dryer.
【０００９】本発明でいう良溶媒、貧溶媒及び非溶媒
は、W.F.CHRISTOPHER,D.W.FOX 著「ポリカーボネー
ト」、１９６２年、３２〜３３頁の表３−１における分
類中の“Good Solvents ”及び“ Fair Solvents”に該
当する溶媒が良溶媒であり、“PoorSolvents ”、“Ver
y Poor Solvents”及び“Weak Precipitants ”に該当
する溶媒が貧溶媒であり、“Nonsolvents ”に該当する
溶媒が非溶媒である。良溶媒の代表的な例としては四塩
化エタン、１，１，２−三塩化エタン、１，２−二塩化
エタン、塩化メチレン等があげられ、貧溶媒の代表的な
例としてはベンゼン、トルエン、アセトン、シクロヘキ
サン等があげられ、非溶媒の代表的な例としてはヘキサ
ン、ヘプタン等があげられる。The good solvent, poor solvent and non-solvent as used in the present invention are "polycarbonate" by WF CHRISTOPHER, DWFOX, 1962, "Good Solvents" and "Fair Solvents" in the classification in Table 3-1 on pages 32-33. The solvent that corresponds to is a good solvent, "PoorSolvents", "Ver
Solvents corresponding to “y Poor Solvents” and “Weak Precipitants” are poor solvents, and solvents corresponding to “Nonsolvents” are non-solvents. Typical examples of good solvents are ethane tetrachloride, 1,1,2 -Ethane trichloride, 1,2-dichloroethane, methylene chloride and the like, typical examples of the poor solvent include benzene, toluene, acetone, cyclohexane and the like, and typical examples of the non-solvent include Examples include hexane and heptane.
【００１０】本発明でいう芳香族ポリカーボネートは、
下記一般式The aromatic polycarbonate referred to in the present invention is
The following general formula
【化１】 [Chemical 1]
【００１１】［式中、Ｘは炭素数が１〜６の置換又は非
置換アルキレン基、アルキリデン基、シクロアルキリデ
ン基、−Ｓ−、−ＳＯ−、−ＳＯ2 −、−Ｏ−又は−Ｃ
Ｏ−であり、Ｙは水素原子、炭素数が１〜３のアルキル
基又はハロゲン原子である。］で表される二価フェノー
ルの一種又は二種以上と、ホスゲンやジアリールカーボ
ネート等のカーボネート前駆物質を反応させさせて得ら
れる芳香族ポリカーボネートであり、かかる芳香族ポリ
カーボネートにテレフタル酸、イソフタル酸、ナフタレ
ンジカルボン酸等の芳香族ジカルボン酸、スベリン酸、
セバシン酸のような脂肪族飽和ジカルボン酸を共重合し
たポリエステルカーボネートであってもよく、また分岐
化された芳香族ポリカーボネートであってもよい。特に
二価フェノールとしてビスフェノールＡを用いて得られ
る芳香族ポリカーボネートが好ましく、その分子量は特
に制限する必要はないが、粘度平均分子量で表して１
２，０００〜５０，０００の範囲が好ましい。[Wherein X is a substituted or unsubstituted alkylene group having 1 to 6 carbon atoms, an alkylidene group, a cycloalkylidene group, -S-, -SO-, -SO 2- , -O- or -C.
O-, and Y is a hydrogen atom, an alkyl group having 1 to 3 carbon atoms, or a halogen atom. ] An aromatic polycarbonate obtained by reacting one or more dihydric phenols represented by the following with a carbonate precursor such as phosgene or diaryl carbonate, wherein terephthalic acid, isophthalic acid, or naphthalene is added to the aromatic polycarbonate. Aromatic dicarboxylic acid such as dicarboxylic acid, suberic acid,
It may be a polyester carbonate obtained by copolymerizing an aliphatic saturated dicarboxylic acid such as sebacic acid, or may be a branched aromatic polycarbonate. In particular, an aromatic polycarbonate obtained by using bisphenol A as the dihydric phenol is preferable, and its molecular weight is not particularly limited, but it is 1 in terms of viscosity average molecular weight.
The range of 2,000 to 50,000 is preferable.
