JP4132799B2 - How to install the level gauge - Google Patents

How to install the level gauge Download PDF

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Publication number
JP4132799B2
JP4132799B2 JP2001369636A JP2001369636A JP4132799B2 JP 4132799 B2 JP4132799 B2 JP 4132799B2 JP 2001369636 A JP2001369636 A JP 2001369636A JP 2001369636 A JP2001369636 A JP 2001369636A JP 4132799 B2 JP4132799 B2 JP 4132799B2
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Prior art keywords
level gauge
liquid level
liquid
pressure side
side detection
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JP2003164703A (en
Inventor
修平 矢田
寧之 小川
潔 高橋
芳郎 鈴木
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Mitsubishi Chemical Corp
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Mitsubishi Chemical Corp
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Priority to JP2001369636A priority Critical patent/JP4132799B2/en
Application filed by Mitsubishi Chemical Corp filed Critical Mitsubishi Chemical Corp
Priority to CN200410069855.6A priority patent/CN1240662C/en
Priority to PCT/JP2002/012709 priority patent/WO2003048100A1/en
Priority to EP02786024A priority patent/EP1452518B1/en
Priority to ES10190825.9T priority patent/ES2547412T3/en
Priority to ES10190824.2T priority patent/ES2552378T3/en
Priority to BRPI0214697-5A priority patent/BR0214697B1/en
Priority to BRBR122012016826-2A priority patent/BR122012016826B1/en
Priority to BRBR122012016827-0A priority patent/BR122012016827B1/en
Priority to CN200410069856.0A priority patent/CN1260201C/en
Priority to EP10190826.7A priority patent/EP2311791B1/en
Priority to ES10190826T priority patent/ES2715315T3/en
Priority to CN200410069857.5A priority patent/CN1260202C/en
Priority to EP10190824.2A priority patent/EP2311789B1/en
Priority to CN200410069854.1A priority patent/CN1272304C/en
Priority to EP10190825.9A priority patent/EP2311790B1/en
Priority to AU2002354084A priority patent/AU2002354084A1/en
Priority to ES02786024T priority patent/ES2387564T3/en
Priority to CNB028243188A priority patent/CN100494155C/en
Priority to RU2004120291/04A priority patent/RU2300515C2/en
Priority to CN200410069853.7A priority patent/CN1247515C/en
Publication of JP2003164703A publication Critical patent/JP2003164703A/en
Priority to US10/859,221 priority patent/US7348455B2/en
Priority to US11/674,247 priority patent/US20070129571A1/en
Publication of JP4132799B2 publication Critical patent/JP4132799B2/en
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【０００１】
【発明の属する技術分野】
本発明は、易重合性化合物の製造設備に使用する液面計の設置方法に係り、更に詳しくは、特に前記液面計の高圧側検出部分の設置方法に関するもので、液面計の検出部が閉塞することなく設備の連続運転を可能とした液面計の設置方法である。
【０００２】
【従来の技術及びその課題】
従来、アクリル酸等を製造する設備において、当該機器本体に直結して液面計の高圧側検出部分を取り付けて圧力測定を行うのが一般的であった。
しかしながら、従来の液面計の設置方法では、易重合性化合物の製造時に使用される重合禁止剤、或いは発生した重合物が液面計の高圧側検出部分に供給されるため、ここに固形物が蓄積されて液面計に誤作動が発生することがあった。
従って、液面計によって連続して正確な測定ができず設備の長期安定運転が行えなかった。
【０００３】
【課題を解決するための手段】
本発明者は、易重合性化合物の製造設備に液面計を設置する方法であって、当該液面計の高圧側検出部分に測定液体の固形物が発生・蓄積するのを防止し、連続して正確な測定を行える液面径の設置方法を庭球するものである。即ち、本発明の要旨は、
