JPS612701A - Polymerization apparatus and its use - Google Patents
Polymerization apparatus and its useInfo
- Publication number
- JPS612701A JPS612701A JP12071084A JP12071084A JPS612701A JP S612701 A JPS612701 A JP S612701A JP 12071084 A JP12071084 A JP 12071084A JP 12071084 A JP12071084 A JP 12071084A JP S612701 A JPS612701 A JP S612701A
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- Japan
- Prior art keywords
- polymer
- polymerization
- container
- vessel
- transfer device
- Prior art date
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- Polymerisation Methods In General (AREA)
- Other Resins Obtained By Reactions Not Involving Carbon-To-Carbon Unsaturated Bonds (AREA)
Abstract
Description
【発明の詳細な説明】
A、 本発明の技術分野
本発明は可搬、かつ密閉可能な重合装置およびその使用
方法に関する。DETAILED DESCRIPTION OF THE INVENTION A. TECHNICAL FIELD OF THE INVENTION The present invention relates to a portable and sealable polymerization apparatus and method of using the same.
B、 従来技術とその問題点
最近、高透明性の重合体が光学繊維、光学レンズなどの
分野で求められている、
高透明性の重合体を得るには塵埃などの異物、熱劣化物
、光の透過を妨げる添加物などを極力少なくするか、実
質的に存在しない状態にする必要がある。B. Prior art and its problems Recently, highly transparent polymers are in demand in fields such as optical fibers and optical lenses. It is necessary to minimize the amount of additives that impede the transmission of light, or to make them virtually non-existent.
従来の重合装置は通常攪拌機構を有するうえ、モノマや
重合体を送液するためのポンプやバルブなどが存在する
ため、これらから光学的異物が混入し高透明性重合体を
得るのが困難であった。また、従来の高透明性の重合体
を得るバッチ方式(1回ごとにモノマ精製・重合をする
)では生産効率が悪く1.工業的見地から問題であった
。Conventional polymerization equipment usually has a stirring mechanism, as well as pumps and valves for feeding monomers and polymers, which can introduce optical foreign substances and make it difficult to obtain highly transparent polymers. there were. In addition, the conventional batch method (monomer purification and polymerization is performed each time) for producing highly transparent polymers has poor production efficiency. This was a problem from an industrial standpoint.
最近、重合体の透明性が透光性能に大きな影響を与える
光学繊維の分野で高透明性重合体をつくり、それを紡糸
して透光性能の良い光学繊維を得る方法が提案されてい
る。Recently, in the field of optical fibers, where the transparency of a polymer has a large effect on light-transmitting performance, a method has been proposed in which a highly transparent polymer is made and then spun to obtain an optical fiber with good light-transmitting performance.
例えば、特公昭53−42260号公報や特公昭58−
171405号公報はPMMA糸高透明性重合体を連続
塊状重合方式により得るものであり、これらの方式では
配管の途中にポンプ、バルブなどが挿入されているが、
連続的にモノマやポリマが流されているため、これらが
介在による悪影響は比較的小さいが、重合容器には攪拌
機の取付けが不可欠となるなど外部からの異物混入や熱
劣化物の混入の機会が多く、光学繊維にした時の透光性
能のレベルは悪くなる。For example, Japanese Patent Publication No. 53-42260 and Special Publication No. 58-
Publication No. 171405 discloses that a highly transparent PMMA thread polymer is obtained by a continuous bulk polymerization method, and in these methods, pumps, valves, etc. are inserted in the middle of piping.
Since the monomers and polymers are continuously flowed, the negative effects of their presence are relatively small, but it is essential to install a stirrer in the polymerization container, so there is an opportunity for foreign substances or heat-degraded substances to enter from the outside. In many cases, the level of light transmission performance when made into optical fibers deteriorates.
°一方、特公昭57−51645号公報では重合容器に
精製モノマを仕込んだ後、実質的に密閉状態で重合し、
続いて重合容器を冷却し重合体を固化させて取り出し、
次いでこの固化させた重合体を紡糸装置に充填した後、
加熱溶融させて紡糸する−ものである。On the other hand, in Japanese Patent Publication No. 57-51645, after a purified monomer is charged into a polymerization container, the polymerization is conducted in a substantially closed state.
Next, the polymerization container is cooled to solidify the polymer and taken out.
Next, after filling this solidified polymer into a spinning device,
It is heated and melted and spun.
しかしながら、この方法では固化させた重合体を取り出
す時゛やこれを紡糸装置に供給する際、塵埃などの混入
が不可避であるうえ、固化させた重合体を熔融する時に
酸化劣化の影響を受は易く、光学繊維の透光性能のレベ
ルが悪い。However, with this method, when taking out the solidified polymer or feeding it to a spinning device, it is unavoidable that dust etc. are mixed in, and when the solidified polymer is melted, it is not affected by oxidative deterioration. The light transmission performance of the optical fiber is poor.
