JP2006316090A - Production equipment for olefin polymer - Google Patents

Production equipment for olefin polymer Download PDF

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JP2006316090A
JP2006316090A JP2005136991A JP2005136991A JP2006316090A JP 2006316090 A JP2006316090 A JP 2006316090A JP 2005136991 A JP2005136991 A JP 2005136991A JP 2005136991 A JP2005136991 A JP 2005136991A JP 2006316090 A JP2006316090 A JP 2006316090A
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reaction stop
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JP4506549B2 (en
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Yoshimitsu Onodera
吉光 小野寺
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Sumitomo Chemical Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To safely retain a reaction stopping gas useful for stopping a reaction in a reactor in a shielded state without leakage from the reactor in an ordinary operation in an olefin polymer production process for a vapor-phase polymerization reaction of an olefin in the presence of a catalyst and to surely supply a reaction stopping gas when required. <P>SOLUTION: The production equipment is a reaction stopping gas supply equipment comprising a storage means A for storing a reaction stopping gas useful in stopping a polymerization reaction in a fluidized-bed reactor, a means B for shielding a reaction stopping gas, in which at least two shut-off valves are arranged in series in a piping part for connecting the storage means of the reaction stopping gas to the fluidized-bed reactor and/or gas circulation equipment attached to the reactor and a low-pressure release means C composed of piping connected from the middle part of at least the two shut-off valves arranged in series through an intermediate purge valve to a low-pressure release part. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

本発明はオレフィン重合体の製造装置に関する。さらに詳しくは、触媒の存在下にオレフィンを気相重合反応させるオレフィン重合体製造プロセスにおいて、通常の運転状態においては、反応器における反応の停止に使用する反応停止ガスを反応器に漏洩させることなく遮断した状態で安全に保持することができ、かつ、必要とされた際に確実に反応停止ガスを供給することができる反応停止ガス供給設備を有するオレフィン重合体の製造設備に関するものである。   The present invention relates to an apparatus for producing an olefin polymer. More specifically, in an olefin polymer production process in which an olefin is subjected to a gas phase polymerization reaction in the presence of a catalyst, in a normal operation state, the reaction stop gas used for stopping the reaction in the reactor is not leaked to the reactor. The present invention relates to an olefin polymer production facility having a reaction stop gas supply facility that can be safely held in a blocked state and can reliably supply a reaction stop gas when needed.

不飽和二重結合を有する炭素数２〜２４程度のオレフィン重合体は、さまざまな用途に用いられる有用な物質であり、流動床反応器で触媒を用いて気相重合させ製造されることが多い。近年、高活性で寿命の長いチーグラーナッタ触媒やメタロセン触媒のような触媒系が用いられるようになったため、温度の異常な上昇などの異常現象が見られたときなど流動床反応器の停止に際しては、速やかにオレフィン重合を停止するために反応系内に反応停止ガスを導入することが行われる。反応停止ガスの投入が遅れた場合、反応系内に残存するポリオレフィンが融着して塊化する等の問題を生ずることがある（特許文献１参照）。   An olefin polymer having about 2 to 24 carbon atoms having an unsaturated double bond is a useful substance used in various applications, and is often produced by gas phase polymerization using a catalyst in a fluidized bed reactor. . In recent years, catalyst systems such as Ziegler-Natta catalysts and metallocene catalysts with high activity and long life have been used, so when an abnormal phenomenon such as an abnormal rise in temperature is observed, when shutting down the fluidized bed reactor In order to quickly stop the olefin polymerization, a reaction stop gas is introduced into the reaction system. When the introduction of the reaction stop gas is delayed, there may be a problem that the polyolefin remaining in the reaction system is fused and agglomerated (see Patent Document 1).