（１）易重合性化合物の製造設備において、易重合性化合物を含有する液体を貯留する箇所へ差圧式液面計、ガラスゲージ型或いはチューブの直視式液面計、ディスプレッサー式液面計より選択された液面計を設置する際の液面計の設置方法であって、当該液面計の高圧側検出ラインと貯留した上記液体抜き出しラインとの接続角αは１０〜９０°で接続され、かつ液面計の高圧側検出ラインの管径Ｄ １ と液体の抜き出しラインの管径Ｄ ２ との寸法比Ｄ ２ ／Ｄ １ は１．３〜２０であるものを使用したことを特徴とする液面計の設置方法である。
（２） 液体抜き出しラインは、蒸留塔、蒸留塔の還流槽、分解反応塔、薄膜蒸発器、塔頂ガス冷却液槽、縦型貯蔵槽、横型貯槽又はタンクに接続されていることを特徴とする上記（１）記載の液面計の設置方法である。
（３） 液面計の高圧側検出ライン及び／又は低圧側検出ラインは、加熱或いは保温してあることを特徴とする上記１〜２記載の液面計の設置方法である。
（４）液面計の高圧側検出ラインび／又は低圧側検出ラインは、ガス及び／又は液体の注入口を接続していることを特徴とする上記１〜３記載の液面計の設置方法である。
（５） 易重合性化合物は、（メタ）アクリル酸又はそのエステルであることを特徴とする上記１〜４記載の液面計の設置方法である。
（６） 液面計で測定する液体は、（メタ）アクリル酸又はそのエステルを製造する場合に副生するアクリル酸２量体、β−（メタ）アクリロキシプロピオン酸エステル類、β−アルコキシプロピオン酸エステル類、β−ヒドロキシプロピオン酸、β−ヒドロキシプロピオン酸エステル類を少なくとも１種類以上含有するものであることを特徴とする上記５記載の液面計の設置方法である。
【０００４】
【発明の実施の形態】
本発明の液面計の設置方法を添付図面に基づいて説明する。
図１はアクリル酸の製造における（高沸物）分解反応塔及び塔頂ガス冷却液槽に本発明の液面計の設置方法を実施した設備全体図、図２は図１の（高沸物）分解反応塔に液面計を設置した部分拡大図及び図３は図１の塔頂ガス冷却液槽に液面計を設置した部分拡大図である。
【０００５】
先ず、図１によりアクリル酸の製造設備の概要を説明する。
Ａは（高沸物）分解反応塔であって、当該（高沸物）分解反応塔Ａには供給ライン１が取付けられている。
Ｂ1は塔底ポンプであって、当該塔底ポンプＢ1の流入側は（高沸物）分解反応塔Ａの塔底に取付けられている塔底液体抜き出しライン２に接続されており、またその流出側は分解残差物抜き出しライン４に接続されている。
Ｃは加熱用熱交換器であって、当該加熱用熱交換器の流入側は上記流出側は分解残差物抜き出しライン４から分岐した加熱用熱交換器供給ライン３に接続されており、またその流出側はラインによって（高沸物）分解反応塔Ａの下側壁に接続されている。
【０００６】
Ｄは塔頂ガス冷却熱交換器であって、当該塔頂ガス冷却熱交換器Ｄの流入側は（高沸物）分解反応塔Ａの塔頂に取付けられた分解後ガス回収ライン６に接続されており、その流出側はラインを介して塔頂ガス冷却液槽Ｅの流入側に接続されている。
また、塔頂ガス冷却液槽Ｅの流出側は槽底液体引き出しライン５及びポンプＢ2を介しての塔頂ガス冷却液抜き出しライン８に接続されており、塔頂ガス冷却液はこのライン８によって次の設備に移送される。
また塔頂ガス冷却液抜き出しライン８から分岐した冷却液戻しライン９は塔頂ガス冷却熱交換器Ｄの流入側に接続されている。
Ｆはベントガス冷却熱交換器であって、当該ベントガス冷却熱交換器Ｆの流入側はラインを介して塔頂ガス冷却液槽Ｅに接続されており、当該ベントガス冷却熱交換器Ｆに流入したベントガスは、冷却されガス中の有価物は回収された後、ベントガス抜き出しライン７に導かれる。
【０００７】
Ｈ1及びＨ2は差圧式液面計であって、この液面計Ｈ1及びＨ2の設置方法が本発明の主要素をなす装置である。
即ち、差圧式液面計Ｈ1の高圧側は高圧側検出ライン１１を介して塔底液体抜き出しライン２に接続されおり、また差圧式液面計Ｈ1の低圧側は低圧側検出ライン１２を介して（高沸物）分解反応塔Ａの下側壁に接続されている。
差圧式液面計Ｈ2の高圧側は高圧側検出ライン１３を介して槽底液体引き出しライン５に接続されており、差圧式液面計Ｈ2の低圧側は低圧側検出ライン１４を介して塔頂ガス冷却液槽Ｅの上面に接続されている。
【０００８】
次に上記差圧式液面計Ｈ1及びＨ2の設置方法の具体例を図２及び３に基づいて詳述する。
図２の（１）及び（２）において、Ａは（高沸物）分解反応塔であって、当該（高沸物）分解反応塔Ａの塔底に貯留された液体は、塔底に取付けられた塔底液体抜き出し短管２ａ及び塔底液体抜き出し導管２ｂで構成された塔底液体抜き出しライン２によって塔外に抜き出される。
Ｈ1は差圧式液面計であって、当該差圧式液面計Ｈ1の高圧側は高圧側検出短管１１ａ及び高圧側検出導管１１ｂで構成された高圧側検出ライン１１によって、塔底液体抜き出しライン２を構成する短管２ａ或いは導管２ｂのいずれかに接続されている。
【０００９】
この高圧側検出ライン１１と塔底液体抜き出しライン２との接続角αは５〜９０°好ましくは１０〜９０°が良い。
当該接続角が５°未満では実質上接続が困難であり、また接続角が９０°を超えた場合には液体中の固形物が高圧側検出ライン１１に流入しやすくなって好ましくない。
【００１０】
高圧側検出ラインの管径Ｄ1と液体抜き出しラインの管径Ｄ2との寸法比Ｄ2／Ｄ1は１〜２０、好ましくは１．３〜１０が良い。
当該Ｄ2／Ｄ1が１未満では液体中の固形物が高圧側検出ライン１１に流入しやすくなって好ましくなく、またＤ2／Ｄ1が２０を超えると液体面の検出が困難となる。
【００１１】
差圧式液面計Ｈ1の低圧側は低圧側検出導管１２ｂ及び低圧側検出短管１２ａで構成さてた低圧側検出ライン１２によって（高沸物）分解反応塔Ａの下側壁に接続されている。
なお、図２の（１）は塔底液体抜き出しライン２の垂直部に高圧側検出ライン１１を接続した例であり、図２の（２）は塔底液体抜き出しライン２の水平部に高圧側検出ライン１１を接続した例である。
【００１２】
図３の（１）及び（２）において、Ｅは塔頂ガス冷却液槽であって、当該塔頂ガス冷却液槽Ｅの槽底に貯留された液体は、槽底に取付けられた槽底液体抜き出し短管５ａ及び槽底液体抜き出し導管５ｂで構成された槽底液体抜き出しライン５によって槽外に抜き出される。
Ｈ2は差圧式液面計であって、当該差圧式液面計Ｈ2の高圧側は高圧側検出短管１３ａ及び高圧側検出導管１３ｂで構成された高圧側検出ライン１３によって、槽底液体抜き出しライン５を構成する短管５ａ或いは導管５ｂのいずれかに接続されている。
また、差圧式液面計Ｈ2の低圧側は低圧側検出導管１４ｂ及び低圧側検出短管１４ａで構成された低圧側検出ライン１４によって塔頂ガス冷却液槽Ｅの上面に接続されている。
【００１３】
この高圧側検出ライン１３と槽底液体抜き出しライン５との接続角α及び高圧側検出ライン１３の管径Ｄ1と槽底液体抜き出しライン５の管径Ｄ2との寸法比Ｄ2／Ｄ1は、上記図２の例で詳述した高圧側検出ライン１１と液体抜き出しライン２との関係を具備していれば良い。
なお、図３の（１）は槽底液体抜き出しライン５の垂直部に高圧側検出ライン１３を接続した例であり、図３の（２）は槽底液体抜き出しライン５の水平部に高圧側検出ライン１３を接続した例である。
【００１４】
