JPS61296026A - Production of polybutylene terephthalate having high polymerization degree - Google Patents
Production of polybutylene terephthalate having high polymerization degreeInfo
- Publication number
- JPS61296026A JPS61296026A JP13771685A JP13771685A JPS61296026A JP S61296026 A JPS61296026 A JP S61296026A JP 13771685 A JP13771685 A JP 13771685A JP 13771685 A JP13771685 A JP 13771685A JP S61296026 A JPS61296026 A JP S61296026A
- Authority
- JP
- Japan
- Prior art keywords
- inert gas
- impurities
- polybutylene terephthalate
- adsorption column
- gas
- 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
Landscapes
- Polyesters Or Polycarbonates (AREA)
- Other Resins Obtained By Reactions Not Involving Carbon-To-Carbon Unsaturated Bonds (AREA)
Abstract
Description
【発明の詳細な説明】
〔発明の利用分野〕
本発明は、ポリブチレンテレフタレートの製造方法に関
し、詳しくは連続法の固相重縮合およびテトラヒドロフ
ラン等の除去を行う際に不活性ガスを循環使用する経済
的な高重合度ポリブチレンテレフタレートの製造方法に
関するものである。[Detailed Description of the Invention] [Field of Application of the Invention] The present invention relates to a method for producing polybutylene terephthalate, and more specifically, the present invention relates to a method for producing polybutylene terephthalate. The present invention relates to an economical method for producing highly polymerized polybutylene terephthalate.
従来の不活性ガス中の不純物を除去する方法としては、
例えば特開昭５６−１１２９２６号公報に記載のように
、−基の吸着塔にて吸着、脱着操作を行なっており、吸
着時は不活性ガスを循環使用していた。しかしながら、
脱着時における不活性パージガスは精製されず、不純物
と共に放出されていた。したがって、脱着時には不活性
ガス使用量は増大し、経済的な運転とはならない欠点が
あった。高重合度重合体２００に９／ｈの生産規模のプ
ラントでは、不活性ガスの消費量は約７０トン／月にも
なる。Conventional methods for removing impurities in inert gas include:
For example, as described in JP-A-56-112926, adsorption and desorption operations were performed in a - group adsorption tower, and an inert gas was circulated during adsorption. however,
The inert purge gas during desorption was not purified and was released along with impurities. Therefore, the amount of inert gas used increases during desorption, which has the drawback of not being economical to operate. In a plant with a production scale of 200 to 9/h of high polymerization degree polymer, the consumption of inert gas is about 70 tons/month.
本発明は、このような現状に鑑みてなされたもので、そ
の目的は、不活性ガスの使用量を減少して、ポリブチレ
ンテレフタレートの固相重縮合およびテトラヒドロフラ
ン等の除去を行ない得るポリブチレンテレフタレートの
製造方法を提供する二と−こある。The present invention has been made in view of the current situation, and its purpose is to provide polybutylene terephthalate that can perform solid phase polycondensation of polybutylene terephthalate and remove tetrahydrofuran, etc., while reducing the amount of inert gas used. There are two methods for manufacturing.
本発明のポリブチ１／ンテレフタレ−１・の製造方法は
、粒状の重合体を不活性ガス流ｉｉＩ下に連続的に同相
重合させると同時に、テトラヒドロフラン等の不純物を
連続的に除去するポリブチレンテレフタレートの製造方
法において、不活性ガス精製用吸着塔を少なくとも２基
並列に設＆Ｊて交互に吸着、脱着を行なわせる。この場
合、吸着を連続操作させるためには、脱着１こ要する時
間を吸着時間よりも短かくする必要があり、そのために
は吸着時よりも脱着時の不活性ガス量が膨大に多くなる
。The method for producing polybutylene terephthalate of the present invention involves continuous in-phase polymerization of a granular polymer under an inert gas flow III, and at the same time, continuous removal of impurities such as tetrahydrofuran. In the production method, at least two adsorption towers for inert gas purification are installed in parallel and adsorption and desorption are performed alternately. In this case, in order to perform adsorption continuously, it is necessary to make the time required for desorption shorter than the adsorption time, and for this purpose, the amount of inert gas during desorption is enormously larger than during adsorption.
