JPS63268736A - Production of polycarbonate - Google Patents
Production of polycarbonateInfo
- Publication number
- JPS63268736A JPS63268736A JP10304587A JP10304587A JPS63268736A JP S63268736 A JPS63268736 A JP S63268736A JP 10304587 A JP10304587 A JP 10304587A JP 10304587 A JP10304587 A JP 10304587A JP S63268736 A JPS63268736 A JP S63268736A
- Authority
- JP
- Japan
- Prior art keywords
- methylene chloride
- polycarbonate
- solvent
- purified
- recovered
- 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
- 229920000515 polycarbonate Polymers 0.000 title claims abstract description 28
- 239000004417 polycarbonate Substances 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 120
- 238000000034 method Methods 0.000 claims abstract description 25
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims abstract description 20
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 239000012535 impurity Substances 0.000 claims abstract description 14
- 238000004821 distillation Methods 0.000 claims abstract description 11
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 claims abstract description 10
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical class C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229930185605 Bisphenol Natural products 0.000 claims abstract description 5
- 238000010924 continuous production Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 claims 1
- 238000000746 purification Methods 0.000 abstract description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 3
- 238000010992 reflux Methods 0.000 abstract description 3
- 229920000642 polymer Polymers 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract 2
- 230000003247 decreasing effect Effects 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 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 8
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000008188 pellet Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 229910002090 carbon oxide Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 238000012696 Interfacial polycondensation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000007787 solid Substances 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の製造方法に関し、詳しくは
リサイクル溶媒として使用する塩化メチレンから不純物
を除去することにより、高品質のポリカーボネートを効
率よく製造する方法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing polycarbonate, and more specifically, a method for efficiently producing high-quality polycarbonate by removing impurities from methylene chloride used as a recycled solvent. Regarding.
［従来の技術及び発明が解決しようとする問題点］一般
に、ホスゲン法によるポリカーボネートの連続製造プロ
セスにおいては、塩化メチレンを溶媒として用い、これ
をリサイクルさせている。[Prior Art and Problems to be Solved by the Invention] Generally, in the continuous polycarbonate production process using the phosgene method, methylene chloride is used as a solvent and recycled.
しかし、この連続製造プロセスの始動時から暫くの間（
通常は数日から数十臼）、得られるポリカーボネート製
品については、色調が不良であったり、射出成形の金型
を錆付かせるなど様々な問題が発生している。However, for some time after the start of this continuous manufacturing process (
(usually several days to several tens of millimeters), the resulting polycarbonate products have various problems such as poor color tone and rusting of injection molds.
本発明者らは、上述の従来技術の問題点を解消し、連続
プロセスの運転のいかなる時期においても品質の良好な
ポリカーボネートを製造できる方法を開発すべく鋭意研
究を重ねた。The present inventors have conducted extensive research in order to solve the problems of the prior art described above and to develop a method that can produce polycarbonate of good quality at any time during continuous process operation.
その結果、連続製造プロセスのホスゲン製造工程（−酸
化炭素と塩素からホスゲンを得る工程）や重合反応工程
において、不純物としてのクロロホルムや四塩化炭素な
どが発生してリサイクル溶媒である塩化メチレン中に蓄
積し、これが製品に悪影響を及ぼしていることが判明し
た。As a result, impurities such as chloroform and carbon tetrachloride are generated during the phosgene production process (-the process of obtaining phosgene from carbon oxide and chlorine) and the polymerization reaction process in the continuous manufacturing process, and accumulate in the recycled solvent methylene chloride. However, it was found that this had a negative impact on the product.
本発明者らは、かかる知見に基いて研究を進め、リサイ
クル溶媒中の不純物を除去することが、得られるポリカ
ーボネート製品の品質向上に効果的であることを確認し
、本発明を完成するに至った。The present inventors conducted research based on this knowledge and confirmed that removing impurities in recycled solvents is effective in improving the quality of the resulting polycarbonate products, leading to the completion of the present invention. Ta.