上記液体抜き出しラインは蒸留塔、蒸留塔の還流槽、分解反応塔、薄膜蒸発器、塔頂ガス冷却液槽、縦型貯蔵槽、横型貯槽或いはタンク等の易重合性化合物を含有する溶液が貯留する箇所に接続し、これに液面計の高圧側検出ラインを取付けて液面を測定することができる。
【００１５】
また、本発明で使用される液面計は、差圧式液面計、ガラスゲージ型或いはチューブの直視式液面計、ディスプレッサー式液面計等を挙げることができる。
これらの液面計の高圧側検出ライン及び／又は低圧側検出ラインには、ガス及び／又は液体の注入口が接続されていることが好ましい。
何らかの運転変動で液体中の固形物が当該検出ラインに流入した場合に、固形物を速やかにガス及び／又は液体によって追い出すことができる。このガス及び／又は液体は、連続供給でも間欠供給でもよい。
これに使用されるガスは空気、窒素、二酸化炭素等がよく、液体はアクリル酸、アクリル酸エステル等の液体抜き出しラインに流れる液体と同一液体を使用することが好ましい。
更に、液面計の高圧側検出ライン及び／又は低圧側検出ラインに液体中の固形物が付着するのを防止するために、この部分を加熱或いは保温を施すとよい。
【００１６】
本発明の液面計の設置方法を使用して測定される易重合性化合物は、（メタ）アクリル酸又はそのエステル類を製造する際に有効である。
更に、液面計で測定する液体は、上記（メタ）アクリル酸又はそのエステルを製造する場合に副生するアクリル酸２量体、β−（メタ）アクリロキシプロピオン酸エステル類、β−アルコキシプロピオン酸エステル類、β−ヒドロキシプロピオン酸、β−ヒドロキシプロピオン酸エステル類を少なくとも１種類以上含有するものが特に有効である。
【００１７】
【実施例】
実施例１
図１及び２に示す設備で高沸液の分解反応を実施した。
高沸液の組成はアクリル酸ブチル２２重量％、β−ブトキシプロピオン酸ブチル６７重量％、アクルロキシプロピオン酸ブチル４重量％、β−ヒドロキシプロピオン酸ブチル２重量％、ハイドロキノン３重量％、メトキシキノン２重量％で、５８０ｋｇ／ｈで供給した。
【００１８】
分解反応触媒として硫酸１重量％水溶液を供給液に対して１０％重量比で供給し、反応圧力１００ｋＰａ、分解温度１９０℃、滞留時間１時間で分解反応を実施した結果、塔底よりアクリル酸ブチル１１．７重量％、β−ブトキシプロピオン酸ブチル６８．５重量％、アクリロキシプロピオン酸ブチル２重量％、β−ヒドロキシプロピオン酸ブチル０．３重量％、ハイドロキノン８．７重量％、メトキシキノン５．８重量％、ブタノール０．８重量％、硫酸２．９重量％で、２００．１ｋｇ／ｈが反応残差物として得られ、塔底より抜き出された。
【００１９】
分解反応塔塔底液は、塔底鏡部の最下位に取付けられた塔底液体抜き出しライン２より抜き出された。塔底の液面計Ｈ1は差圧式液面計で図２の（１）に示す配置で設置した。高圧側検出ライン１１と塔底液体抜き出しラインとの接続角αは４５°に設定した。
６ヶ月連続運転を行った後、運転を停止して液面計Ｈ1の高圧側検出ライン１１の高圧側検出短管１１ａ及び高圧側検出導管１１ｂを点検した。その点検の結果、何れにも蓄積物の付着がなかった。
【００２０】
比較例１
差圧式液面計Ｈ1の高圧側検出ライン１１を、分解反応塔Ａの下側壁に水平に接続した以外は実施例１と同一条件である。
２ヶ月運転後、塔底ポンプＢ1内で突然キャビテーションが発生した。急遽、分解反応塔Ａの運転を停止し、内部を点検した結果、分解反応塔Ａの塔底部に液が無く、液面計Ｈ1が誤指示していることが判明した。
液面計Ｈ1の高圧側検出ライン１１の高圧側検出短管１１ａ及び高圧側検出導管１１ｂを点検した結果、当該短管１１ａ及び導管１１ｂが閉塞していた。
【００２１】
比較例２
差圧式液面計Ｈ1の高圧側検出ライン１１を、分解反応塔Ａの下側壁に対して接続角αを４５°で接続した以外は実施例１と同一条件である。
３ヶ月運転後、塔底ポンプＢ1内で突然キャビテーションが発生した。急遽、分解反応塔Ａの運転を停止し、内部を点検した結果、分解反応塔Ａの塔底部に液が無く、液面計Ｈ1が誤指示していることが判明した。
液面計Ｈ1の高圧側検出ライン１１の高圧側検出短管１１ａ及び高圧側検出導管１１ｂを点検した結果、当該短管１１ａ及び導管１１ｂが閉塞していた。
【００２２】
実施２
薄膜型蒸発器を使用して、下記条件を満たす蒸発操作を実施した。
原料（粗アクリルモノマー）組成は、アクリル酸６６．６重量％、マレイン酸８．０、アクリル酸多量体２５．０重量％、ハイドロキノン０．５重量％、フェノチアジン０．５重量％を含む混合物を８５℃で３０００ｋｇ／ｈで供給した。
塔頂圧力９ｋＰａ、塔底圧力１０ｋＰａ、塔頂温度９５℃、塔底温度９８℃で運転に入り、塔頂からは供給量の５３％が抜き出され、純度８８重量％以上のアクリル酸が得られた。
塔底より、アクリル酸４１．１重量％、マレイン酸１０．９重量％、アクリル酸多量体４６．１６重量％、ハイドロキノン０．９２重量％、フェノチアジン０．９２重量％を含む混合物が抜き出された。
【００２３】
薄膜型蒸発器の塔底液は、塔底鏡部の最下位に取付けられた塔底液体抜き出しラインより抜き出された。塔底の液面計は差圧式液面計で図２の（１）に示す配置で設置した。高圧側検出ライン１１と塔底液体抜き出しラインとの接続角αは４５°に設定した。
６ヶ月連続運転を行った後、運転を停止して液面計の高圧側検出ライン１１の高圧側検出短管１１ａ及び高圧側検出導管１１ｂを点検した。その点検の結果、何れにも蓄積物の付着がなかった。
【００２４】
比較例３
差圧式液面計の高圧側検出ライン１１を、薄膜型蒸発器の下側壁に水平に接続した以外は実施例２と同一条件で蒸発操作を実施した。
１ヶ月運転後、塔底ポンプ内で突然キャビテーションが発生した。薄膜型蒸発器の運転を停止し、内部を点検した結果、薄膜型蒸発器に液が無く、液面計が誤指示していることが判明した。
液面計の高圧側検出ライン１１の高圧側検出短管１１ａ及び高圧側検出導管１１ｂを点検した結果、当該短管１１ａ及び導管１１ｂが閉塞していた。
【００２５】
【発明の効果】
易重合性化合物の製造設備中に、本発明の液面計設置方法を採用すれば、易重合性化合物の液体中に存在する固形物が液面計の高圧側検出ラインへの流入が無い。
従って、測定すべき液体によって液面計の検出部が閉塞しないので当該液面計によって正確に連続測定が可能となり、長期に亘って設備を運転することができる。
【図面の簡単な説明】
【図１】アクリル酸の製造における（高沸物）分解反応塔及び塔頂ガス冷却液槽に本発明の液面計の設置方法を実施した設備全体図
【図２】図１の（高沸物）分解反応塔に液面計を設置した部分拡大図。
【図３】図１の塔頂ガス冷却液槽に液面計を設置した部分拡大図。
【符号の説明】
Ａ…（高沸物）分解反応塔
Ｅ…塔頂ガス冷却液槽
Ｈ1及びＨ2…液面計
２…塔底液体抜き出しライン
２ａ…塔底液体抜き出し短管、 ２ｂ…塔底液体抜き出し導管
５…槽底液体抜き出しライン
５ａ…槽底液体抜き出し短管、 ５ｂ…槽底液体抜き出し導管
１１及び１３…高圧側検出ライン
１１ａ及び１３ａ…高圧側検出短管、 １１ｂ及び１３ｂ…高圧側検出導管
１２及び１４…低圧側検出ライン