【００１２】本発明で対象にする上記芳香族ポリカーボ
ネートの粉粒体は、任意の方法で製造されたものであっ
てもよく、その形状は任意であり、大きさも通常粉粒体
と言われる程度の大きさであれば何等制限する必要はな
いが、貧溶媒の一種又は二種以上及び／又は非溶媒の一
種又は二種以上が５〜５５重量％、好ましくは８〜５５
重量％残留する芳香族ポリカーボネート粉粒体であり、
水分の残留量が１重量％以下のものが好ましい。このよ
うな貧溶媒及び／又は非溶媒の添加方法、添加圧力は特
に制限する必要は無い。また添加温度はガラス転移温度
以下であればよい。この残留溶媒量が５重量％未満の粉
粒体では本発明の方法による必要はなく、５５重量％よ
り多量の溶媒が残留する粉粒体では乾燥中に塊状になり
本発明の目的が達成し得ない。このように多量の溶媒が
残留する粉粒体は、加熱等によって適当な残留溶媒量に
すればよい。The above-mentioned aromatic polycarbonate powder or granule to be used in the present invention may be produced by any method, and its shape is arbitrary, and its size is also a level that is usually called a granule or granule. There is no need to limit it so long as it is 5 to 55% by weight, preferably 8 to 55% by weight of one or more poor solvents and / or one or more nonsolvents.
Aromatic polycarbonate powder particles that remain by weight%,
The residual amount of water is preferably 1% by weight or less. The method of adding such a poor solvent and / or non-solvent and the pressure of addition are not particularly limited. The addition temperature may be the glass transition temperature or lower. It is not necessary to use the method of the present invention for the powder or granular material having a residual solvent amount of less than 5% by weight, and for the powder or granular material having a residual solvent amount of more than 55% by weight, the powder or granular material may be agglomerated during drying to achieve the object of the present invention. I don't get it. The powder or granular material in which a large amount of solvent remains may be heated to a suitable amount of residual solvent.
【００１３】本発明にあっては、かかる芳香族ポリカー
ボネート粉粒体の残留溶媒量が少くとも５重量％未満に
なるまでは非翼型乾燥機を使用して連続式又は回分式に
より乾燥する。残留溶媒量が５重量％未満になる以前、
即ち残留溶媒量が５重量％以上であるときに非翼型乾燥
機による乾燥を止め、以後の乾燥を他の形式の乾燥機に
よって乾燥するときは、粉粒体の分子量低下や色相悪
化、異物の増加、更には微粉の発生を避けることはでき
なくなる。残留溶媒量が５重量％未満になった以後の乾
燥では、最早粉粒体の分子量低下、色相悪化、異物の増
加、微粉の発生は生じ難くなり、任意の形式の乾燥機を
使用することができる。本発明の非翼型乾燥機による乾
燥には、特別の条件をとる必要はなく、通常の乾燥条件
でよい。例えばビスフェノールＡからの芳香族ポリカー
ボネート粉粒体では常圧下４０〜１５０℃で２０〜１８
０分間程度でよく、また減圧下で乾燥してもよい。In the present invention, the aromatic polycarbonate powder or granules are dried continuously or batchwise by using a non-blade dryer until the residual solvent amount becomes at least less than 5% by weight. Before the residual solvent amount is less than 5% by weight,
That is, when the amount of the residual solvent is 5% by weight or more, the drying by the non-blade type dryer is stopped, and when the subsequent drying is performed by the other type of dryer, the molecular weight of the granular material is lowered, the hue is deteriorated, and the foreign matter It is impossible to avoid the increase of the amount of dust and the generation of fine powder. In the drying after the residual solvent amount becomes less than 5% by weight, the decrease in the molecular weight of the powder or granular material, the deterioration of the hue, the increase of the foreign matter and the generation of the fine powder are less likely to occur, and the dryer of any type can be used. it can. For drying with the non-blade dryer of the present invention, it is not necessary to take special conditions, and ordinary drying conditions may be used. For example, in the case of aromatic polycarbonate granules from bisphenol A, it is 20 to 18 at 40 to 150 ° C under normal pressure.
It may take about 0 minutes or may be dried under reduced pressure.
【００１４】本発明で使用する非翼型乾燥機は、粉粒体
にシェヤーのかからない形式の乾燥機であり、例えばド
ラムドライヤー、スチームチューブドライヤー、バンド
型乾燥機、流動乾燥機等があげられる。また、非翼型乾
燥機以外の形式の翼型乾燥機は翼の回転により粉粒体に
剪断力をかけて自己発熱（内部発熱）を発生させて熱効
率を向上させた乾燥機であり、例えばパドルドライヤ
ー、マルチフィンドライヤー等があげられる。The non-blade type dryer used in the present invention is a type of dryer in which the granules do not have sheer, and examples thereof include a drum dryer, a steam tube dryer, a band type dryer and a fluidized dryer. In addition, blade type dryers other than the non-blade type dryer are dryers that generate a self-heating (internal heat generation) by applying a shearing force to the powder particles by the rotation of the blades to improve thermal efficiency. Examples include paddle dryers and multi-fin dryers.