これらの反応停止ガスには、系内ガス中に数〜数百ＰＰＭ程度含まれるように外部から投入すれば反応を停止させることができるような、強力な反応停止作用をもつガスが一般的に用いられる。この反応停止ガスは通常の運転状態では反応器と遮断された状態に保持され、緊急停止時、もしくは反応停止操作時には、煩雑な操作を伴わずに使用できるように待機させる必要がある。このとき、遮断方法に簡易な方法を採用した場合は、通常運転時に反応停止ガスがごくわずか反応系内に混入するおそれがある。そのような事態が発生した場合、重合反応の低下を引起こし運転の妨げとなる。その対策として、厳重な遮断を行うために同一の配管に直列に複数の遮断弁を設置したり、仕切り板を挿入するなどの方法が採用されることがある。しかし、単純に遮断弁の数を増加したとしても必ずしも反応器へのガスの漏洩を安全に防止できるとは限らず、かつ、緊急に投入を要した場合などに弁の操作が煩雑になり、誤操作を起しかねない。また、仕切り板を挿入する遮断方法では、遮断は完全であるが仕切り板を取りはずすことに要する時間が長いため、緊急用として有用ではない。   These reaction-stopping gases are generally gases having a strong reaction-stopping action so that the reaction can be stopped if they are introduced from the outside so as to be contained in the system gas by several to several hundreds PPM. Used. This reaction stop gas is kept in a state of being disconnected from the reactor in a normal operation state, and it is necessary to wait for an emergency stop or a reaction stop operation so that it can be used without complicated operations. At this time, when a simple method is adopted as the shut-off method, there is a possibility that a very small amount of reaction stop gas is mixed in the reaction system during normal operation. When such a situation occurs, it lowers the polymerization reaction and hinders operation. As countermeasures, a method of installing a plurality of shut-off valves in series in the same pipe or inserting a partition plate may be employed in order to perform severe shut-off. However, even if the number of shut-off valves is simply increased, it is not always possible to safely prevent the leakage of gas to the reactor, and the operation of the valves becomes complicated when urgent charging is required. Misoperations can occur. Further, the blocking method in which the partition plate is inserted is not useful for emergency because the blocking is complete but the time required to remove the partition plate is long.

従来、かかる反応停止ガスの取扱いについて、前記のように反応器へ有効に導入する方法についての記載はあるが、反応停止ガスの反応器への漏洩を安全に防止し、かつ、緊急時に容易に使用可能な設備等についての記載がなく、有効な対策が求められていた。   Conventionally, there is a description of the method of effectively introducing the reaction stop gas into the reactor as described above, but it is possible to safely prevent the reaction stop gas from leaking into the reactor and easily in an emergency. There was no description of available equipment, and effective measures were required.

特開平１０−１３９８０２号公報（第1頁〜第２頁）JP-A-10-139802 (first page to second page)

かかる状況において、本発明は、触媒の存在下にオレフィンを気相重合反応させるオレフィン重合体製造プロセスにおいて、通常の運転状態においては反応器における反応の停止に使用する反応停止ガスを反応器に漏洩させることなく遮断した状態で安全に保持することができ、かつ、必要とされた際に確実に反応停止ガスを供給することができる反応停止ガス供給設備を有するオレフィン重合体の製造設備の提供を目的とする。   Under such circumstances, the present invention is a process for producing a gas phase polymerization reaction of an olefin in the presence of a catalyst. In a normal operation state, the present invention leaks a reaction stop gas used for stopping a reaction in the reactor to the reactor. Providing equipment for producing an olefin polymer that has a reaction stop gas supply facility that can be safely held in a shut-off state without interruption, and that can reliably supply a reaction stop gas when needed. Objective.

すなわち本発明は、触媒の存在下にオレフィンを気相重合反応させるオレフィン重合体の製造プロセスにおいて、下記Ａ〜Ｃ手段を含んでなる反応停止ガス供給設備を有することを特徴とするオレフィン重合体の製造装置に係るものである。
Ａ手段：流動床反応器における重合反応を停止させる際に使用する、反応停止ガスを貯蔵する貯蔵手段
Ｂ手段：前記反応停止ガスの貯蔵手段と流動床反応器および／または該反応器に付属するガス循環設備とを連結する配管部分に、少なくとも２基の遮断弁を直列に設置した反応停止ガスの遮断手段
Ｃ手段：前記直列に設置された少なくとも２基の遮断弁の中間部分より中間パージ弁を介して低圧放出部分へ連結された配管よりなる低圧放出手段
前記のＡ手段および／またはＢ手段を少なくとも２セット含んでなる反応停止ガス供給設備を有することおよび反応停止ガス供給設備が、コンピューターにあらかじめプログラムされた手順に従い反応停止ガスを供給することは、本発明における好ましい形態である。 That is, the present invention provides an olefin polymer comprising a reaction stop gas supply facility comprising the following means A to C in a process for producing an olefin polymer in which a gas phase polymerization reaction of olefin is performed in the presence of a catalyst. It relates to a manufacturing apparatus.
Mean A: Storage means for storing the reaction stop gas used when stopping the polymerization reaction in the fluidized bed reactor. Mean B: Means for storing the reaction stop gas, the fluidized bed reactor, and / or the reactor. Reaction-stopping gas shut-off means in which at least two shut-off valves are connected in series to a pipe portion connecting the gas circulation facility C means: an intermediate purge valve from an intermediate portion of the at least two shut-off valves installed in series Low-pressure discharge means comprising a pipe connected to the low-pressure discharge portion via the above-mentioned reaction stop gas supply equipment comprising at least two sets of the A means and / or B means and the reaction stop gas supply equipment provided in the computer Supplying the stop gas according to a pre-programmed procedure is a preferred form in the present invention.