１２ａ及び１４ａ…低圧側検出短管、 １２ｂ及び１４ａ…低圧側検出導管
α…高圧側検出ラインと液体抜き出しラインとの接続角[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for installing a level gauge used in a production facility for an easily polymerizable compound, and more particularly, particularly to a method for installing a high-pressure side detection portion of the level gauge. This is a liquid level gauge installation method that allows continuous operation of equipment without obstruction.
[0002]
[Prior art and problems]
Conventionally, in facilities for manufacturing acrylic acid or the like, it is common to perform pressure measurement by directly connecting to the device body and attaching a high-pressure side detection portion of a liquid level gauge.
However, in the conventional level gauge installation method, the polymerization inhibitor used in the production of the easily polymerizable compound or the generated polymer is supplied to the high pressure side detection part of the level gauge, so that the solid substance is used here. May accumulate, causing malfunctions in the level gauge.
Therefore, continuous accurate measurement could not be performed with the liquid level gauge, and long-term stable operation of the equipment could not be performed.
[0003]
[Means for Solving the Problems]
The present inventor is a method of installing a liquid level gauge in a production facility of an easily polymerizable compound, preventing the generation and accumulation of solids of the measurement liquid in the high pressure side detection portion of the liquid level gauge, Thus, a method of setting the liquid surface diameter that can perform accurate measurement is used. That is, the gist of the present invention is as follows.
(1) In a production facility for an easily polymerizable compound, to a location for storing a liquid containing the easily polymerizable compound, from a differential pressure type liquid level gauge, a glass gauge type or tube direct-view type liquid level gauge, and a displacer type liquid level gauge A method of installing a liquid level gauge when installing a selected liquid level gauge, wherein a connection angle α between the high pressure side detection line of the liquid level gauge and the stored liquid extraction line is 10 to 90 °. And the dimensional ratio D 2 / D 1 between the pipe diameter D 1 of the high-pressure side detection line of the liquid level gauge and the pipe diameter D 2 of the liquid extraction line is 1.3 to 20 It is the installation method of the liquid level gauge.
( 2 ) The liquid extraction line is connected to a distillation tower, a reflux tank of the distillation tower, a decomposition reaction tower, a thin film evaporator, a tower top gas cooling liquid tank, a vertical storage tank, a horizontal storage tank or a tank. It is the installation method of the liquid level meter as described in said (1).
(3) high voltage side detection line and / or the low pressure side detection line of the liquid level meter is a method of installing the 1-2 wherein the liquid level meter, characterized in that are heated or kept warm.