さらに特開昭58−68003号公報は重合容器に精製
モノマ仕込口込後、実質的に密閉状態で重合し、この重
合体を複合紡糸するもので、この方法で得られる光学繊
維は透光性能を優れているが1回ごとにモノマ精製・重
合・紡糸を行う必要があるため生産効率が劣るという問
題がある。Furthermore, in JP-A-58-68003, after charging a purified monomer into a polymerization vessel, polymerization is carried out in a substantially closed state, and this polymer is composite-spun, and the optical fiber obtained by this method has a light-transmitting property. However, since it is necessary to perform monomer purification, polymerization, and spinning each time, there is a problem that production efficiency is inferior.
C9本発明の目的
本発明は、かかる従来技術の諸欠点に鑑み創案されたも
ので、その目的とするところは重合装置自体、可搬にし
てコンパクトであると共に塵埃や熱劣化物等の混入がな
く、しかも生産効率を著しく向上できる重合装置および
その使用方法を提供することにある。C9 Purpose of the Present Invention The present invention was devised in view of the various drawbacks of the prior art, and its purpose is to make the polymerization apparatus itself portable and compact, and to prevent contamination by dust, heat-degraded substances, etc. It is an object of the present invention to provide a polymerization apparatus and a method for using the same, which can significantly improve production efficiency.
D9本発明の構成 即ち本発明は次の構成からなる。D9 Structure of the present invention That is, the present invention consists of the following configuration.
(11可搬で、密閉可能であり、かつ攪拌機構を有しな
い重合容器であって、しかも該1合容器は重合体移送装
置との接続用係合部を備えてなる重合装置。(11) A polymerization device that is portable, airtight, and does not have a stirring mechanism, and furthermore, the polymerization container is provided with an engaging portion for connection to a polymer transfer device.
(2) 可搬で、密閉可能であり、かつ攪拌機構を有
しない重合容器でモノマを重合した後、該重合体が流動
状態にある状態で該重合容器を重合体移送装置に取付け
、次いで上記重合体を移送装置に移送することを特徴と
する重合体の使用方法。(2) After polymerizing the monomer in a polymerization container that is portable, airtight, and does not have a stirring mechanism, the polymerization container is attached to a polymer transfer device while the polymer is in a fluid state, and then the above-mentioned A method of using a polymer, comprising transferring the polymer to a transfer device.
以下本発明を図面にて詳細に説明する。The present invention will be explained in detail below with reference to the drawings.
第1図は本発明に係る重合装置の1例を示すもので、重
合容器1は攪拌機構を有さす、内面が鏡面(表面の粗さ
は28以上)仕上げされたステンレス鋼で形成されてい
る。容器、内面の表面粗さが粗い場合には洗浄しても清
浄化が難しく、高透明性重合体が得られにくい。重合容
器1にはモノマ仕込口2が取付けられており、仕込口2
に設けたバルブ3を通して重合触媒を含んだ精製モノマ
が仕込まれる。重合容器1の下部は重合体の移送装置に
着脱自在に装着出来るようにフランジからなる係合部4
を備え、このフランジ部4に盲板5を当接してボルト6
で締結して気密性を保持させる。FIG. 1 shows an example of a polymerization apparatus according to the present invention, in which a polymerization container 1 is made of stainless steel with a mirror-finished inner surface (surface roughness of 28 or more) and has a stirring mechanism. . If the surface of the container or inner surface is rough, it is difficult to clean it even by washing, and it is difficult to obtain a highly transparent polymer. A monomer charging port 2 is attached to the polymerization container 1.
A purified monomer containing a polymerization catalyst is charged through a valve 3 provided in the tank. The lower part of the polymerization container 1 has an engaging part 4 made of a flange so that it can be detachably attached to a polymer transfer device.
A blind plate 5 is brought into contact with this flange portion 4, and a bolt 6 is attached.
to maintain airtightness.
仕込口2からモノマを仕込んだ後、仕込口2の先端にキ
ャンプ26を取りつけ、仕込口2の先端が汚れないよう
になされる。仕込口2から仕込まれたモノマは所定の重
合温度、重合時間で重合された後、重合容器1内の重合
体がまだ流動(熔融)状態にあるうちに重合体移送装置
まで搬び、重合容器1の下部の盲板5をはずして重合装
置を装着する。After charging the monomer from the charging port 2, a camp 26 is attached to the tip of the charging port 2 to prevent the tip of the charging port 2 from getting dirty. After the monomer charged from the charging port 2 is polymerized at a predetermined polymerization temperature and polymerization time, it is transported to the polymer transfer device while the polymer in the polymerization container 1 is still in a fluid (molten) state, and is transferred to the polymerization container 1. Remove the blind plate 5 at the bottom of 1 and attach the polymerization device.