【００１５】[0015]
【実施例】以下に実施例をあげて更に説明する。なお、
測定は下記の方法によった。 (a) 異物量（個／g)：試料２０g を塩化メチレン２００
０mlに溶解し、各粒径区分における異物濃度をレーザー
センサーにより液体微粒子カウンター（HIAC/ROYCO社
製）を用いて光散乱法で０．５μm 以上の異物を測定し
た。 (b) 平均粒径(mm)及び粒度分布（n)：ロジン・ラムラー
の式のｎを日本粉体工業協会編、造粒便覧、１編、２
章、２・４項の粒度測定法に準拠して測定した。ロジン
・ラムラーの式のｎは粒度分布の目安になり、値が大き
い程粒度分布の巾が狭いことを示す。EXAMPLES The present invention will be further described below with reference to examples. In addition,
The measurement was performed by the following method. (a) Amount of foreign matter (pieces / g): 20 g of the sample was used as methylene chloride
The particles were dissolved in 0 ml, and the concentration of foreign matter in each particle size section was measured by a light scattering method using a liquid fine particle counter (manufactured by HIAC / ROYCO) with a laser sensor to measure foreign matter of 0.5 μm or more. (b) Average particle size (mm) and particle size distribution (n): n in the Rosin-Rammler equation is edited by Japan Powder Industry Association, Granulation Handbook, 1 edition, 2
It was measured according to the particle size measurement method in Chapter 2.4. The n in the Rosin-Rammler equation is a measure of the particle size distribution, and the larger the value, the narrower the width of the particle size distribution.
【００１６】(c) 粘度平均分子量（Ｍ）：試料０．７g
を塩化メチレン１００mlに溶解した溶液から２０℃でオ
ストワールド粘度計により比粘度（ηsp）を測定し、次
式により計算した。(C) Viscosity average molecular weight (M): 0.7 g of sample
Was dissolved in 100 ml of methylene chloride, and the specific viscosity (η sp ) was measured by an Ostworld viscometer at 20 ° C. and calculated by the following formula.
【００１７】[0017]
【数１】ηsp／Ｃ＝［η］＋Ｋ［η］2 Ｃ ［η］＝１．２３×１０-4Ｍ0.83 （式中、Ｃは濃度で０．７、Ｋは定数で０．４５であ
る） (d) 色相(b値）：射出成形機により２８０℃で５０×５
０×５mmの見本板を成形し、色差計［スガ試験機（株）
製］により JIS K−７１０５−Z ８７２２準拠して測定
した。値が小さい程黄色味が小さいことを示す。 (e) 塩素残留量（ppm)：全有機ハロゲン分析装置［三菱
化成（株）製 TOX］により測定した。 (f) アセトン及びn-ヘプタンの残留量（ppm)：ガスクロ
マトグラフィー［（株）日立製作所製２６３型］により
カラム充填剤にジオクチルセバケートを用い、アセトン
は１５０℃、n-ヘプタンは２５０℃でヘッドスペース法
で測定した。## EQU1 ## η sp / C = [η] + K [η] 2 C [η] = 1.23 × 10 −4 M 0.83 (where C is the concentration of 0.7 and K is a constant of 0.45 (D) Hue (b value): 50 × 5 at 280 ° C. by injection molding machine
A 0x5mm sample plate was formed and color difference meter [Suga Test Instruments Co., Ltd.
Manufactured according to JIS K-7105-Z 8722. The smaller the value, the smaller the yellow tint. (e) Residual amount of chlorine (ppm): measured with a total organic halogen analyzer [TOX manufactured by Mitsubishi Kasei Co., Ltd.]. (f) Residual amount of acetone and n-heptane (ppm): Dioctyl sebacate was used as a column packing material by gas chromatography [Hitachi Ltd. Model 263], acetone was 150 ° C, n-heptane was 250 ° C. Was measured by the headspace method.