( 4 ) The method for installing a liquid level gauge according to any one of the above items 1 to 3, wherein the high pressure side detection line and / or the low pressure side detection line of the liquid level gauge is connected to a gas and / or liquid inlet. It is.
(5) easily polymerizable compound is a method of installing the 1-4 wherein the liquid level meter, which is a (meth) acrylic acid or its ester.
( 6 ) The liquid to be measured by a liquid level meter is acrylic acid dimer, β- (meth) acryloxypropionic acid esters, β-alkoxypropion, which are by-produced when (meth) acrylic acid or its ester is produced. 6. The method for installing a liquid level meter as described in 5 above, which comprises at least one acid ester, β-hydroxypropionic acid, and β-hydroxypropionic acid ester.
[0004]
DETAILED DESCRIPTION OF THE INVENTION
A method for installing the level gauge of the present invention will be described with reference to the accompanying drawings.
FIG. 1 is an overall view of the facility in which the method for installing the liquid level gauge of the present invention is installed in the (high boiling point) decomposition reaction tower and the tower top gas cooling liquid tank in the production of acrylic acid, and FIG. FIG. 3 is a partially enlarged view in which a liquid level gauge is installed in the decomposition reaction tower and FIG. 3 is a partial enlarged view in which a liquid level gauge is installed in the tower top gas cooling liquid tank of FIG.
[0005]
First, an outline of an acrylic acid production facility will be described with reference to FIG.
A is a (high boiling point) decomposition reaction tower, and a supply line 1 is attached to the (high boiling point) decomposition reaction tower A.
B 1 is a column bottom pump, and the inflow side of the column bottom pump B 1 is connected to a column bottom liquid extraction line 2 attached to the column bottom of the (high boiling point) decomposition reaction column A; The outflow side is connected to a decomposition residue extraction line 4.
C is a heating heat exchanger, the inflow side of the heating heat exchanger is connected to the heating heat exchanger supply line 3 branched from the decomposition residue extraction line 4 on the outflow side, and The outflow side is connected to the lower side wall of the decomposition reaction tower A by a line (high boiling matter).
[0006]
D is a tower top gas cooling heat exchanger, and the inflow side of the tower top gas cooling heat exchanger D is connected to a post-cracking gas recovery line 6 attached to the top of the (high boiling point) cracking reaction tower A. The outflow side is connected to the inflow side of the tower top gas coolant tank E through a line.
The outflow side of the tower top gas coolant tank E is connected to the tower bottom liquid draw line 5 and the tower top gas coolant draw line 8 via the pump B 2. Is transferred to the next facility.
A coolant return line 9 branched from the tower top gas coolant extraction line 8 is connected to the inflow side of the tower top gas cooling heat exchanger D.
F is a vent gas cooling heat exchanger, the inflow side of the vent gas cooling heat exchanger F is connected to the tower top gas cooling liquid tank E via a line, and the vent gas flowing into the vent gas cooling heat exchanger F Is cooled and valuables in the gas are recovered and then led to a vent gas extraction line 7.
[0007]
H 1 and H 2 are differential pressure type liquid level gauges, and the installation method of the liquid level gauges H 1 and H 2 is an apparatus that constitutes the main element of the present invention.
That is, the high pressure side of the differential pressure type liquid level gauge H 1 is connected to the tower bottom liquid extraction line 2 via the high pressure side detection line 11, and the low pressure side of the differential pressure type liquid level gauge H 1 is connected to the low pressure side detection line 12. (High boiling point) through the bottom wall of the decomposition reaction column A.
The high pressure side of the differential pressure type liquid level gauge H 2 is connected to the tank bottom liquid drawing line 5 via the high pressure side detection line 13, and the low pressure side of the differential pressure type liquid level gauge H 2 is connected to the low pressure side detection line 14. The top gas cooling liquid tank E is connected to the upper surface.
[0008]
Next, a specific example of the installation method of the differential pressure type liquid level gauges H 1 and H 2 will be described in detail with reference to FIGS.
In (1) and (2) of FIG. 2, A is a (high boiling point) decomposition reaction column, and the liquid stored in the bottom of the (high boiling point) decomposition reaction column A is attached to the bottom of the column. The column bottom liquid extraction short pipe 2a and the column bottom liquid extraction conduit 2b are extracted to the outside of the column by a column bottom liquid extraction line 2.
H 1 is a differential pressure type liquid level gauge, and the high pressure side of the differential pressure type liquid level gauge H 1 has a column bottom liquid by a high pressure side detection line 11 constituted by a high pressure side detection short tube 11a and a high pressure side detection conduit 11b. It is connected to either the short pipe 2a or the conduit 2b constituting the extraction line 2.
[0009]
The connection angle α between the high-pressure side detection line 11 and the column bottom liquid extraction line 2 is 5 to 90 °, preferably 10 to 90 °.
If the connection angle is less than 5 °, connection is practically difficult, and if the connection angle exceeds 90 °, solids in the liquid easily flow into the high-pressure side detection line 11, which is not preferable.
[0010]
The dimensional ratio D 2 / D 1 between the pipe diameter D 1 of the high-pressure side detection line and the pipe diameter D 2 of the liquid extraction line is 1 to 20, preferably 1.3 to 10.
If D 2 / D 1 is less than 1, solids in the liquid are liable to flow into the high-pressure side detection line 11, and if D 2 / D 1 exceeds 20, it becomes difficult to detect the liquid level.
[0011]
The low pressure side of the differential pressure type liquid level gauge H 1 is connected to the lower side wall of the decomposition reaction tower A (high boiling point) by a low pressure side detection line 12 constituted by a low pressure side detection conduit 12b and a low pressure side detection short tube 12a. .