なお、ここで重合体移送装置とは重合装置と連結される
べき次行程の成形装置、脱モノマ装置、紡糸装置などで
あり、重合体中の未反応モノマを脱モノマするための脱
モノマ槽などポリマ貯槽的なものも含まれる。Note that the polymer transfer device here refers to a molding device, a demonomer device, a spinning device, etc. for the next process to be connected to the polymerization device, and a demonomer tank for demonomizing unreacted monomers in the polymer. This includes things like polymer storage tanks.
本発明の装置では攪拌翼などがなく、しかも気密性が良
いため外部からの塵埃などの取り込みがないので高透明
性重合体を容易に得ることができる。又、本発明の装置
は可搬式であるので、予め複数個の重合装置を用意して
別々に重合し、これら重合体を順次重合体移送装置に仕
込むことが出来、生産効率を上げる事が出来る。In the apparatus of the present invention, there is no stirring blade or the like, and since the apparatus has good airtightness, no dust or the like is taken in from the outside, so that a highly transparent polymer can be easily obtained. Furthermore, since the apparatus of the present invention is portable, it is possible to prepare a plurality of polymerization apparatuses in advance, perform polymerization separately, and sequentially charge these polymers to a polymer transfer apparatus, thereby increasing production efficiency. .
第2図は本発明に係る重合装置の別の実施例で重合容器
1の内面はクロムメッキなどで鏡面状態に形成されてい
る。27は重合容器1の下部に増りつけられた気密性の
良いバルブ、28は周面にネジ部を有する接続用係合部
で、この係合部28にはキャンプ7が嵌装されて気密性
が保持される。FIG. 2 shows another embodiment of the polymerization apparatus according to the present invention, in which the inner surface of the polymerization vessel 1 is plated with chrome or the like to have a mirror surface. 27 is a valve with good airtightness added to the lower part of the polymerization container 1, 28 is a connection engagement part having a threaded part on the circumference, and the camp 7 is fitted into this engagement part 28 to make it airtight. Gender is preserved.
重合容器1の上部には重合体を移送するためのピストン
8が取りつけられ、このピストン8の下部には気密性保
持のためテフロンなどのガスケット9が嵌着−されてい
る。仕込口2から仕込まれたモノマは第1図の場合と同
様に重合された後、重合容器1内の重合体が流動(熔融
)状態にあるうちに重合装置を重合体移送装置の所まで
搬び、重合装置の係合部28を重合体移送装置の係合部
に装着させる。A piston 8 for transferring the polymer is attached to the upper part of the polymerization container 1, and a gasket 9 made of Teflon or the like is fitted to the lower part of the piston 8 to maintain airtightness. After the monomer charged from the charging port 2 is polymerized in the same manner as in the case shown in Fig. 1, the polymerization device is transported to the polymer transfer device while the polymer in the polymerization container 1 is in a fluid (melted) state. Then, the engaging portion 28 of the polymerization device is attached to the engaging portion of the polymer transfer device.
第3図は本発明に係る別の重合装置を例示するもので、
重合容器10は全体がガラスで形成されている。11は
仕込口、12.13は重合容器の上下にそれぞれ形成さ
れた熔封用部兼接続用係合部である。重合容器10は洗
浄、乾燥後、溶封用部12.13がそれぞれ熔封され、
次いでモノマ仕込口11から重合触媒を入れた精製モノ
マを仕込んだ後、仕込口11を熔封して気密性を保持さ
せる。所定の重合を行った後、この重合体がまだ流動(
熔融)状態にあるうちに下部12、上部13を切断し、
下端係合部は重合体移送装置に係合し、上端係合部は例
えばホースを係合しN2ガスなど加圧気体で重合容器1
0の重合体を重合体移送装置に移送する。FIG. 3 illustrates another polymerization apparatus according to the present invention,
The entire polymerization container 10 is made of glass. Reference numeral 11 designates a charging port, and reference numerals 12 and 13 designate sealing portions and connecting engagement portions formed at the top and bottom of the polymerization container, respectively. After the polymerization container 10 is washed and dried, the melt-sealing parts 12 and 13 are melt-sealed, respectively.