本発明により、触媒の存在下にオレフィンを気相重合反応させるオレフィン重合体製造プロセスにおいて、通常の運転状態においては反応器における反応の停止に使用する反応停止ガスを反応器に漏洩させることなく遮断した状態で安全に保持することができ、かつ、必要とされた際に確実に反応停止ガスを供給することができる反応停止ガス供給設備を有するオレフィン重合体の製造設備を提供することが可能となった。   According to the present invention, in an olefin polymer production process in which an olefin is subjected to a gas phase polymerization reaction in the presence of a catalyst, the reaction stop gas used for stopping the reaction in the reactor is shut off without leaking to the reactor in a normal operation state. It is possible to provide an olefin polymer production facility having a reaction stop gas supply facility that can be safely held in a state in which the reaction stop gas is supplied and can reliably supply the reaction stop gas when needed. became.

本発明における、触媒の存在下にオレフィンを気相重合反応させるオレフィン重合体製造プロセスにおいて、流動床反応器によりエチレン、プロピレン、ブテン、ヘキセンなど炭素数２-２０のオレフィン類を、単独重合または複数を組合わせて重合が行われる。流動床反応器における圧力は０．１−５０ＭＰａＧで反応させることが可能であるが、一般的に１−３ＭＰａＧで反応させることが多い。触媒は、チーグラーナッタ触媒もしくはメタロセン触媒が用いられ、重合温度は一般的に１０−２００℃の範囲内であるが、４０−１００℃程度が好ましい。   In the process for producing an olefin polymer in which gas phase polymerization reaction of olefin is carried out in the presence of a catalyst in the present invention, olefins having 2 to 20 carbon atoms such as ethylene, propylene, butene and hexene are homopolymerized or pluralized by a fluidized bed reactor. The polymerization is carried out in combination. The pressure in the fluidized bed reactor can be reacted at 0.1-50 MPaG, but generally it is often reacted at 1-3 MPaG. As the catalyst, a Ziegler-Natta catalyst or a metallocene catalyst is used, and the polymerization temperature is generally in the range of 10-200 ° C, preferably about 40-100 ° C.

前述したように、このようなオレフィン重合体製造プロセスにおいて高活性で寿命の長い触媒系が用いられるようになり、流動床反応器における反応の停止のために、反応停止ガスを投入する設備を備えるようになった。反応の停止については、計画された反応停止であるならば緊急性を要しないが、突然発生するトラブル時など緊急時には、異常発見後直ちに反応停止ガス投入を行う必要がある。もし、反応停止ガスの投入が遅れた場合、異常反応が継続し流動床反応器の内部で保有されたオレフィン重合体が溶解し巨大な塊が発生することがある。塊が発生した場合、塊の除去に膨大な労力と時間を要することになり、その損失は非常に大きなものとなる。したがって緊急時における反応停止ガスの投入は可及的速やかに行う必要がある。このとき用いられる反応停止ガスとしては、一酸化炭素、酸素、二酸化炭素等、反応停止作用のあるガスが用いられるが、中でも一酸化炭素が好ましく用いられる。   As described above, in such an olefin polymer production process, a highly active and long-life catalyst system has been used, and a facility for injecting a reaction stop gas is provided for stopping the reaction in the fluidized bed reactor. It became so. The stop of the reaction is not urgent if it is a planned stop of the reaction, but in an emergency such as a sudden trouble, it is necessary to input the stop gas immediately after the abnormality is detected. If the introduction of the reaction stop gas is delayed, the abnormal reaction may continue and the olefin polymer retained in the fluidized bed reactor may dissolve and a huge lump may be generated. When a lump is generated, enormous labor and time are required to remove the lump, and the loss is very large. Therefore, it is necessary to input the reaction stop gas in an emergency as quickly as possible. As the reaction stop gas used at this time, a gas having a reaction stop action such as carbon monoxide, oxygen, carbon dioxide or the like is used, and among these, carbon monoxide is preferably used.