2 is an example in which a high-pressure side detection line 11 is connected to a vertical portion of the column bottom liquid extraction line 2, and FIG. 2 (2) is a high-pressure side in the horizontal portion of the column bottom liquid extraction line 2. This is an example in which the detection line 11 is connected.
[0012]
In (1) and (2) of FIG. 3, E is a tower top gas cooling liquid tank, and the liquid stored in the tank bottom of the tower top gas cooling liquid tank E is the tank bottom attached to the tank bottom. The liquid is extracted out of the tank by a tank bottom liquid extraction line 5 including a liquid extraction short pipe 5a and a tank bottom liquid extraction conduit 5b.
H 2 is a differential pressure type liquid level gauge, and the high pressure side of the differential pressure type liquid level gauge H 2 is a tank bottom liquid by a high pressure side detection line 13 comprising a high pressure side detection short tube 13a and a high pressure side detection conduit 13b. It is connected to either the short pipe 5a or the conduit 5b constituting the extraction line 5.
Further, the low-pressure side of the differential pressure type liquid level meter H 2 are connected by the low-pressure side detection line 14 composed of a low voltage side detection conduit 14b and the low pressure side of the detected short tube 14a on the upper surface of the overhead gas cooling liquid tank E.
[0013]
The connection angle α between the high pressure side detection line 13 and the tank bottom liquid extraction line 5 and the dimensional ratio D 2 / D 1 between the pipe diameter D 1 of the high pressure side detection line 13 and the pipe diameter D 2 of the tank bottom liquid extraction line 5. Need only have the relationship between the high-pressure side detection line 11 and the liquid extraction line 2 described in detail in the example of FIG.
3 is an example in which the high pressure side detection line 13 is connected to the vertical portion of the tank bottom liquid extraction line 5, and FIG. 3 (2) is the high pressure side to the horizontal portion of the tank bottom liquid extraction line 5. This is an example in which the detection line 13 is connected.
[0014]
The liquid extraction line stores a solution containing an easily polymerizable compound such as a distillation tower, a reflux tower of a distillation tower, a decomposition reaction tower, a thin film evaporator, a tower top gas cooling liquid tank, a vertical storage tank, a horizontal storage tank or a tank. The level of the liquid can be measured by connecting to a high pressure side detection line of the liquid level gauge.
[0015]
Examples of the liquid level gauge used in the present invention include a differential pressure type liquid level gauge, a glass gauge type or tube direct-view type liquid level gauge, and a displacer type liquid level gauge.
A gas and / or liquid inlet is preferably connected to the high-pressure side detection line and / or the low-pressure side detection line of these liquid level gauges.
When solid matter in the liquid flows into the detection line due to some operational fluctuation, the solid matter can be quickly expelled by the gas and / or liquid. The gas and / or liquid may be supplied continuously or intermittently.
The gas used for this is air, nitrogen, carbon dioxide or the like, and the liquid is preferably the same liquid as the liquid flowing in the liquid extraction line such as acrylic acid or acrylic ester.
Furthermore, in order to prevent the solid matter in the liquid from adhering to the high-pressure side detection line and / or the low-pressure side detection line of the liquid level gauge, this portion may be heated or kept warm.
[0016]
The easily polymerizable compound measured using the method for installing the liquid level gauge of the present invention is effective in producing (meth) acrylic acid or esters thereof.
Furthermore, the liquid to be measured with a liquid level meter is acrylic acid dimer, β- (meth) acryloxypropionic acid esters, β-alkoxypropion, which are by-produced when the (meth) acrylic acid or its ester is produced. Those containing at least one acid ester, β-hydroxypropionic acid, or β-hydroxypropionic acid ester are particularly effective.
[0017]
【Example】
Example 1
The high boiling liquid decomposition reaction was carried out with the equipment shown in FIGS.
The composition of the high-boiling liquid is 22% by weight of butyl acrylate, 67% by weight of butyl β-butoxypropionate, 4% by weight of butyloxypropionate, 2% by weight of butyl β-hydroxypropionate, 3% by weight of hydroquinone, 2 methoxyquinone It was supplied at 580 kg / h in weight%.
[0018]
As a decomposition reaction catalyst, a 1% by weight sulfuric acid aqueous solution was supplied at a 10% weight ratio with respect to the feed solution, and the decomposition reaction was carried out at a reaction pressure of 100 kPa, a decomposition temperature of 190 ° C., and a residence time of 1 hour. 11.7 wt%, butyl β-butoxypropionate 68.5 wt%, butyl acryloxypropionate 2 wt%, butyl β-hydroxypropionate 0.3 wt%, hydroquinone 8.7 wt%, methoxyquinone 5. 200.1 kg / h was obtained as a reaction residue at 8 wt%, butanol 0.8 wt% and sulfuric acid 2.9 wt%, and was extracted from the bottom of the column.
[0019]
The cracking reaction column bottom liquid was extracted from a column bottom liquid extraction line 2 attached at the bottom of the column bottom mirror. The liquid level gauge H 1 at the bottom of the tower is a differential pressure type liquid level gauge and is installed in the arrangement shown in FIG. The connection angle α between the high pressure side detection line 11 and the column bottom liquid extraction line was set to 45 °.
After 6 months continuous operation was inspected high voltage side detection short pipe 11a and the high voltage side detection conduit 11b of the high-pressure side detection line 11 of the liquid level meter H 1 to stop the operation. As a result of the inspection, there was no deposit on any of them.
[0020]
Comparative Example 1
The conditions are the same as in Example 1 except that the high pressure side detection line 11 of the differential pressure type liquid level gauge H 1 is connected horizontally to the lower side wall of the decomposition reaction tower A.
After two months of operation, suddenly cavitation in the tower bottom pump B 1 it has occurred. Suddenly, the operation of the decomposition reaction tower A was stopped and the inside was inspected. As a result, it was found that there was no liquid at the bottom of the decomposition reaction tower A, and the liquid level gauge H 1 indicated erroneously.