すなわち、本発明はビスフェノール類とホスゲンを原料
として使用すると共に、塩化メチレンをリサイクル溶媒
として使用してポリカーボネートを連続的に製造するに
あたり、回収された塩化メチレンの少なくとも一部を精
製し、得られた精製塩化メチレンをリサイクル溶媒とし
て使用することを特徴とするポリカーボネートの製造方
法を提供するものである。That is, the present invention uses bisphenols and phosgene as raw materials and methylene chloride as a recycled solvent to continuously produce polycarbonate, and at least a part of the recovered methylene chloride is purified. The present invention provides a method for producing polycarbonate, characterized in that purified methylene chloride is used as a recycled solvent.
本発明の方法は、ビスフェノールＡ等のビスフェノール
類とホスゲンを原料とするホスゲン法のうちの連続製造
プロセス、特に連続界面重縮合プロセスにおいて有効に
適用される。The method of the present invention is effectively applied to a continuous production process of the phosgene method using bisphenols such as bisphenol A and phosgene as raw materials, particularly a continuous interfacial polycondensation process.
本発明の方法によれば、反応系を循環し再使用に供され
る溶媒、即ちリサイクル溶媒である塩化メチレンを、製
造プロセスの適宜工程（通常は生成したポリカーボネー
トと溶媒の分離工程）から回収して、これを精製し、し
かる後に再度反応系に戻すわけであるが、ここで精製手
段としては、特に制限はなく公知の種々の手段を適用す
ることができる。具体的な精製手段としては、蒸留法。According to the method of the present invention, the solvent that is circulated through the reaction system for reuse, that is, methylene chloride, which is a recycled solvent, is recovered from an appropriate step in the manufacturing process (usually a step for separating the produced polycarbonate and the solvent). This is then purified and then returned to the reaction system, and there are no particular restrictions on the purification means, and various known means can be applied. A specific purification method is the distillation method.
吸着法あるいは膜分離法などがあるが、必ずしもこれら
に限定されず、要するに回収した塩化メチレン中の不純
物を除去しうる手段であればよい。Examples include an adsorption method and a membrane separation method, but the method is not necessarily limited to these methods, and in short, any method that can remove impurities from the recovered methylene chloride may be used.
しかし、好ましい手段としては、蒸留法があげられ、特
に３０〜６０段の多段藩留塔を用いて、還流比０．３〜
５．０．圧力常圧〜２． Ｏｋｇ／ ｃｍ、” Ｇ 。However, a preferred method is a distillation method, in particular using a multi-stage distillation column with 30 to 60 stages, with a reflux ratio of 0.3 to 0.3.
5.0. Pressure normal pressure~2. Okg/cm,”G.
塔頂温度４０〜７０℃、塔底温度４５〜８０°Ｃの条件
で蒸留操作を行うことが最適である。It is optimal to carry out the distillation operation under conditions of a tower top temperature of 40 to 70°C and a tower bottom temperature of 45 to 80°C.
回収した塩化メチレンを精製して不純物を除去するわけ
であるが、ここで塩化メチレンに混入している不純物は
様々なものがある０本発明の方法では、これらの不純物
のうち、特にクロロホルム（ＣＨＣ／！、）や四塩化炭
素（ＣＣ／！、）を除去できればよく、他の極く微量の
不純物（塩素化炭化水素など）については、クロロホル
ムや四塩化炭素を除去する際に同時にその大部分が除か
れる。The recovered methylene chloride is purified to remove impurities, but there are various impurities mixed into the methylene chloride.In the method of the present invention, among these impurities, chloroform (CHC /!,) and carbon tetrachloride (CC/!,), and when removing trace amounts of other impurities (chlorinated hydrocarbons, etc.), most of them can be removed at the same time. is removed.
回収した塩化メチレンの精製の程度は、所望する製品の
品質に応じて異なるが、通常はクロロホルムや四塩化炭
素の濃度（両化合物の合計濃度）が２０ｐｐｎ＋以下、
好ましくは１０ｐｐｍ以下となるようにすればよく、こ
の程度に塩化メチレンを精製できれば、回収した塩化メ
チレンの全部を精製せずとも、その一部のみを精製し、
未精製の塩化メチレンとともに反応系に戻してもよい。The degree of purification of recovered methylene chloride varies depending on the quality of the desired product, but usually the concentration of chloroform and carbon tetrachloride (total concentration of both compounds) is 20 ppn+ or less,
Preferably, it should be 10 ppm or less, and if methylene chloride can be purified to this extent, it is not necessary to purify all of the recovered methylene chloride, but only a part of it,
It may be returned to the reaction system together with unpurified methylene chloride.