このような目的に用いられる反応停止ガスは、通常運転時には、流動床反応器に混入しないように安全に遮断され、緊急時には速やかに投入可能な状態にしておくことが求められる。本発明においては、下記Ａ〜Ｃ手段を含んでなる反応停止ガス供給設備を設置することにより、上記の要請を実現することができる。   The reaction stop gas used for such a purpose is required to be safely shut off so as not to be mixed into the fluidized bed reactor during normal operation, and to be put in a state in which it can be quickly supplied in an emergency. In this invention, said request | requirement is realizable by installing the reaction stop gas supply equipment which comprises the following AC means.

以下、本発明の製造装置の概略を示すフロー図（図１）に基づいて、詳細に説明する。図１に示したオレフィン重合体の製造装置は、流動床反応器１、反応ガス循環ライン２、熱交換器３、製品抜出配管４、循環ガスコンプレッサー５、触媒供給設備６、原料供給設備７、次工程８、反応停止ガス貯槽９ａ、９ｂ、低圧放出部分１０、遮断弁１１ａ、１１ｂ、１１ｃ、１１ｄ、中間パージ弁１２ａ、１２ｂ、反応停止ガス供給配管１３a、１３ｂ、コンピューター１４等を含むように構成されている。次工程には図示していないが生成したオレフィン重合体を処理する乾燥機、混練造粒機等がある。   Hereinafter, it demonstrates in detail based on the flowchart (FIG. 1) which shows the outline of the manufacturing apparatus of this invention. The olefin polymer production apparatus shown in FIG. 1 includes a fluidized bed reactor 1, a reaction gas circulation line 2, a heat exchanger 3, a product extraction pipe 4, a circulation gas compressor 5, a catalyst supply facility 6, and a raw material supply facility 7. , Next step 8, reaction stop gas storage tanks 9a, 9b, low pressure discharge portion 10, shutoff valves 11a, 11b, 11c, 11d, intermediate purge valves 12a, 12b, reaction stop gas supply pipes 13a, 13b, computer 14 and the like It is configured. In the next step, although not shown, there are a dryer, a kneading granulator and the like for processing the produced olefin polymer.

Ａ手段は、流動床反応器１における重合反応を停止させる際に使用する、反応停止ガスを貯蔵する反応停止ガス貯槽９ａ、９ｂ等の貯蔵手段を備えている。かかる貯蔵手段としては、１５ＭＰａＧ程度の圧力に耐えられる高圧容器であればよい。反応停止ガスの必要量は、多くの場合において流動床反応器の中に数１０ｐｐｍ〜数％程度存在させれば効果があるので、例えば、いわゆるガスボンベを数本並列に連結して用いてもよい。また、反応停止ガス使用後、再度反応停止ガス使用可能な状態に復帰することを早めることができるように、このような貯槽を予備として複数持つのが好ましい。反応停止ガスの保持圧力は、反応停止ガスが必要とされる異常反応時に、反応停止に必要な量の反応停止ガスを反応器に十分な速度で投入できる圧力であれば問題ないが、最低でも投入流動床反応器の運転圧力１〜３ＭＰａＧよりも高くしておくことが必要である。   The means A includes storage means such as reaction stop gas storage tanks 9a and 9b for storing the reaction stop gas used when the polymerization reaction in the fluidized bed reactor 1 is stopped. Such storage means may be a high-pressure container that can withstand a pressure of about 15 MPaG. In many cases, the required amount of the reaction stop gas is effective if it is present in the fluidized bed reactor by several tens of ppm to several percent. For example, several so-called gas cylinders may be connected in parallel. . In addition, it is preferable to have a plurality of such storage tanks as a reserve so that it can be quickly returned to the state where the reaction stop gas can be used again after the use of the reaction stop gas. The holding pressure of the reaction stop gas is not a problem as long as it is a pressure at which a sufficient amount of the reaction stop gas can be charged into the reactor at the time of an abnormal reaction that requires the reaction stop gas. It is necessary to keep the operating pressure of the input fluidized bed reactor higher than 1 to 3 MPaG.