しかして、脱着時の不活性ガスを経済的に使用するため
、脱着後の不純物を含んだ不活性ガスを精製して、脱着
再生パージガスとして再使用することにより、不活性ガ
スの使用量を減少させるようにしたものである。Therefore, in order to use the inert gas during desorption economically, the inert gas containing impurities after desorption is purified and reused as desorption regeneration purge gas, thereby reducing the amount of inert gas used. It was designed so that
〔発明の実施例〕
以下、本発明の一実施例を図面に基づいて詳細に説明す
る。図面は本発明におけるポリブチレンテレフタレート
の製造装置の一実施例を示した系統図で、１は固相重縮
合反応器、２は加熱器、３は微粉末状のポリブヂレンテ
レフタレートｆｆｉ合体を除去するためのフィルタ、４
は不活性ガス冷却用の熱交換器、５ａ、５ｂは循環ガス
中の不純物（テトラヒドロフラン等）を吸着除去するた
めの吸着塔、６は不活＋’ｌ Ｍス循壌用のブロア、７
は固相重縮合反応器１の出ロガス熱鳳を人口ガスと熱交
換させて回収するための熱交換器、８はガス加熱用の熱
交換器、９は脱着再生パージガス循環用のブロア、１０
はガス加熱用の熱交換器、１１は循環ガス中の不純物（
テトラヒドロフラン等）を除去するための吸収塔、１２
は吸着および脱着操作するためにガスの流れを制御する
ための切替弁を示す。[Embodiment of the Invention] Hereinafter, an embodiment of the present invention will be described in detail based on the drawings. The drawing is a system diagram showing one embodiment of the polybutylene terephthalate production apparatus according to the present invention, in which 1 is a solid-phase polycondensation reactor, 2 is a heater, and 3 is a system in which finely powdered polybutylene terephthalate ffi coalescing is carried out. filter for removing, 4
5 is a heat exchanger for cooling inert gas, 5a and 5b are adsorption towers for adsorbing and removing impurities (tetrahydrofuran, etc.) in circulating gas, 6 is a blower for circulating inert gas, 7 is a heat exchanger for cooling inert gas;
1 is a heat exchanger for recovering the output log gas from the solid-phase polycondensation reactor 1 by heat exchange with artificial gas; 8 is a heat exchanger for heating the gas; 9 is a blower for desorption and regeneration purge gas circulation; 10
11 is a heat exchanger for heating gas, and 11 is a heat exchanger for heating gas; 11 is a heat exchanger for heating gas;
an absorption tower for removing tetrahydrofuran (such as tetrahydrofuran), 12
shows a switching valve for controlling gas flow for adsorption and desorption operations.
原着の粒状のポリブチレンテレフタレート爪合体は、加
熱器２を通過して固相重縮合反応器１の上部に連続的に
供給され、融点以下の温度で固相重縮合およびテトラヒ
ドロフラン等のガスが′ａ離ラフ
０れて、固相重縮合反応器１の下部から製品チノとして
取り出される。The uncoated granular polybutylene terephthalate nail aggregate passes through a heater 2 and is continuously supplied to the upper part of the solid phase polycondensation reactor 1, where it undergoes solid phase polycondensation and gases such as tetrahydrofuran at a temperature below its melting point. The product is removed from the bottom of the solid phase polycondensation reactor 1 as a product.
一方、不活性ガスはブロア６を用いて循環使用され、固
相重縮合反応器ｌ内で循環ガス中に流入してくるテトラ
ヒドロフラン等の不純物を吸着塔５ａにより除去して、
不純物が系内に蓄積することを防止する。吸着塔５ａの
吸着剤が不純物で飽和するｎａに、脱着操作が完了して
いる吸着塔５ｂに切替えて吸着操作を連続的に行なう。On the other hand, the inert gas is recycled using the blower 6, and impurities such as tetrahydrofuran flowing into the circulating gas in the solid phase polycondensation reactor 1 are removed by the adsorption tower 5a.
Prevents impurities from accumulating in the system. When the adsorbent in the adsorption tower 5a is saturated with impurities, the adsorption tower 5b is switched to the adsorption tower 5b for which the desorption operation has been completed, and the adsorption operation is continuously performed.
他方、ブロア９を用いて不活性ガスを加熱器１０で加熱
した後、吸着塔５ａに送り込み、テトラヒドロフラン等
の不純物を離脱させ、吸収塔１１で不純物を含んだ不活
性ガスを冷却水と接触させ、冷却水側に不純物を吸収さ
せて排出することにより、精製された不活性ガスは再生
パージガスとして再使用される。On the other hand, after heating the inert gas with the heater 10 using the blower 9, it is sent to the adsorption tower 5a to remove impurities such as tetrahydrofuran, and the inert gas containing the impurities is brought into contact with cooling water in the absorption tower 11. By absorbing impurities into the cooling water and discharging them, the purified inert gas is reused as regenerated purge gas.
本実施例によれば、脱着時の不活性ガスの循環使用によ
って、吸着および脱着時の不活性ガスの使用量を最小限
に減少することができる。According to this embodiment, by recycling the inert gas during desorption, the amount of inert gas used during adsorption and desorption can be reduced to a minimum.