本発明の方法を適用するには、既存のポリカーボネート
の連続製造装置に回収塩化メチレンの精製設備を取り付
けるだけでよく、設備費も安価ですみ、また操作も簡単
である。To apply the method of the present invention, it is only necessary to attach a purification equipment for recovered methylene chloride to an existing continuous polycarbonate production apparatus, and the equipment cost is low and the operation is simple.
次に、本発明を実施例および比較例によりさらに詳しく
説明する。Next, the present invention will be explained in more detail with reference to Examples and Comparative Examples.
実施例１
水酸化ナトリウム水溶液（濃度６重量％）にビスフェノ
ールＡを溶解し、濃度１３重量％（固形物換算）のビス
フェノールＡの水酸化ナトリウム水溶液を調製した。こ
の水溶液を４３１ ／ｈｒ。Example 1 Bisphenol A was dissolved in an aqueous sodium hydroxide solution (concentration: 6% by weight) to prepare an aqueous sodium hydroxide solution of bisphenol A with a concentration of 13% by weight (in terms of solid matter). 431/hr of this aqueous solution.
（４６ｋｇ／ｈｒ、 ）の割合で、また塩化メチレンを
１９４２ ／ｈｒ、の割合で、内径８１Ｉｎ、管長２０
ｍの管型反応器に連続的に供給した。(46 kg/hr, ) and methylene chloride at a rate of 1942/hr, inner diameter 81 In, pipe length 20
m tube reactor was continuously fed.
一方、−酸化炭素１．２ｋｇ／ｈｒ、、塩素２．８ｋｇ
／ｈｒ。On the other hand, - carbon oxide 1.2 kg/hr, chlorine 2.8 kg
/hr.
を、活性炭を充填し９０℃に制御した反応器に供給して
ホスゲンを得、これをガス状で連続的に前記管型反応器
に並流にて吹き込み、反応を行った。was supplied to a reactor filled with activated carbon and controlled at 90° C. to obtain phosgene, which was continuously blown in gaseous form into the tubular reactor in parallel flow to carry out the reaction.
次いで、３０ｆｆｉの種型反応器に、上記の反応液を触
媒のトリエチルアミン水溶液（濃度１重量％）０、５
Ｉｔ ／ｈｒ、と併せて連続的に供給し、ポリカーボネ
ートオリゴマーを製造した。Next, the above reaction solution was added to a 30ffi seed reactor with an aqueous solution of triethylamine (concentration 1% by weight) as a catalyst.
It was continuously supplied together with It 2 /hr to produce polycarbonate oligomer.
水相と油相を静置分離後、油相中のポリカーボネートオ
リゴマーの数平均分子量を測定したところ、８００であ
った。After the aqueous phase and oil phase were separated by standing, the number average molecular weight of the polycarbonate oligomer in the oil phase was measured and found to be 800.
上記で得られたポリカーボネートオリゴマー２０１ ／
ｈｒ、、前述と同濃度のビスフェノールＡの水酸化ナト
リウム水溶液１１１／ｈｒ、、濃度２５重量％の水酸化
ナトリウム水溶液０．３Ｉ！、／ｈｒ、。Polycarbonate oligomer 201/
hr,, a sodium hydroxide aqueous solution of bisphenol A with the same concentration as above 111/hr,, 0.3 I of a sodium hydroxide aqueous solution with a concentration of 25% by weight! ,/hr,.