Ｂ手段は、前記反応停止ガスの貯蔵手段と流動床反応器および／または該反応器に付属するガス循環設備とを連結する配管部分に、２基以上の遮断弁１１ａ、１１ｂ、１１ｃ、１１ｄ、を直列に設置した反応停止ガスの遮断手段である。ガス循環設備は主として、反応ガス循環ライン２、熱交換器３、循環ガスコンプレッサー５等から構成されている。遮断弁を少なくとも２基直列に設置するのは、反応停止ガスと流動床反応器および／または該反応器に付属するガス循環設備との遮断をより確実にすることができるからである。   B means comprises two or more shut-off valves 11a, 11b, 11c, 11d, and a pipe portion connecting the storage means for the reaction stop gas and the fluidized bed reactor and / or the gas circulation equipment attached to the reactor. Is a means for shutting off the reaction stop gas installed in series. The gas circulation facility mainly comprises a reaction gas circulation line 2, a heat exchanger 3, a circulation gas compressor 5, and the like. The reason for installing at least two shut-off valves in series is that it is possible to more reliably shut off the reaction stop gas from the fluidized bed reactor and / or the gas circulation equipment attached to the reactor.

Ｃ手段は、前記直列に設置された少なくとも２基の遮断弁の中間部分より中間パージ弁を介して低圧放出部分へ連結された配管よりなる低圧放出手段である。具体的には、例えば、２基の遮断弁１１ａと１１ｂの中間部分に中間パージ弁１２ａを設けて、フレアスタック等の低圧放出部分８へパージできるようにする。高圧の反応停止ガスと反応系との間に遮断された低圧部分を設けることにより、反応系への反応停止ガスの混入をさらに確実に防止することができる。低圧部分の圧力は、０〜１ＭＰａＧ程度である。   C means is a low pressure discharge means comprising a pipe connected from the intermediate part of the at least two shutoff valves installed in series to the low pressure discharge part via the intermediate purge valve. Specifically, for example, an intermediate purge valve 12a is provided at an intermediate portion between the two shutoff valves 11a and 11b so that the low pressure discharge portion 8 such as a flare stack can be purged. By providing a low-pressure portion that is blocked between the high-pressure reaction stop gas and the reaction system, it is possible to more reliably prevent the reaction stop gas from being mixed into the reaction system. The pressure in the low pressure portion is about 0 to 1 MPaG.

前記のＢ手段は、少なくとも２セット以上含んでなる反応停止ガス供給設備が好ましい。たとえば反応停止ガスの遮断手段を２セット設け、一方を反応停止ガス供給配管１３aを通じて直接流動床反応器に接続し、他方を反応停止ガス供給配管１３ｂを通じて循環ガスラインに接続しておくことにより、仮に緊急時に１セットの遮断弁の作動が不良であっても、安全確実に反応停止ガスを反応器に供給できる可能性を高めることができるからである。従って、前記のＢ手段は、１セットの供給設備のみでもよいが、そのときは反応停止に必要な量の反応停止ガス投入を十分な速度で供給できるような、適切なサイズの反応停止ガス供給設備であることが好ましい。また、供給設備の設置数は、２セット以上であれば十分な信頼性が得られることが多いが、大量に設置しても設置コストに対する信頼性の向上が小さくなるので、たとえば２〜１０セット程度にするなど、系の重要度や弁の信頼性を評価した上で経済的な設置数を選択する必要がある。   The B means is preferably a reaction stop gas supply facility comprising at least two sets. For example, by providing two sets of reaction stop gas blocking means, one is directly connected to the fluidized bed reactor through the reaction stop gas supply pipe 13a, and the other is connected to the circulation gas line through the reaction stop gas supply pipe 13b. This is because even if the operation of one set of shut-off valves is defective in an emergency, the possibility that the reaction stop gas can be safely and reliably supplied to the reactor can be increased. Therefore, the B means may be only one set of supply equipment, but at that time, a reaction stop gas supply of an appropriate size that can supply an amount of the reaction stop gas necessary for stopping the reaction at a sufficient rate. Equipment is preferred. Further, sufficient reliability is often obtained if the number of installations of the supply facilities is 2 sets or more. However, even if a large number of installations are installed, the improvement in reliability with respect to installation costs is small. It is necessary to select the number of economical installations after evaluating the importance of the system and the reliability of the valves, such as to the extent.