Next, after charging purified monomer containing a polymerization catalyst through the monomer charging port 11, the charging port 11 is sealed to maintain airtightness. After a given polymerization, the polymer is still flowing (
Cut the lower part 12 and the upper part 13 while it is in a molten state,
The lower end engaging part engages with a polymer transfer device, and the upper end engaging part engages, for example, a hose to supply the polymerization container 1 with pressurized gas such as N2 gas.
0 polymer to a polymer transfer device.
この場合、重合容器IOを重合体移送装置に気密性良く
係合させるには重合容器10の下部12を実質的に同一
径にし、その長さを少なくとも3CI11以上にする事
が望ましい。In this case, in order to engage the polymerization container IO with the polymer transfer device with good airtightness, it is desirable that the lower part 12 of the polymerization container 10 has substantially the same diameter and its length is at least 3 CI11 or more.
このような簡易装置でも高透明性重合体を得ることがで
きるが、この重合装置の場合、再使用が困難である。Although it is possible to obtain a highly transparent polymer using such a simple device, it is difficult to reuse this polymerization device.
第4図は第1図に示す重合装置を重合体移送装置・紡糸
装置に取りつけた状態を示す概略図で、重合終了後、重
合装置を内部の重合体が流動(熔融)状態にあるうちに
重合体移送装置16の位置まで1般びフランジ15.1
4をボルトにより強固に接合して気密性を保持させる。Figure 4 is a schematic diagram showing the state in which the polymerization apparatus shown in Figure 1 is attached to a polymer transfer apparatus/spinning apparatus. 1 to the location of the polymer transfer device 16 and the flange 15.1
4 are firmly joined with bolts to maintain airtightness.
次いで仕込口2からN2ガスを供給し、その圧力で重合
体を重合体移送装置16に移送させた後、光学繊維のコ
ア成分とするため押出用スクリュ18で移送する。この
移送途中で未反応モノマをベントロ17から脱モノマし
、次いで重合体計量用ギヤポンプ部19に送液する。他
方、光学繊維のクラッド成分となる重合体は押出機21
のホッパ20に塵埃の混入がないように供給され、続い
て押出機21で加熱溶融しながら計量用ギヤポンプ部2
2に送液される。各々のギヤポンプで計量された重合体
は複合用バンク部23で合流し口金24で複合して光学
繊維25として紡出される。得られた光学繊維25は光
伝送性能が優れたものであり、光通信用途などにも有効
に使用できる。Next, N2 gas is supplied from the charging port 2, and the polymer is transferred to the polymer transfer device 16 under the pressure thereof, and then transferred by the extrusion screw 18 to be used as the core component of the optical fiber. During this transfer, unreacted monomer is removed from the vent 17 and then sent to the gear pump section 19 for metering the polymer. On the other hand, the polymer that becomes the cladding component of the optical fiber is produced in an extruder 21.
It is supplied to the hopper 20 of 20 so that no dust is mixed in, and then heated and melted in the extruder 21 while being fed to the metering gear pump part 2.
The liquid is sent to 2. The polymers measured by each gear pump are combined in a composite bank part 23, composited in a spinneret 24, and spun as an optical fiber 25. The obtained optical fiber 25 has excellent optical transmission performance and can be effectively used for optical communication applications.
本発明の重合装置は可搬式で、かつ均一な物性を有する
高透明性重合体を得るため重合容器の内径が15cm以
下、長さが100cm以下のものが好ましい。重合容器
の内径および長さが前述条件を満足しない場合は、得ら
れる重合体が不均一となるうえ、運搬、取付は等が困難
になるため好ましくない。The polymerization apparatus of the present invention is preferably portable, and in order to obtain a highly transparent polymer having uniform physical properties, the polymerization vessel preferably has an inner diameter of 15 cm or less and a length of 100 cm or less. If the inner diameter and length of the polymerization container do not satisfy the above-mentioned conditions, the obtained polymer will not only be non-uniform, but also difficult to transport, install, etc., which is not preferable.
本発明の重合装置は高透明性重合体を得るためには重合
装置の開口部を極力少なくするのが良く、2個乃至4個
の範囲で設けるのが好ましい。開口部が1カ所では重合
体の移送が困難であり、5力所以上では開口部がデッド
スペースとなったりして装置の清浄化に支障を来たすの
で好ましくない。また、本発明の重合装置は高透明性重
合体を得るため、重合中は実質的に開口部が密閉されて
いることが好ましい。In order to obtain a highly transparent polymer, the polymerization apparatus of the present invention preferably has as few openings as possible, and is preferably provided with two to four openings. If there is only one opening, it will be difficult to transfer the polymer, and if there are five or more openings, the opening will become a dead space, which will impede cleaning of the apparatus, which is not preferable. Furthermore, in order to obtain a highly transparent polymer in the polymerization apparatus of the present invention, it is preferable that the opening is substantially sealed during polymerization.