濃度１重量％のトリエチルアミン水溶液０．２ｆ／ｈｒ
、、塩化メチレン１４ ｆ！、／ｈｒ、および分子量調
節剤のｐ−ｔ−ブチルフェノールの４重量％塩化メチレ
ン溶液２．６１ ／ｈｒ、を、直列に連設した８０４２
容の種型反応器二基に連続的に供給して、重合反応を進
行させた。Triethylamine aqueous solution with a concentration of 1% by weight 0.2f/hr
,,methylene chloride 14 f! , /hr, and a 4 wt% methylene chloride solution of pt-butylphenol as a molecular weight regulator, 2.61/hr, were connected in series.
The polymerization reaction was allowed to proceed by continuously supplying the polymer to two seed reactors each having a capacity of 1.
得られた重合液は、塩化メチレンで希釈した後、アルカ
リ洗浄、酸洗浄、水洗浄の工程を経て、ポリカーボネー
トを含む油相と水相とに分離した。The obtained polymerization solution was diluted with methylene chloride, and then subjected to the steps of alkaline washing, acid washing, and water washing, and was separated into an oil phase containing polycarbonate and an aqueous phase.
さらに、ポリカーボネートを含む油相は、薄膜蒸発器、
二軸混練機を通して塩化メチレンを分離するとともに、
ポリカーボネートを粉末化し、その後造粒化してポリカ
ーボネートペレットとした。Additionally, the oil phase containing polycarbonate can be processed using a thin film evaporator,
While separating methylene chloride through a twin-screw kneader,
Polycarbonate was powdered and then granulated to form polycarbonate pellets.
このポリカーボネートの数平均分子量は、２３５００で
あった。The number average molecular weight of this polycarbonate was 23,500.
一方、主として薄膜蒸発器および二軸混練機から、塩化
メチレンが蒸気として回収され、冷却後１ｒｒｒの貯槽
にためられた。Meanwhile, methylene chloride was recovered as vapor mainly from the thin film evaporator and the twin-screw kneader, and was stored in a 1 rrr storage tank after cooling.
次に、この回収された塩化メチレンを、４０段を有する
蒸留塔の２０段目に、５２．０１． ／ｈｒ、で導入し
、塔頂温度４０’Ｃ，塔底温度５０℃、塔頂還流比２．
０で蒸留を行ったところ、塔頂から塩化メチレンが、回
収率９９．５％にて蒸留回収された。Next, this recovered methylene chloride is transferred to the 20th stage of a distillation column having 40 stages at 52.01. /hr, the top temperature was 40'C, the bottom temperature was 50°C, and the top reflux ratio was 2.
When distillation was carried out at 0, methylene chloride was distilled and recovered from the top of the column at a recovery rate of 99.5%.
この蒸留回収された塩化メチレンを、上記前型反応器及
び槽型反応器に導入し、再使用に供した。The methylene chloride recovered by distillation was introduced into the above-mentioned front reactor and tank reactor for reuse.
３００時間連続運転後における塩化メチレン回収貯槽で
の塩化メチレン中のクロロホルム（ＣＨＣｊ！ｓ）、四
塩化炭素（ＣＣ２４）の濃度、並びに得られたポリカー
ボネートベレット中の不純物である塩化メチレン（ＣＨ
２Ｃｆ ｚ ） 、クロロホルム、四塩化炭素の濃度を
測定した。さらに、得られたペレットを用いて、金型績
テスト及び耐熱テストを行った。結果を表に示す。Concentrations of chloroform (CHCj!s) and carbon tetrachloride (CC24) in methylene chloride in the methylene chloride recovery and storage tank after 300 hours of continuous operation, as well as methylene chloride (CH), an impurity in the obtained polycarbonate pellets.
The concentrations of 2Cf z ), chloroform, and carbon tetrachloride were measured. Furthermore, a mold test and a heat resistance test were conducted using the obtained pellets. The results are shown in the table.
実施例２
実施例１において、回収され貯槽から供給される塩化メ
チレンの半分（２６，Ｏｆ／ｈｒ、）を蒸留塔に導入し
て蒸留回収（精製）し、その後残りの未精製の回収塩化
メチレンと混合して再使用に供したこと以外は、実施例
１と同様の操作を行った。Example 2 In Example 1, half of the methylene chloride recovered and supplied from the storage tank (26 Of/hr) was introduced into a distillation column to be distilled and recovered (purified), and then the remaining unpurified recovered methylene chloride The same operation as in Example 1 was performed except that the mixture was mixed with the sample and reused.