【００１８】[0018]
【実施例１】 (A) ビスフェノールＡを塩化メチレンの存在下ホスゲン
と常法によって反応させ、充分に精製した粘度平均分子
量２３，５００の芳香族ポリカーボネートの塩化メチレ
ン溶液（濃度１５重量％）をニーダーに投入して塩化メ
チレンを除去した後粗粉砕し、次いで目開き５mmのスク
リーン付きハンマーミルにより粉砕し、水を添加して芳
香族ポリカーボネート粉粒体濃度２５重量％、液温３５
℃の水スラリーを得た。Example 1 (A) Bisphenol A was reacted with phosgene in the presence of methylene chloride by a conventional method, and a sufficiently purified methylene chloride solution of aromatic polycarbonate having a viscosity average molecular weight of 23,500 (concentration 15% by weight) was kneadered. To remove methylene chloride and then coarsely pulverize, then pulverize with a hammer mill with a screen having a 5 mm opening, add water to add aromatic polycarbonate powder concentration of 25% by weight, liquid temperature of 35
A water slurry of ℃ was obtained.
【００１９】(B) このスラリーを攪拌下９５℃に昇温し
て１時間保持した後、遠心分離機により脱水し、パドル
ドライヤーにより１４５℃で４時間予備乾燥して塩素残
留量２，９００ppm の粉粒体を得た。この予備乾燥後の
粉粒体の異物量、平均粒径、粒度分布、粘度平均分子
量、色相を表１に示した。(B) This slurry was heated to 95 ° C. under stirring and held for 1 hour, then dehydrated by a centrifuge and pre-dried at 145 ° C. for 4 hours by a paddle dryer to obtain a chlorine residual amount of 2,900 ppm. A granular material was obtained. Table 1 shows the amount of foreign matter, the average particle size, the particle size distribution, the viscosity average molecular weight, and the hue of the pre-dried powder.
【００２０】(C) この粉粒体をドラムドライヤーに投入
し、攪拌下常温で粉粒体に対して５０重量％のアセトン
を加え、３０分間混合した後１４５℃に昇温して４時間
本乾燥した。本乾燥後の粉粒体の異物量、平均粒径、粒
度分布、粘度平均分子量、色相、塩素残留量、アセトン
残留量を表１に示した。(C) The powder and granules were put into a drum dryer, 50% by weight of acetone was added to the powder and granules at room temperature with stirring, and the mixture was mixed for 30 minutes and then heated to 145 ° C. for 4 hours. Dried. Table 1 shows the amount of foreign matter, the average particle size, the particle size distribution, the viscosity average molecular weight, the hue, the residual chlorine amount, and the residual acetone amount of the powder after the main drying.
【００２１】[0021]
【実施例２】本乾燥時間を１時間にする以外は実施例１
と同様に実施してアセトン残留量が０．３重量％の芳香
族ポリカーボネート粉粒体を得た。更にこの粉粒体をパ
ドルドライヤーにより１４５℃で３時間乾燥し、その評
価結果を表１に示した。Example 2 Example 1 except that the main drying time is 1 hour.
Acetone residual amount of 0.3 wt% was obtained in the same manner as described above to obtain an aromatic polycarbonate powder or granular material. Further, the powder and granules were dried with a paddle dryer at 145 ° C. for 3 hours, and the evaluation results are shown in Table 1.
【００２２】[0022]
【実施例３】実施例１(a) で得た芳香族ポリカーボネー
ト粉粒体濃度２５重量％、液温３５℃の水スラリーに攪
拌下常温で粉粒体に対して３０重量％のn-ヘプタンを加
えて２０分間混合した後、攪拌下９５℃に昇温して１時
間保持した後、遠心分離機により脱水し、ドラムドライ
ヤーにより１４５℃で４時間予備乾燥してn-ヘプタン残
留量１．８重量％の粉粒体を得た。この予備乾燥後の粉
粒体の評価結果を表１に示した。Example 3 Aqueous slurry having a concentration of 25% by weight of the aromatic polycarbonate powder obtained in Example 1 (a) and a liquid temperature of 35 ° C. was stirred and at room temperature, 30% by weight of n-heptane was added to the powder. Was added, mixed for 20 minutes, heated to 95 ° C. under stirring and held for 1 hour, dehydrated by a centrifuge, pre-dried at 145 ° C. for 4 hours by a drum dryer, and the residual amount of n-heptane was 1. 8% by weight of powder and granules were obtained. Table 1 shows the evaluation results of the powdery particles after the preliminary drying.
【００２３】更に、攪拌下常温でこの粉粒体に対して５
０重量％のアセトンを加え、３０分間混合した後１４５
℃で４時間本乾燥した。その評価結果を表１に示した。Furthermore, 5 times with respect to this powder and granular material at room temperature with stirring.