以−ト説明したように１本発明によれば、粒状のポリブ
チレンテレフタレート重合体を不活性カスパージ下で固
相重縮合およびテトラヒドロフラン等の不純物の除去を
行なうポリブチレンテレフタレートの製造方法において
、少なくとも２基の不活性ガス精製用吸着塔を切換えて
不活性ガスを循環使用すると共に、飽和状態にある吸着
塔に高温不活性ガスを送り込んで不純物を脱着し、不純
物含有不活性ガスを吸収塔で精製した後再使用するよう
にしたものであるから、不活性ガスの使用量を約９８％
低減して、経済的な運転を行なうことができる。As explained below, according to the present invention, in the method for producing polybutylene terephthalate, which involves solid-phase polycondensation of a granular polybutylene terephthalate polymer under an inert caspage and removal of impurities such as tetrahydrofuran, at least two The original adsorption tower for inert gas purification is switched to circulate and use the inert gas, and high-temperature inert gas is sent to the saturated adsorption tower to desorb impurities, and the impurity-containing inert gas is purified by the absorption tower. Because it is designed to be reused after cleaning, the amount of inert gas used has been reduced by approximately 98%.
This allows for economical operation.
図面は本発明を実施した高重合度ポリブチレンテレフタ
レートの製造装置の一例を示ｌノだ系統図である。
１・・・・・・固相重縮合反応器、２・・・・・・加熱
器、３・・・フィルタ、４，７，８．１０・・・・・・
熱交換器、５ａ。The drawing is a system diagram showing an example of an apparatus for producing high polymerization degree polybutylene terephthalate according to the present invention. 1... Solid phase polycondensation reactor, 2... Heater, 3... Filter, 4, 7, 8.10...
Heat exchanger, 5a.
Claims (1)
ガス流通下に固相重縮合させると同時にテトラビドロフ
ラン等の不純物を除去する高重合度ポリブチレンテレフ
タレートの製造方法において、少なくとも２基の不活性
ガス精製用吸着塔を切換えて不活性ガスを循環使用する
と共に、飽和状態にある吸着塔に高温不活性ガスを送り
込んで不純物を脱着し、不純物含有不活性ガスを吸収塔
で精製した後再使用することを特徴とする高重合度ポリ
ブチレンテレフタレートの製造方法。1. In a method for producing highly polymerized polybutylene terephthalate in which granular polybutylene terephthalate polymer is subjected to solid phase polycondensation under inert gas flow and at the same time impurities such as tetrahydrofuran are removed, at least two inert gases are used. In addition to switching the purification adsorption tower and reusing the inert gas, high-temperature inert gas is sent to the saturated adsorption tower to desorb impurities, and the impurity-containing inert gas is purified in the absorption tower and then reused. A method for producing high polymerization degree polybutylene terephthalate, characterized by the following.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13771685A JPS61296026A (en) | 1985-06-26 | 1985-06-26 | Production of polybutylene terephthalate having high polymerization degree |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13771685A JPS61296026A (en) | 1985-06-26 | 1985-06-26 | Production of polybutylene terephthalate having high polymerization degree |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61296026A true JPS61296026A (en) | 1986-12-26 |
| JPH0587528B2 JPH0587528B2 (en) | 1993-12-17 |
Family
ID=15205148
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13771685A Granted JPS61296026A (en) | 1985-06-26 | 1985-06-26 | Production of polybutylene terephthalate having high polymerization degree |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61296026A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01126325A (en) * | 1987-11-11 | 1989-05-18 | Polyplastics Co | Method for solid-phase polymerization of polybutylene terephthalate |
| US7449048B2 (en) | 2002-03-29 | 2008-11-11 | Mitsui Chemicals, Inc. | Method of reusing exhaust gas in polymer production plant |
| EP3214108A1 (en) * | 2016-03-01 | 2017-09-06 | Novamont S.p.A. | Process for removal of tetrahydrofuran |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5128196A (en) * | 1974-09-04 | 1976-03-09 | Toray Industries | KOJUGODOHORIBUCHIRENTEREFUTAREETO NO SEIZOHOHO |
-
1985
- 1985-06-26 JP JP13771685A patent/JPS61296026A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5128196A (en) * | 1974-09-04 | 1976-03-09 | Toray Industries | KOJUGODOHORIBUCHIRENTEREFUTAREETO NO SEIZOHOHO |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01126325A (en) * | 1987-11-11 | 1989-05-18 | Polyplastics Co | Method for solid-phase polymerization of polybutylene terephthalate |
| US7449048B2 (en) | 2002-03-29 | 2008-11-11 | Mitsui Chemicals, Inc. | Method of reusing exhaust gas in polymer production plant |
| EP3214108A1 (en) * | 2016-03-01 | 2017-09-06 | Novamont S.p.A. | Process for removal of tetrahydrofuran |
| WO2017148931A1 (en) * | 2016-03-01 | 2017-09-08 | Novamont S.P.A. | Process for removal of tetrahydrofuran |
| US10711098B2 (en) | 2016-03-01 | 2020-07-14 | Novamont S.P.A. | Process for removal of tetrahydrofuran |
| EP4141045A1 (en) * | 2016-03-01 | 2023-03-01 | Novamont S.p.A. | Process for removal of tetrahydrofuran |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0587528B2 (en) | 1993-12-17 |
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