結果を表に示す。The results are shown in the table.
比較例１
実施例１において、回収され貯槽にためられた塩化メチ
レンを、蒸留精製することなく再使用に供したこと以外
は、実施例１と同様の操作を行った。結果を表に示す。Comparative Example 1 The same operation as in Example 1 was performed except that the methylene chloride recovered and stored in the storage tank was reused without being purified by distillation. The results are shown in the table.
＊１ 射出成形機を用いて、３２０℃の温度にてポリカ
ーボネートペレットのサンプル１０ｇを１シツツトとし
て、１００シヨツト成形した後の金型（材質Ｓ−５５Ｃ
）の錆発生状況を目視で観察した。*1 Using an injection molding machine, mold 100 shots of 10 g of polycarbonate pellet sample at 320°C (1 shot) (material: S-55C).
) was visually observed for rust occurrence.
＊２ 耐熱テストとして、射出成形機を用いて、３５０
℃の温度にて３０分間ボリカーボネートペレフトをスク
リュー内に滞留させた後、射出成形し、２シヨツト目の
成形品のＹＩ値（黄色度）をＪＩＳ Ｋ−７１０５に準
拠して測定した。*2 As a heat resistance test, using an injection molding machine, 350
The polycarbonate pellets were allowed to stay in the screw for 30 minutes at a temperature of .degree. C., then injection molded, and the YI value (yellowness) of the second shot molded product was measured in accordance with JIS K-7105.
本発明の方法によれば、得られるポリカーボネートは不
純物を殆ど含有していないため、高温下でも色調が安定
しており、熱安定性のすぐれたものとなる。また、クロ
ロホルムや四塩化炭素等の不純物が殆ど存在しないため
、各種成形にあたって、成形金型の錆の発生が抑制され
る等様々な利点がある。According to the method of the present invention, the polycarbonate obtained contains almost no impurities, so the color tone is stable even at high temperatures, and the polycarbonate has excellent thermal stability. In addition, since there are almost no impurities such as chloroform or carbon tetrachloride, there are various advantages such as suppressing the occurrence of rust in molding molds during various moldings.
したがって、本発明の方法は高品質のポリカーボネート
を連続的に製造するものとして有効に利用されることが
期待される。Therefore, it is expected that the method of the present invention will be effectively used to continuously produce high quality polycarbonate.
Claims (4)
ると共に、塩化メチレンをリサイクル溶媒として使用し
てポリカーボネートを連続的に製造するにあたり、回収
された塩化メチレンの少なくとも一部を精製し、得られ
た精製塩化メチレンをリサイクル溶媒として使用するこ
とを特徴とするポリカーボネートの製造方法。(1) In the continuous production of polycarbonate using bisphenols and phosgene as raw materials and methylene chloride as a recycled solvent, at least a portion of the recovered methylene chloride is purified, and the purified chloride obtained is A method for producing polycarbonate, characterized in that methylene is used as a recycled solvent.
物として存在するクロロホルムおよび／または四塩化炭
素を除去する特許請求の範囲第１項記載の製造方法。(2) The production method according to claim 1, wherein methylene chloride is purified to remove chloroform and/or carbon tetrachloride present as impurities in methylene chloride.
ルムおよび／または四塩化炭素を、濃度２０ｐｐｍ以下
に除去する特許請求の範囲第２項記載の製造方法。(3) The manufacturing method according to claim 2, wherein chloroform and/or carbon tetrachloride present as impurities in methylene chloride are removed to a concentration of 20 ppm or less.