After adding 0% by weight of acetone and mixing for 30 minutes, 145
This was dried at 4 ° C for 4 hours. The evaluation results are shown in Table 1.
【００２４】[0024]
【実施例４】実施例１(b) で得た予備乾燥後の芳香族ポ
リカーボネート粉粒体を攪拌槽に投入し、攪拌下常温で
粉粒体に対して１５０重量％のアセトンを加え、３０分
間混合した後遠心分離機により脱液した。得られたアセ
トンを５３重量％含有する粉粒体をドラムドライヤーに
より１４５℃で４時間本乾燥し、その評価結果を表１に
示した。Example 4 The pre-dried aromatic polycarbonate powder obtained in Example 1 (b) was put into a stirring tank, and 150% by weight of acetone was added to the powder at room temperature with stirring to give 30 After mixing for a minute, the liquid was drained by a centrifuge. The obtained granular material containing 53% by weight of acetone was finally dried at 145 ° C. for 4 hours with a drum dryer, and the evaluation results are shown in Table 1.
【００２５】[0025]
【比較例１】実施例１(b) で得た予備乾燥後の芳香族ポ
リカーボネート粉粒体を攪拌槽に投入し、攪拌下常温で
粉粒体に対して５０重量％のアセトンを加え、３０分間
混合した後パドルドライヤーにより１４５℃で４時間本
乾燥し、その評価結果を表１に示した。なお、表１中の
PC は芳香族ポリカーボネートを、 AC はアセトンを、
HP はn-ヘプタンを示す。[Comparative Example 1] The pre-dried aromatic polycarbonate powder obtained in Example 1 (b) was put into a stirring tank, and 50% by weight of acetone was added to the powder at room temperature with stirring to give 30 After mixing for 1 minute, the paddle dryer was used for main drying at 145 ° C. for 4 hours, and the evaluation results are shown in Table 1. In addition, in Table 1
PC is aromatic polycarbonate, AC is acetone,
HP indicates n-heptane.
【００２６】[0026]
【表１】 [Table 1]
【００２７】[0027]
【発明の効果】本発明の乾燥方法によれば、貧溶媒や非
溶媒を含有する芳香族ポリカーボネート粉粒体を、分子
量低下や色相悪化を生じることなく、また異物を増加さ
せることなく乾燥することが可能になり、更に乾燥によ
る粉粒体の形状の変化も極めて少なく、その奏する効果
は格別のものである。EFFECT OF THE INVENTION According to the drying method of the present invention, an aromatic polycarbonate powder containing a poor solvent or a non-solvent can be dried without lowering the molecular weight or deteriorating the hue or increasing the amount of foreign substances. In addition, the change in the shape of the powder or granule due to drying is extremely small, and the effect achieved is exceptional.
Claims (1)
る芳香族ポリカーボネート粉粒体を、該溶媒の残留量が
少くとも５重量％未満になるまでは非翼型乾燥機で乾燥
することを特徴とする芳香族ポリカーボネート粉粒体の
乾燥方法。1. Aromatic polycarbonate powder granules in which a poor solvent or non-solvent remains in an amount of 5 to 55% by weight are dried in a non-blade dryer until the residual amount of the solvent is at least less than 5% by weight. A method for drying an aromatic polycarbonate powder or granule, comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31012492A JP3001733B2 (en) | 1992-11-19 | 1992-11-19 | Method for drying aromatic polycarbonate powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31012492A JP3001733B2 (en) | 1992-11-19 | 1992-11-19 | Method for drying aromatic polycarbonate powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06155466A true JPH06155466A (en) | 1994-06-03 |
| JP3001733B2 JP3001733B2 (en) | 2000-01-24 |
Family
ID=18001467
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP31012492A Expired - Fee Related JP3001733B2 (en) | 1992-11-19 | 1992-11-19 | Method for drying aromatic polycarbonate powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3001733B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4819777A (en) * | 1986-04-14 | 1989-04-11 | Toyota Jidosha Kabushiki Kaisha | System for integrally controlling an engine and an automatic transmission having a device for determining engagement of the lockup clutch when a certain time duration elapses after output of an engagement signal |
-
1992
- 1992-11-19 JP JP31012492A patent/JP3001733B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4819777A (en) * | 1986-04-14 | 1989-04-11 | Toyota Jidosha Kabushiki Kaisha | System for integrally controlling an engine and an automatic transmission having a device for determining engagement of the lockup clutch when a certain time duration elapses after output of an engagement signal |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3001733B2 (en) | 2000-01-24 |
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