JPH0587528B2 - - Google Patents
Info
- Publication number
- JPH0587528B2 JPH0587528B2 JP60137716A JP13771685A JPH0587528B2 JP H0587528 B2 JPH0587528 B2 JP H0587528B2 JP 60137716 A JP60137716 A JP 60137716A JP 13771685 A JP13771685 A JP 13771685A JP H0587528 B2 JPH0587528 B2 JP H0587528B2
- Authority
- JP
- Japan
- Prior art keywords
- inert gas
- impurities
- desorption
- polybutylene terephthalate
- circulated
- 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.)
- Expired - Lifetime
Links
- 239000011261 inert gas Substances 0.000 claims description 37
- 238000001179 sorption measurement Methods 0.000 claims description 24
- 239000012535 impurity Substances 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 20
- 238000003795 desorption Methods 0.000 claims description 18
- -1 polybutylene terephthalate Polymers 0.000 claims description 15
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 239000007790 solid phase Substances 0.000 claims description 11
- 238000006068 polycondensation reaction Methods 0.000 claims description 10
- 239000006227 byproduct Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 229920000642 polymer Polymers 0.000 claims description 5
- 230000008929 regeneration Effects 0.000 claims description 5
- 238000011069 regeneration method Methods 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 238000010926 purge Methods 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Polyesters Or Polycarbonates (AREA)
- Other Resins Obtained By Reactions Not Involving Carbon-To-Carbon Unsaturated Bonds (AREA)
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
反応副生物ならびに分解ガス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, and more specifically, the present invention relates to a method for producing polybutylene terephthalate. The present invention relates to an economical method for producing polybutylene terephthalate with a high degree of polymerization in which gas is recycled. .
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、一基の吸着塔にて吸着、脱着操作を行な
つており、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。したがつて、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つ
た。高重合度重合体数百Kg/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。
As a conventional method for removing impurities from inert gas, for example, as described in JP-A-56-112926, adsorption and desorption operations are performed in a single adsorption tower, and during adsorption, Inert gas was used in circulation. However, the inert purge gas during desorption was not purified and was released together 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 several hundred kg/h of highly polymerized polymers, the consumption of inert gas is approximately 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
よび反応副生物ならびに分解ガス等の除去を行な
い得るポリブチレンテレフタレートの製造方法を
提供することにある。
The present invention was made in view of the current situation, and its purpose is to reduce the amount of inert gas used and to improve the solid phase polycondensation of polybutylene terephthalate and the removal of reaction by-products and cracked gas. An object of the present invention is to provide a method for producing polybutylene terephthalate that can be carried out.
本発明のポリブチレンテレフタレートの製造方
法は、粒状の重合体を不活性ガス流通下に連続的
に固相重合させると同時に、反応副生物ならびに
分解ガス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基並列に設けて交
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、脱着に要する時間を吸
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。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。
The method for producing polybutylene terephthalate of the present invention involves continuous solid-phase polymerization of granular polymer under inert gas flow, and at the same time, continuous removal of reaction by-products and impurities of cracked gas. In the production method, at least two adsorption towers for inert gas purification are provided in parallel to perform adsorption and desorption alternately. In this case, in order to operate the 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 significantly larger than during adsorption. Therefore, in order to use the inert gas during desorption economically, the amount of inert gas used is reduced by purifying the inert gas containing impurities after desorption and reusing it as desorption regeneration purge gas. It was designed so that
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、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（反応副生物ならびに分解ガス）を吸着除去
するための吸着塔、６は不活性ガス循環用のブロ
ア、７は固相重縮合反応器１の出口ガス熱量を入
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（反応副生物なら
びに分解ガス）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。
Hereinafter, one 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, 4 is a heat exchanger for cooling with inert gas, and 5a and 5b are in the circulating gas. an adsorption column for adsorbing and removing impurities (reaction by-products and cracked gas); 6 a blower for inert gas circulation; heat exchanger for recovery,
8 is a heat exchanger for gas heating, 9 is a blower for desorption/regeneration purge gas circulation, 10 is a heat exchanger for gas heating, and 11 is a heat exchanger for removing impurities (reaction by-products and cracked gas) in the circulating gas. Absorption tower, 12 indicates a switching valve for controlling the flow of gas for adsorption and desorption operations.
原料の粒状のポリブチレンテレフタレート重合
体は、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反応副
生物ならびに分解ガスのガスが遊離されて、固相
重縮合反応器１の下部から製品チツプとして取り
出される。 The granular polybutylene terephthalate polymer as a raw material is continuously fed to the upper part of the solid-phase polycondensation reactor 1, and the solid-phase polycondensation is performed at a temperature below the melting point, and reaction by-products and cracked gas are liberated. Product chips are taken out from the bottom of the solid phase polycondensation reactor 1.