本発明の重合装置はあらゆる重合体の重合装置として使
用可能であるが、高透明性重合体を(尋ろには塊状重合
法による重合体の重合装置として適用するのが好ましい
。塊状重合法を適用するのに好ましい重合体としては、
例えばメチルメタクリレートを主成分とする重合体、ス
チレンを主成分とする重合体、重水素化メチルメタクリ
レートを主成分とする重合体、重水素化スチレンを主成
分とする重合体などが挙げられる。Although the polymerization apparatus of the present invention can be used as a polymerization apparatus for all types of polymers, it is preferable to use it as a polymerization apparatus for polymerizing highly transparent polymers (in particular, by bulk polymerization method. Preferred polymers for application include:
Examples include polymers mainly composed of methyl methacrylate, polymers mainly composed of styrene, polymers mainly composed of deuterated methyl methacrylate, and polymers mainly composed of deuterated styrene.
E、 本発明の効果
本発明の重合装置は上述のごとく構成を有するため可1
般にしてコンパクトであると共に塵埃や熱劣化物等の混
入が極力防止可能である。又本発明によれば重合装置を
複数個用意し同時に取り扱うことも出来るので、例えば
従って高価なモノマを重合する場合、多品種のものを重
合する場合などに特に有用である。また、少量の重合体
は間けつ的に実質的に連続して次行程へ送ることも可能
であり、生産性の点からも有用である。E. Effect of the present invention Since the polymerization apparatus of the present invention has the configuration as described above, it is possible to achieve 1.
In general, it is compact and can prevent dust, heat-degraded substances, etc. from entering as much as possible. Furthermore, according to the present invention, it is possible to prepare a plurality of polymerization apparatuses and handle them at the same time, which is particularly useful, for example, when polymerizing expensive monomers or when polymerizing a wide variety of products. Further, a small amount of the polymer can be sent to the next step substantially continuously intermittently, which is also useful from the viewpoint of productivity.
以下本発明を実施例にて説明する。The present invention will be explained below with reference to Examples.
実施例1 第1図に示すような重合装置2個を使用した。Example 1 Two polymerization apparatuses as shown in FIG. 1 were used.
重合容器の内径は40部mφで、ステンレス鋼で形成さ
れており、内面は事情に(表面粗さ=38)磨かれてい
る。この重合容器の下部の盲板をはずし、n−ヘキサン
で2回洗浄後、蓼留ア七トンで3回洗浄し、その後重合
容器を加熱して乾燥させる。この重合容器に盲板を取り
つけ気密性が十分なことを確認後、精製したメチルメタ
クリレート95部、メチルアクリレート5部、重合開始
剤としてジターシャリブチルパーオキサイド0.002
部、連鎖移動剤L−ブチルメルカプタン0.01部の混
合液400ccを仕込み、仕込口のバルブを閉じて容器
内を密閉した。The polymerization vessel has an inner diameter of 40 parts mφ and is made of stainless steel, the inner surface being polished (surface roughness=38). The blind plate at the bottom of the polymerization vessel was removed, washed twice with n-hexane, and then three times with 50% acetate, and then the polymerization vessel was heated and dried. After attaching a blind plate to this polymerization container and confirming that the airtightness is sufficient, 95 parts of purified methyl methacrylate, 5 parts of methyl acrylate, and 0.002 parts of ditertiary butyl peroxide as a polymerization initiator were added.
400 cc of a mixed solution containing 0.01 part of L-butyl mercaptan as a chain transfer agent were charged, and the valve at the charging port was closed to seal the inside of the container.
このようにしてモノマを仕込んだ2個の重合装置を乾燥
機の中に入れ、100°c−180℃で20時間重合さ
せた。The two polymerization apparatuses charged with the monomers in this manner were placed in a dryer and polymerized at 100°C-180°C for 20 hours.
得られた重合体がまだ熔融状態にある間に盲板をはずし
、第4図に示すような重合体移送装置のフランジ部に装
置した後、重合容器にヒータを取りつけ重合容器中の重
合体が溶融状態を保持するよう200℃に加熱しておく
。その後、仕込口から10kg/cJのN2ガスを繍し
220℃に加熱されている重合体移送装置に重合体を移
送する。重合体中に存在する約3%のモノマは重合体移
送装置のヘントロから真空脱気する。While the obtained polymer was still in a molten state, the blind plate was removed and the device was placed on the flange of a polymer transfer device as shown in Figure 4. A heater was attached to the polymerization container to ensure that the polymer in the polymerization container was Heat to 200°C to maintain a molten state. Thereafter, 10 kg/cJ of N2 gas was supplied from the charging port to transfer the polymer to a polymer transfer device heated to 220°C. Approximately 3% of the monomer present in the polymer is vacuum degassed from the hentro of the polymer transfer device.