High voltage side detection short pipe 11a and a result of the check the high voltage side detection conduit 11b of the high-pressure side detection line 11 of the liquid level meter H 1, the short pipe 11a and conduit 11b were closed.
[0021]
Comparative Example 2
The conditions are the same as in Example 1 except that the high pressure side detection line 11 of the differential pressure type liquid level gauge H 1 is connected to the lower side wall of the decomposition reaction tower A at a connection angle α of 45 °.
After three months of operation, suddenly cavitation in the tower bottom pump B 1 it has occurred. Suddenly, the operation of the decomposition reaction tower A was stopped and the inside was inspected. As a result, it was found that there was no liquid at the bottom of the decomposition reaction tower A, and the liquid level gauge H 1 indicated erroneously.
High voltage side detection short pipe 11a and a result of the check the high voltage side detection conduit 11b of the high-pressure side detection line 11 of the liquid level meter H 1, the short pipe 11a and conduit 11b were closed.
[0022]
Implementation 2
Using a thin film evaporator, an evaporation operation satisfying the following conditions was performed.
The composition of the raw material (crude acrylic monomer) is a mixture containing 66.6% by weight of acrylic acid, 8.0% of maleic acid, 25.0% by weight of acrylic acid multimer, 0.5% by weight of hydroquinone, and 0.5% by weight of phenothiazine. It was supplied at 3000 kg / h at 85 ° C.
The operation was started at a tower top pressure of 9 kPa, a tower bottom pressure of 10 kPa, a tower top temperature of 95 ° C., and a tower bottom temperature of 98 ° C., and 53% of the supplied amount was extracted from the tower top to obtain acrylic acid having a purity of 88% by weight or more. It was.
A mixture containing 41.1 wt% acrylic acid, 10.9 wt% maleic acid, 46.16 wt% acrylic acid multimer, 0.92 wt% hydroquinone, and 0.92 wt% phenothiazine was extracted from the bottom of the column. It was.
[0023]
The bottom liquid of the thin film evaporator was extracted from the bottom liquid extraction line attached to the bottom of the bottom mirror part. The liquid level gauge at the bottom of the tower was a differential pressure type liquid level gauge and was installed in the arrangement shown in FIG. The connection angle α between the high pressure side detection line 11 and the column bottom liquid extraction line was set to 45 °.
After 6 months of continuous operation, the operation was stopped and the high-pressure side detection short tube 11a and the high-pressure side detection conduit 11b of the high-pressure side detection line 11 of the level gauge were inspected. As a result of the inspection, there was no deposit on any of them.
[0024]
Comparative Example 3
The evaporation operation was performed under the same conditions as in Example 2 except that the high pressure side detection line 11 of the differential pressure type liquid level gauge was connected horizontally to the lower wall of the thin film evaporator.
After one month of operation, cavitation suddenly occurred in the bottom pump. As a result of stopping the operation of the thin film type evaporator and inspecting the inside, it was found that there was no liquid in the thin film type evaporator and the liquid level gauge indicated erroneously.
As a result of inspecting the high pressure side detection short tube 11a and the high pressure side detection conduit 11b of the high pressure side detection line 11 of the liquid level gauge, the short tube 11a and the conduit 11b were blocked.
[0025]
【The invention's effect】
If the liquid level gauge installation method of the present invention is adopted in the production facility of the easily polymerizable compound, the solid substance present in the liquid of the easily polymerizable compound does not flow into the high pressure side detection line of the liquid level gauge.
Therefore, since the detection part of the liquid level gauge is not blocked by the liquid to be measured, accurate continuous measurement is possible with the liquid level gauge, and the equipment can be operated for a long time.
[Brief description of the drawings]
FIG. 1 is an overall view of equipment in which the method for installing a liquid level gauge of the present invention is applied to a (high boiling point) decomposition reaction tower and an overhead gas cooling liquid tank in the production of acrylic acid. Article) Partial enlarged view in which a liquid level gauge is installed in the decomposition reaction tower.