また、緊急時に反応停止ガスを使用すると、一度の使用で反応停止ガス貯槽全量が使用されることが多い。そのためこの貯槽を再び待機状態にするまでは、次の異常反応には対応できない。よって一度反応停止に使用された反応停止ガス貯槽は、何らかの手段で、再び充填し待機させる必要がある。好ましくは、この使用され空となった貯槽をすぐに交換できるように、反応停止ガスが保持された予備の貯槽を、常時１つ以上持つことが好ましい。そうすることですばやく反応停止ガスを使用可能な状態に復帰できるため、反応停止ガスが投入できない時間を最短にすることができ、信頼性を向上することができる。   Further, when the reaction stop gas is used in an emergency, the entire amount of the reaction stop gas storage tank is often used in one use. Therefore, the next abnormal reaction cannot be dealt with until this storage tank is brought into a standby state again. Therefore, the reaction stop gas storage tank once used for stopping the reaction needs to be filled again by some means and waited. Preferably, it is preferable to always have at least one spare storage tank in which the reaction stop gas is held so that the used and empty storage tank can be replaced immediately. By doing so, since the reaction stop gas can be quickly returned to a usable state, the time during which the reaction stop gas cannot be introduced can be minimized, and the reliability can be improved.

さらに、反応停止ガス供給設備の遮断弁および中間パージ弁の作動順序をあらかじめコンピューターにプログラムすることにより、反応停止ガスを供給する際の煩雑な操作を回避することができ、緊急時における信頼性を一層向上することができる。遮断弁および中間パージ弁の作動順序は、例えば、通常運転時に遮断弁１１ａ、１１ｂを閉とし、中間パージ弁１２ａを開にしておく。このとき、もし反応停止ガスが弁１１ｂ、１１ｃから内通漏洩した場合は、それぞれ中間パージ弁１２ａ、１２ｂを経由して低圧放出部分１０へ放出されるのでプロセスに影響を与えることはない。緊急時には、中間パージ弁１２ａを閉にした後、遮断弁１１ａ、１１ｂを同時に開とするようにプログラムしておく。この弁操作は、流動床反応器内に温度センサー等の異常を検出できる手段を設置して異常反応が生じた場合に作動するようにしてもいいし、手動で作動させてもよい。   In addition, since the operation sequence of the shutoff valve and the intermediate purge valve of the reaction stop gas supply facility is programmed in advance in the computer, complicated operations when supplying the reaction stop gas can be avoided, and reliability in an emergency can be improved. This can be further improved. The operation order of the shutoff valve and the intermediate purge valve is such that, for example, the shutoff valves 11a and 11b are closed and the intermediate purge valve 12a is opened during normal operation. At this time, if the reaction stop gas leaks from the valves 11b and 11c, it is discharged to the low pressure discharge portion 10 via the intermediate purge valves 12a and 12b, respectively, so that the process is not affected. In an emergency, the intermediate purge valve 12a is closed and then the shutoff valves 11a and 11b are programmed to be opened simultaneously. This valve operation may be operated when an abnormal reaction occurs by installing means capable of detecting an abnormality such as a temperature sensor in the fluidized bed reactor, or may be operated manually.