最初の重合装置の重合体を移送後、直ちに次の重合装置
を重合体移送装置に取りつけ重合体を移送する。この重
合体を光学繊維のコア成分とする。クラッド成分として
弗化ビニリデンとテトラフルオロエチレンの共重合体を
用いる。クラット成分は押出機で210℃で加熱溶融さ
れる。コア成分、クラッド成分ともにギヤポンプで容量
比で90:10になるように計量し、口金部で複合し5
00μ径の光学繊維として単孔口金から20m/min
で紡糸する。Immediately after transferring the polymer from the first polymerization device, the next polymerization device is attached to the polymer transfer device and the polymer is transferred. This polymer is used as the core component of the optical fiber. A copolymer of vinylidene fluoride and tetrafluoroethylene is used as the cladding component. The Krat component is heated and melted at 210°C in an extruder. Weigh both the core component and cladding component using a gear pump so that the volume ratio is 90:10, and combine them at the mouthpiece.
20m/min from a single hole base as an optical fiber with a diameter of 00μ
Spun with.
このようにして得た光学繊維の透光損失→よ570部m
で88dB/kmであった。従来の攪拌機付重合槽で重
合した重合体からの光学繊維は200dB/kmであっ
た。Transmission loss of the optical fiber thus obtained → 570 parts m
It was 88 dB/km. Optical fibers made from polymers polymerized in a conventional polymerization tank with a stirrer had a power of 200 dB/km.
本発明によれば、得られた重合体が高透明性であるうえ
、次行程の重合体移送装置に容易に気密性良く装着でき
る。また、本発明重合装置は複数個(ここでは2個)の
重合装置の重合体をほぼ連続した状態で次行程の重合体
移送装置に送れることがわかる。According to the present invention, the obtained polymer is highly transparent and can be easily attached to a polymer transfer device for the next step with good airtightness. It is also understood that the polymerization apparatus of the present invention can send polymers from a plurality of (in this case two) polymerization apparatuses almost continuously to the polymer transfer apparatus for the next step.
実施例2
第2図に示すような重合装置を使用した。重合容器の内
径は35m1φでクロムメッキされたステンレス鋼で形
成されている。また重合容器の上部のピストンもクロム
メッキされたステンレス鋼で形成されており、ピストン
と重合容器間の気密性を保つためテフロンガスケットを
使用している。この重合容器をn−ヘキサンで2回洗浄
後、蒸留アセトンで3回洗浄した。その後、この重合装
置を加熱して乾燥さゼる。この重合容器の下部にキャッ
プを装着後、精製したメチルメタクリレート100部、
重合開始剤としてジターシャリブチルパーオキサイド0
.001部、連鎖移動剤とし゛ζn−ブチルメルカプク
ン0.001部の混合液を200cc仕込み、仕込口の
バルブを閉して容器内を密閉した。この重合装置を乾燥
機内に入れ、130°C−180°Cで25時間重合さ
せた。このようにしで重合した重合体が熔融状態を保っ
ている間に重合装置の下部のキャップをはずし、重合体
移送装置のネジ部に装着した。この重合体が重合容器の
中で熔融状態を保持するようヒータを取りつけて220
℃に加熱しておく。その後、重合装置のピストンを油圧
シリンダで加圧して重合体を240℃に加熱された重合
体移送装置に移送する。Example 2 A polymerization apparatus as shown in FIG. 2 was used. The polymerization vessel had an inner diameter of 35 m1φ and was made of chrome-plated stainless steel. The piston at the top of the polymerization vessel is also made of chrome-plated stainless steel, and a Teflon gasket is used to maintain airtightness between the piston and the polymerization vessel. This polymerization vessel was washed twice with n-hexane and then three times with distilled acetone. Thereafter, the polymerization apparatus is heated and dried. After attaching a cap to the bottom of this polymerization container, 100 parts of purified methyl methacrylate,
Ditertiary butyl peroxide 0 as polymerization initiator
.. 0.001 part of a chain transfer agent and 0.001 part of a chain transfer agent, 200 cc of a mixed solution was charged, and the valve at the charging port was closed to seal the inside of the container. This polymerization apparatus was placed in a dryer, and polymerization was carried out at 130°C to 180°C for 25 hours. While the polymer polymerized in this manner remained in a molten state, the lower cap of the polymerization device was removed, and the polymerization device was attached to the threaded portion of the polymer transfer device. A heater is installed to keep this polymer in a molten state in the polymerization container.