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１内で循環ガス中に流入
してくる反応副生物ならびに分解ガスの不純物を
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
物で飽和する前に、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。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、反応副生物
ならびに分解ガスの不純物を離脱させ、吸収塔１
１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, the inert gas is recycled using the blower 6, and the reaction by-products and impurities of the cracked gas flowing into the circulating gas in the solid-phase polycondensation reactor 1 are removed by the adsorption tower 5a. Prevents the accumulation of substances in the system. Before the adsorbent in the adsorption tower 5a becomes 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. On the other hand, after the inert gas is heated by the heater 10 using the blower 9, it is sent to the adsorption tower 5a, and the reaction by-products and impurities of the cracked gas are removed.
In step 1, the inert gas containing impurities is brought into contact with cooling water, and the impurities are absorbed into the cooling water and discharged, whereby 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
使用によつて、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 circulating the inert gas during desorption, the amount of inert gas used during adsorption and desorption can be reduced to a minimum.
以上説明したように、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ガス
パージ下で固相重縮合および反応副生物ならびに
分解ガス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替えて不活性ガ
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 above, according to the present invention, in a method for producing polybutylene terephthalate, in which a granular polybutylene terephthalate polymer is subjected to solid phase polycondensation under an inert gas purge and impurities of reaction by-products and cracked gas are removed, at least 2
In addition to switching the inert gas purification adsorption tower to circulate and use the inert gas, high-temperature inert gas is sent to the saturated adsorption tower to desorb impurities.
Since the impurity-containing inert gas is purified in the absorption tower and then reused, the amount of inert gas used can be reduced by about 98%, making it possible to operate economically.
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した系統図
である。
１……固相重縮合反応器、４，７，８，１０…
…熱交換器、５ａ，５ｂ……吸着塔、６，９……
ブロア、１１……吸収塔、１２……切替弁。
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, 4,7,8,10...
...Heat exchanger, 5a, 5b...Adsorption tower, 6,9...
Blower, 11... absorption tower, 12... switching valve.
Claims (1)
不活性ガス流通下の反応器に供給し、融点以下の
温度で固相重縮合させると同時に遊離する反応副
生物ならびに分解ガス等の不純物を循環供給され
る不活性ガスと同伴させて反応器外に排出除去す
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、 前記不活性ガスは少なくとも２基の不活性ガス
精製用吸着塔を切換えて循環供給し、固相重縮合
時不活性ガス中に流入してくる前記不純物を一方
の吸着塔で吸着除去し、精製された不活性ガスを
反応器に循環させると共に、該不純物を吸収して
飽和状態にある他方の吸着塔には別の流路で循環
供給される脱着・再生用の不活性ガスを送り込ん
で不純物を脱着し、該脱着した不純物含有の不活
性ガスを水洗式の吸収塔で水側に不純物を吸収さ
せて不活性ガスを精製した後、該不純物を除去し
た脱着・再生用の不活性ガスを前記不活性ガス精
製用吸着塔の脱着・再生用にに循環させることを
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。[Scope of Claims] 1. Particulate polybutylene terephthalate polymer is supplied to a reactor under inert gas flow, and subjected to solid phase polycondensation at a temperature below its melting point, simultaneously releasing impurities such as reaction by-products and cracked gas. In the method for producing highly polymerized polybutylene terephthalate, the inert gas is discharged and removed from the reactor together with an inert gas that is supplied in circulation, and the inert gas is circulated by switching between at least two adsorption towers for purifying inert gas. The impurities flowing into the inert gas during solid-phase polycondensation are adsorbed and removed by one adsorption tower, and the purified inert gas is circulated to the reactor, and the impurities are absorbed and saturated. Inert gas for desorption and regeneration, which is circulated and supplied through a separate flow path, is sent to the other adsorption tower in the state of desorption to desorb impurities, and the desorbed inert gas containing impurities is sent to the water-washed absorption tower. After purifying the inert gas by absorbing impurities on the water side, the inert gas for desorption/regeneration from which the impurities have been removed is circulated to the adsorption tower for purification of the inert gas for desorption/regeneration. A method for producing highly polymerized polybutylene terephthalate.
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 JPS61296026A (en) | 1986-12-26 |
| JPH0587528B2 true 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) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2513735B2 (en) * | 1987-11-11 | 1996-07-03 | ポリプラスチックス株式会社 | Solid-state polymerization method of polybutylene terephthalate |
| KR100633739B1 (en) | 2002-03-29 | 2006-10-13 | 미쓰이 가가쿠 가부시키가이샤 | Method of recycling waste 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61296026A (en) | 1986-12-26 |
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