以下、実施例によって本発明をより具体的に説明するが、これに限定されることがないのはもとよりのことである。
実施例１
図1に示したオレフィン重合体の製造装置により、２．０ＭＰａＧにおいて、触媒、原料としてエチレンおよび１−ブテン、水素を流動床反応器に供給し、重合させた。通常運転時は遮断弁１１ａ、１１ｂ、１１ｃ、１１ｄは閉、中間パージ弁１２ａ、１２ｂは開の状態で保持した。反応停止ガスとしては貯槽圧力１０ＭＰａＧの一酸化炭素を使用し、貯槽の体積は６２５Ｌであった。低圧放出部分の圧力は５ｋＰａＧであった。この状態で予め定められたプログラムに従って、コンピューターにより遮断弁および中間パージ弁を操作させ一酸化炭素を流動床反応器内へ投入し、反応を停止させた。一酸化炭素は、６２５Ｌの貯槽の圧力が反応器の圧力と同等圧力になるまで投入された。コンピューターにより制御された遠隔操作弁はプログラム通り自動的に作動し、すみやかに投入が完了し反応停止を実現できた。流動床反応器内の状態は、ポリマー塊を形成することなく安定的に停止することができた。また通常運転においても、反応停止ガスの漏洩によるものと考えられる反応低下現象は起ることがなかった。また、この操作には、反応停止ガス貯槽１１ａのガスを使用したが、使用後、反応停止ガス貯槽１１ｂに切替えて、すばやく反応停止ガスを使用可能な状態に復帰することができ、すみやかに緊急事態に備えることができた。 Hereinafter, the present invention will be described more specifically by way of examples. However, the present invention is not limited to these examples.
Example 1
With the olefin polymer production apparatus shown in FIG. 1, at 2.0 MPaG, a catalyst, ethylene, 1-butene and hydrogen as raw materials were supplied to a fluidized bed reactor and polymerized. During normal operation, the shut-off valves 11a, 11b, 11c, and 11d were closed and the intermediate purge valves 12a and 12b were kept open. As the reaction stop gas, carbon monoxide having a storage tank pressure of 10 MPaG was used, and the volume of the storage tank was 625L. The pressure in the low pressure discharge part was 5 kPaG. In this state, according to a predetermined program, the shutoff valve and the intermediate purge valve were operated by a computer, carbon monoxide was introduced into the fluidized bed reactor, and the reaction was stopped. Carbon monoxide was added until the pressure in the 625 L storage tank was equal to the pressure in the reactor. The remote control valve controlled by the computer automatically operated according to the program, and the injection was completed immediately and the reaction stopped. The conditions in the fluidized bed reactor could be stopped stably without forming a polymer mass. Moreover, even in normal operation, there was no occurrence of a reaction lowering phenomenon that was considered to be caused by leakage of the reaction stop gas. Moreover, although the gas of the reaction stop gas storage tank 11a was used for this operation, after use, it can switch to the reaction stop gas storage tank 11b, and can return to the state which can use reaction stop gas quickly, and is urgent. I was prepared for the situation.

本発明の製造装置の概略を示すフロー図である。It is a flowchart which shows the outline of the manufacturing apparatus of this invention.

符号の説明Explanation of symbols

１…流動床反応器、２…循環ガス配管、３…熱交換器、４…製品抜出配管、５…循環ガスコンプレッサー、６…触媒供給ライン、７…原料供給ライン、８…次工程、９ａ、９ｂ…反応停止ガス貯槽、１０…低圧放出部分、１１ａ、１１ｂ、１１ｃ、１１ｄ…遮断弁、１２ａ、１２ｂ…中間パージ弁、１３ａ、１３ｂ…反応停止ガス供給配管、１４…コンピューター

DESCRIPTION OF SYMBOLS 1 ... Fluidized bed reactor, 2 ... Circulating gas piping, 3 ... Heat exchanger, 4 ... Product extraction piping, 5 ... Circulating gas compressor, 6 ... Catalyst supply line, 7 ... Raw material supply line, 8 ... Next process, 9a , 9b ... Reaction stop gas storage tank, 10 ... Low pressure discharge portion, 11a, 11b, 11c, 11d ... Shut-off valve, 12a, 12b ... Intermediate purge valve, 13a, 13b ... Reaction stop gas supply pipe, 14 ... Computer

Claims (4)