Heat to ℃. Thereafter, the piston of the polymerization device is pressurized with a hydraulic cylinder to transfer the polymer to a polymer transfer device heated to 240°C.
重合体中に存在する約4%のモノマは重合体移送移送装
置のヘントロから真空脱気する。この重合体移送装置の
先端に取りつけた金型に重合体を射出し直径30龍φ、
長さ20nの円筒に加圧成型する。この成型物を主波長
660nmのし・−ザーダイオードでその透過光を検出
した所、透過光が99%であった。従来の攪拌翼付重合
槽で重合した重合体の同一形状の成型物について透過光
を検出した所96%であった。Approximately 4% of the monomer present in the polymer is vacuum degassed from the hentro of the polymer transfer transfer device. The polymer was injected into a mold attached to the tip of this polymer transfer device, and the diameter was 30 mm.
Pressure mold it into a cylinder with a length of 20n. When the transmitted light of this molded product was detected using a laser diode having a main wavelength of 660 nm, the transmitted light was 99%. When the transmitted light was detected for a molded product of the same shape of a polymer polymerized in a conventional polymerization tank equipped with stirring blades, the result was 96%.
本発明の重合装置では高透明性重合体が容易に得られ、
かつ次行程の重合体移送に容易に気密性良く装着できる
ことがわかる。With the polymerization apparatus of the present invention, highly transparent polymers can be easily obtained,
Moreover, it can be seen that it can be easily and airtightly installed for transferring the polymer in the next step.
実施例3 第3図に示すような重合装置(容器)を4個使用した。Example 3 Four polymerization apparatuses (containers) as shown in FIG. 3 were used.
この重合容器は“パイレックス”ガラスで出来ており、
内径は30龍φである。開口部は3カ所ある。このガラ
ス重合容器を蒸留アセトンで3回洗浄後、乾燥機内で乾
燥する。This polymerization container is made of “Pyrex” glass,
The inner diameter is 30 mm. There are three openings. This glass polymerization container is washed three times with distilled acetone and then dried in a dryer.
この重合容器の上部と下部の開口部を熔封する。The upper and lower openings of this polymerization container are sealed.
熔封した重合容器の上部と下部は外径10菖層φのスト
レート部を6cm有している。精製したスチレンを仕込
部から少量仕込み、重合容器内を洗浄後、スチレン10
0部、重合開始剤ジターシャリブチルパーオキサイドO
,OO2部、連鎖移動剤n−オクチルメルカプタン0.
01部の混合液を150cc仕込み、その後仕込口を熔
封する。この重合容器を乾燥器の中に入れ、100℃〜
180℃で重合させる。この重合体が溶融状態にある間
に重合容器の上部と下部の先端を切断し、重合容器の下
部は重合体移送装置の取付口にテフロンフェルールを使
った係合部材で気密性良く係合し、上部はN2ガス用テ
フロンホースと同様の係合部材で係合する。重合容器に
はヒーターを巻き210℃に加熱すると共に重合容器の
上部にはN2ガスを入れ23kg/cnlに加圧する。The upper and lower parts of the sealed polymerization container had a straight part of 6 cm with an outer diameter of 10 iris layers φ. After charging a small amount of purified styrene from the charging section and washing the inside of the polymerization container, styrene 10
0 parts, polymerization initiator ditertiary butyl peroxide O
, 2 parts OO, chain transfer agent n-octyl mercaptan 0.
Pour 150 cc of the 01 part mixed solution, and then seal the charging port. Place this polymerization container in a dryer at 100℃~
Polymerize at 180°C. While this polymer is in a molten state, the top and bottom tips of the polymerization container are cut off, and the bottom of the polymerization container is tightly engaged with the attachment port of the polymer transfer device using an engaging member using a Teflon ferrule. , the upper part is engaged with an engagement member similar to a Teflon hose for N2 gas. A heater was wound around the polymerization vessel to heat it to 210°C, and at the same time, N2 gas was introduced into the upper part of the polymerization vessel and the pressure was increased to 23 kg/cnl.
220℃に加熱された重合体移送装置で重合体を計量部
に送り、この成分を光学繊維のコア成分とする。411
1の重合容器の重合体が移送終了後ただちにつなぎかえ
、実質的に連続的に重合体を送液する。クラ・ノド成分
はポリトリフルオロエチルメタクリレートで220℃に
加熱された押出機で溶融加熱し、計量部に送る。コア成
分とクラッド成分の容量比を85:15にし、口金部で
複合し500μの光学繊維として単孔口金から40m/
winで紡出する。The polymer is sent to a measuring section using a polymer transfer device heated to 220° C., and this component is used as a core component of an optical fiber. 411
Immediately after the transfer of the polymer in one polymerization container is completed, the connection is changed, and the polymer is transferred substantially continuously. The Kuranodo component is melted and heated with polytrifluoroethyl methacrylate in an extruder heated to 220°C, and then sent to the measuring section. The capacitance ratio of the core component and cladding component is set to 85:15, and the fiber is composited at the base and is made into a 500μ optical fiber.