膜分離法で行う特許請求の範囲第１項記載の製造方法。(4) The manufacturing method according to claim 1, wherein methylene chloride is purified by a distillation method, an adsorption method, or a membrane separation method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10304587A JPH0694502B2 (en) | 1987-04-28 | 1987-04-28 | Method for producing polycarbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10304587A JPH0694502B2 (en) | 1987-04-28 | 1987-04-28 | Method for producing polycarbonate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63268736A true JPS63268736A (en) | 1988-11-07 |
| JPH0694502B2 JPH0694502B2 (en) | 1994-11-24 |
Family
ID=14343695
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10304587A Expired - Lifetime JPH0694502B2 (en) | 1987-04-28 | 1987-04-28 | Method for producing polycarbonate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0694502B2 (en) |
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|---|---|---|---|---|
| WO2009142227A1 (en) * | 2008-05-21 | 2009-11-26 | 三菱瓦斯化学株式会社 | Manufacturing method for polycarbonate resin granular material |
| WO2013137297A1 (en) * | 2012-03-13 | 2013-09-19 | 出光興産株式会社 | Method for continuous production of polycarbonate |
| WO2014007128A1 (en) | 2012-07-05 | 2014-01-09 | 出光興産株式会社 | Polycarbonate-polyorganosiloxane copolymer and method for continuously producing same |
| KR20140145884A (en) * | 2013-06-14 | 2014-12-24 | 주식회사 엘지화학 | Method For Preparing Polycarbonate |
| KR20140145885A (en) * | 2013-06-14 | 2014-12-24 | 주식회사 엘지화학 | Method For Preparing Polycarbonate |
| JP2017052966A (en) * | 2016-11-15 | 2017-03-16 | 出光興産株式会社 | Polycarbonate-polyorganosiloxane copolymer |
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| US10863667B2 (en) | 2015-09-28 | 2020-12-15 | Precision Planting Llc | Systems and devices for controlling and monitoring liquid applications of agricultural fields |
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1987
- 1987-04-28 JP JP10304587A patent/JPH0694502B2/en not_active Expired - Lifetime
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|---|---|---|---|---|
| WO2009142227A1 (en) * | 2008-05-21 | 2009-11-26 | 三菱瓦斯化学株式会社 | Manufacturing method for polycarbonate resin granular material |
| JP5387573B2 (en) * | 2008-05-21 | 2014-01-15 | 三菱瓦斯化学株式会社 | Method for producing polycarbonate resin granular material |
| KR20140137355A (en) * | 2012-03-13 | 2014-12-02 | 이데미쓰 고산 가부시키가이샤 | Method for continuous production of polycarbonate |
| WO2013137297A1 (en) * | 2012-03-13 | 2013-09-19 | 出光興産株式会社 | Method for continuous production of polycarbonate |
| JP2013189516A (en) * | 2012-03-13 | 2013-09-26 | Idemitsu Kosan Co Ltd | Method for continuous production of polycarbonate |
| US9371419B2 (en) | 2012-07-05 | 2016-06-21 | Idemitsu Kosan Co., Ltd. | Polycarbonate-polyorganosiloxane copolymer and method for continuously producing same |
| KR20150031423A (en) | 2012-07-05 | 2015-03-24 | 이데미쓰 고산 가부시키가이샤 | Polycarbonate-polyorganosiloxane copolymer and method for continuously producing same |
| WO2014007128A1 (en) | 2012-07-05 | 2014-01-09 | 出光興産株式会社 | Polycarbonate-polyorganosiloxane copolymer and method for continuously producing same |
| US9850351B2 (en) | 2012-07-05 | 2017-12-26 | Idemitsu Kosan Co., Ltd. | Polycarbonate-polyorganosiloxane copolymer and method for continuously producing same |
| EP2871200B1 (en) | 2012-07-05 | 2019-01-30 | Idemitsu Kosan Co., Ltd | Polycarbonate-polyorganosiloxane copolymer and method for continuously producing same |
| KR20140145884A (en) * | 2013-06-14 | 2014-12-24 | 주식회사 엘지화학 | Method For Preparing Polycarbonate |
| KR20140145885A (en) * | 2013-06-14 | 2014-12-24 | 주식회사 엘지화학 | Method For Preparing Polycarbonate |
| JP2017052966A (en) * | 2016-11-15 | 2017-03-16 | 出光興産株式会社 | Polycarbonate-polyorganosiloxane copolymer |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0694502B2 (en) | 1994-11-24 |
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