触媒の存在下にオレフィンを気相重合反応させるオレフィン重合体の製造プロセスにおいて、下記Ａ〜Ｃ手段を含んでなる反応停止ガス供給設備を有することを特徴とするオレフィン重合体の製造装置。
Ａ手段：流動床反応器における重合反応を停止させる際に使用する、反応停止ガスを貯蔵する貯蔵手段
Ｂ手段：前記反応停止ガスの貯蔵手段と流動床反応器および／または該反応器に付属するガス循環設備とを連結する配管部分に、少なくとも２基の遮断弁を直列に設置した反応停止ガスの遮断手段
Ｃ手段：前記直列に設置された少なくとも２基の遮断弁の中間部分より中間パージ弁を介して低圧放出部分へ連結された配管よりなる低圧放出手段 In the process for producing an olefin polymer in which an olefin is subjected to a gas phase polymerization reaction in the presence of a catalyst, the apparatus for producing an olefin polymer has a reaction stop gas supply facility comprising the following AC means.
Mean A: Storage means for storing the reaction stop gas used when stopping the polymerization reaction in the fluidized bed reactor. Mean B: Means for storing the reaction stop gas, the fluidized bed reactor, and / or the reactor. Reaction-stopping gas shut-off means in which at least two shut-off valves are connected in series to a pipe portion connecting the gas circulation facility C means: an intermediate purge valve from an intermediate portion of the at least two shut-off valves installed in series Low pressure discharge means consisting of a pipe connected to the low pressure discharge part via 請求項１記載のＡ手段を少なくとも２セット含んでなる反応停止ガス供給設備を有することを特徴とする請求項１記載のオレフィン重合体の製造装置。 The apparatus for producing an olefin polymer according to claim 1, further comprising a reaction stop gas supply facility comprising at least two sets of the means A according to claim 1. 請求項１記載のＢ手段を少なくとも２セット含んでなる反応停止ガス供給設備を有することを特徴とする請求項１または２記載のオレフィン重合体の製造装置。 The apparatus for producing an olefin polymer according to claim 1 or 2, further comprising a reaction stop gas supply facility comprising at least two sets of the B means according to claim 1. 請求項１記載の反応停止ガス供給設備が、コンピューターにあらかじめプログラムされた手順に従い反応停止ガスを供給することを特徴とする請求項１から３のいずれかに記載のオレフィン重合体の製造装置。
The apparatus for producing an olefin polymer according to any one of claims 1 to 3, wherein the reaction stop gas supply facility according to claim 1 supplies the reaction stop gas in accordance with a procedure programmed in advance in a computer.
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JPS6072904A (en) * 1983-09-01 1985-04-25 モ−ビル　オイル　コ−ポレ−ション Method and device for injecting kill gas into gas phase catalytic polymerization reactor
JPH0625317A (en) * 1992-01-29 1994-02-01 Union Carbide Chem & Plast Technol Corp Method and apparatus for terminating reaction in vapor-phase polymerization reactor
JPH0719465A (en) * 1991-10-21 1995-01-20 Landis Gear Inter Syst Kk Cutoff valve mechanism in gas combustion equipment
JPH0995505A (en) * 1995-09-28 1997-04-08 Nippon Petrochem Co Ltd Method for stopping olefin polymerization reaction in emergency
JP2001098006A (en) * 1999-09-10 2001-04-10 Union Carbide Chem & Plast Technol Corp Method for feeding liquid comonomer into polymerization occurring in fluidized bed reactor
JP2002531600A (en) * 1998-11-30 2002-09-24 ビーピー ケミカルズ リミテッド Polymerization control method
JP2003513121A (en) * 1999-10-29 2003-04-08 ビーピー ケミカルズ リミテッド Gas phase polymerization method
JP2003130347A (en) * 2001-10-25 2003-05-08 Miura Co Ltd Control method for combustion device

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6072904A (en) * 1983-09-01 1985-04-25 モ−ビル　オイル　コ−ポレ−ション Method and device for injecting kill gas into gas phase catalytic polymerization reactor
JPH0719465A (en) * 1991-10-21 1995-01-20 Landis Gear Inter Syst Kk Cutoff valve mechanism in gas combustion equipment
JPH0625317A (en) * 1992-01-29 1994-02-01 Union Carbide Chem & Plast Technol Corp Method and apparatus for terminating reaction in vapor-phase polymerization reactor
JPH0995505A (en) * 1995-09-28 1997-04-08 Nippon Petrochem Co Ltd Method for stopping olefin polymerization reaction in emergency
JP2002531600A (en) * 1998-11-30 2002-09-24 ビーピー ケミカルズ リミテッド Polymerization control method
JP2001098006A (en) * 1999-09-10 2001-04-10 Union Carbide Chem & Plast Technol Corp Method for feeding liquid comonomer into polymerization occurring in fluidized bed reactor
JP2003513121A (en) * 1999-10-29 2003-04-08 ビーピー ケミカルズ リミテッド Gas phase polymerization method
JP2003130347A (en) * 2001-10-25 2003-05-08 Miura Co Ltd Control method for combustion device

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