Spun with win.
このようにして得た光学繊維は透光損失が610r+n
+で125dB/kI11であった。従来の攪拌機付重
合槽で重した重合体からの光学繊維の透光損失は同一波
長で280dB/kI11であった。The optical fiber thus obtained has a transmission loss of 610r+n
+ was 125 dB/kI11. The light transmission loss of the optical fiber from the polymer layered in a conventional stirrer-equipped polymerization tank was 280 dB/kI11 at the same wavelength.
本発明装置で得られた重合体は高透明性であり、かつ次
行程の重合体移送装置に容易に装着できることがわかっ
た。また、本発明重合装置は複数個(ここでは4個)の
重合装置の重合体をほぼ連続した状態で次行程の重合体
移送装置に送れることがわかった。It was found that the polymer obtained by the apparatus of the present invention has high transparency and can be easily attached to the polymer transfer apparatus for the next step. Furthermore, it has been found that the polymerization apparatus of the present invention can send polymers from a plurality of polymerization apparatuses (four in this case) almost continuously to the polymer transfer apparatus for the next step.
第1図、第2図および第3図はそれぞれ本発明に係る重
合装置を例示する概要図、第4図は本発明に係る重合装
置を重合体移送装置に取りつけた状態を示す概要図であ
る。
■・・・金属製重合容器、2.11・・・仕込口、3゜
27・・・バルブ、4,14・・・フランジ、5・・・
盲板、6.15・・・ボルト、7.26・・・キャップ
、8・・・ピストン、9・・・ガスケット、10・・・
ガラス11合容器、12.13・・・取付口、16・・
・重合体移送装置、17・・・ヘントロ、1日・・・ス
クリュー、19.22・・・ギヤポンプ、20・・・ホ
ッパー、21・・・押出機、23・・・複合用パック部
、24・・・口金、25・・・光学繊維。1, 2, and 3 are schematic diagrams each illustrating a polymerization device according to the present invention, and FIG. 4 is a schematic diagram showing a state in which the polymerization device according to the present invention is attached to a polymer transfer device. . ■... Metal polymerization container, 2.11... Feeding port, 3゜27... Valve, 4, 14... Flange, 5...
Blind plate, 6.15... Bolt, 7.26... Cap, 8... Piston, 9... Gasket, 10...
Glass 11 container, 12.13...Installation port, 16...
・Polymer transfer device, 17...Hentro, 1st...Screw, 19.22...Gear pump, 20...Hopper, 21...Extruder, 23...Composite pack section, 24 ...Base, 25...Optical fiber.
Claims (2)
い重合容器であって、しかも該重合容器は重合体移送装
置との接続用係合部を備えてなる重合装置。(1) A polymerization device that is a portable, sealable polymerization container that does not have a stirring mechanism, and that the polymerization container is provided with an engaging portion for connection to a polymer transfer device.
い重合容器でモノマを重合した後、該重合体が流動状態
にある状態で該重合容器を重合体移送装置に取付け、次
いで上記重合体を移送装置に移送することを特徴とする
重合体の使用方法。(2) After polymerizing the monomer in a polymerization container that is portable, airtight, and does not have a stirring mechanism, the polymerization container is attached to a polymer transfer device while the polymer is in a fluid state, and then the above-mentioned A method of using a polymer, comprising transferring the polymer to a transfer device.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP12071084A JPS612701A (en) | 1984-06-14 | 1984-06-14 | Polymerization apparatus and its use |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP12071084A JPS612701A (en) | 1984-06-14 | 1984-06-14 | Polymerization apparatus and its use |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS612701A true JPS612701A (en) | 1986-01-08 |
Family
ID=14793073
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP12071084A Pending JPS612701A (en) | 1984-06-14 | 1984-06-14 | Polymerization apparatus and its use |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS612701A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2023101190A (en) * | 2022-01-07 | 2023-07-20 | ダイキン工業株式会社 | Polymerization tank for production of fluorine-containing polymer and method for producing fluorine-containing polymer |
-
1984
- 1984-06-14 JP JP12071084A patent/JPS612701A/en active Pending
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2023101190A (en) * | 2022-01-07 | 2023-07-20 | ダイキン工業株式会社 | Polymerization tank for production of fluorine-containing polymer and method for producing fluorine-containing polymer |
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