FIG. 3 is a partially enlarged view in which a liquid level gauge is installed in the tower top gas cooling liquid tank of FIG. 1;
[Explanation of symbols]
A ... (high boiling point) decomposition reaction tower E ... tower top gas cooling liquid tanks H 1 and H 2 ... level gauge 2 ... tower bottom liquid extraction line 2a ... tower bottom liquid extraction short pipe, 2b ... tower bottom liquid extraction conduit DESCRIPTION OF SYMBOLS 5 ... Tank bottom liquid extraction line 5a ... Tank bottom liquid extraction short pipe, 5b ... Tank bottom liquid extraction conduits 11 and 13 ... High pressure side detection line 11a and 13a ... High pressure side detection short pipe, 11b and 13b ... High pressure side detection conduit 12 And 14 ... Low-pressure side detection lines 12a and 14a ... Low-pressure side detection short pipes, 12b and 14a ... Low-pressure side detection conduit α ... Connection angle between the high-pressure side detection line and the liquid extraction line

Claims (6)

易重合性化合物の製造設備において、易重合性化合物を含有する液体を貯留する箇所へ差圧式液面計、ガラスゲージ型或いはチューブの直視式液面計、ディスプレッサー式液面計より選択された液面計を設置する際の液面計の設置方法であって、当該液面計の高圧側検出ラインと貯留した上記液体抜き出しラインとの接続角αは１０〜９０°で接続され、かつ液面計の高圧側検出ラインの管径Ｄ １ と液体抜き出しラインの管径Ｄ ２ との寸法比Ｄ ２ ／Ｄ １ は１．３〜２０であるものを使用したことを特徴とする液面計の設置方法。In a production facility for easily polymerizable compounds, selected from a differential pressure type liquid level gauge, a glass gauge type or a tube direct-view type liquid level gauge, and a displacer type liquid level gauge to a location for storing a liquid containing the easily polymerizable compound . A method for installing a level gauge when installing a level gauge, wherein the connection angle α between the high-pressure side detection line of the level gauge and the stored liquid extraction line is 10 to 90 °, and A liquid level gauge having a dimensional ratio D 2 / D 1 of 1.3 to 20 between the pipe diameter D 1 of the high pressure side detection line of the surface gauge and the pipe diameter D 2 of the liquid extraction line Installation method. 液体抜き出しラインは、蒸留塔、蒸留塔の還流槽、分解反応塔、薄膜蒸発器、塔頂ガス冷却液槽、縦型貯蔵槽、横型貯槽又はタンクに接続されていることを特徴とする請求項１記載の液面計の設置方法。 The liquid extraction line is connected to a distillation tower, a reflux tank of the distillation tower, a decomposition reaction tower, a thin film evaporator, a tower top gas cooling liquid tank, a vertical storage tank, a horizontal storage tank or a tank. The installation method of the liquid level gauge of 1. 液面計の高圧側検出ライン及び／又は低圧側検出ラインは、加熱或いは保温してあることを特徴とする請求項１〜２記載の液面計の設置方法。The method for installing a liquid level gauge according to claim 1 or 2 , wherein the high pressure side detection line and / or the low pressure side detection line of the liquid level gauge is heated or kept warm. 液面計の高圧側検出ラインび／又は低圧側検出ラインは、ガス及び／又は液体の注入口を接続していることを特徴とする請求項１〜３記載の液面計の設置方法。High voltage side detection line beauty / or low pressure side detection line of the liquid level gauge, the installation method according to claim 1-3, wherein the liquid level meter, characterized by connecting the gas and / or inlet of liquid. 易重合性化合物は、（メタ）アクリル酸又はそのエステルであることを特徴とする請求項１〜４記載の液面計の設置方法。Easily polymerizable compound is (meth) Installation according to claim 1-4, wherein the liquid level meter, which is a acrylic acid or its ester. 液面計で測定する液体は、（メタ）アクリル酸又はそのエステルを製造する場合に副生するアクリル酸２量体、β−（メタ）アクリロキシプロピオン酸エステル類、β−アルコキシプロピオン酸エステル類、β−ヒドロキシプロピオン酸、β−ヒドロキシプロピオン酸エステル類を少なくとも１種類以上含有するものであることを特徴とする請求項５記載の液面計の設置方法。The liquid to be measured with a level gauge is acrylic acid dimer, β- (meth) acryloxypropionic acid esters, β-alkoxypropionic acid esters produced as a by-product when producing (meth) acrylic acid or its ester. 6. The method for installing a liquid level gauge according to claim 5 , comprising at least one of β-hydroxypropionic acid and β-hydroxypropionic acid esters.
JP2001369636A 2001-12-04 2001-12-04 How to install the level gauge Expired - Lifetime JP4132799B2 (en)

Priority Applications (23)

Application Number Priority Date Filing Date Title
JP2001369636A JP4132799B2 (en) 2001-12-04 2001-12-04 How to install the level gauge
CN200410069853.7A CN1247515C (en) 2001-12-04 2002-12-04 Process for producing (meth)acrylic acid compound
EP10190824.2A EP2311789B1 (en) 2001-12-04 2002-12-04 Process for producing (meth)acrylic acids
ES10190825.9T ES2547412T3 (en) 2001-12-04 2002-12-04 Production process of (meth) acrylic acids
ES10190824.2T ES2552378T3 (en) 2001-12-04 2002-12-04 Production process of (meth) acrylic acids
BRPI0214697-5A BR0214697B1 (en) 2001-12-04 2002-12-04 process for the production of (meth) acrylic acids.
BRBR122012016826-2A BR122012016826B1 (en) 2001-12-04 2002-12-04 Method for decomposing by-product formed during the production of (meth) acrylic acids
BRBR122012016827-0A BR122012016827B1 (en) 2001-12-04 2002-12-04 Method for installing liquid level meter
CN200410069856.0A CN1260201C (en) 2001-12-04 2002-12-04 Process for producing (meth)acrylic acid compound
EP10190826.7A EP2311791B1 (en) 2001-12-04 2002-12-04 Process for producing (meth)acrylic acids
ES10190826T ES2715315T3 (en) 2001-12-04 2002-12-04 Procedure to produce (meth) acrylic acids
CN200410069857.5A CN1260202C (en) 2001-12-04 2002-12-04 Process for producing (meth) acrylic acids
CN200410069855.6A CN1240662C (en) 2001-12-04 2002-12-04 Process for producing (meth)acrylic acid compound
EP02786024A EP1452518B1 (en) 2001-12-04 2002-12-04 Process for producing (meth)acrylic acid compounds
CN200410069854.1A CN1272304C (en) 2001-12-04 2002-12-04 Process for producing (meth)acrylic acid compound
AU2002354084A AU2002354084A1 (en) 2001-12-04 2002-12-04 Process for producing (meth) acrylic acid compound
ES02786024T ES2387564T3 (en) 2001-12-04 2002-12-04 Production process of (meth) acrylic acid compounds
CNB028243188A CN100494155C (en) 2001-12-04 2002-12-04 Process for producing (meth) acrylic acids
RU2004120291/04A RU2300515C2 (en) 2001-12-04 2002-12-04 Method of production of methacrylic acids by catalytic oxidation of propylene or isobutylene (versions), method of decomposition of by-product (versions) and plant for realization of this method
PCT/JP2002/012709 WO2003048100A1 (en) 2001-12-04 2002-12-04 Process for producing (meth)acrylic acid compound
EP10190825.9A EP2311790B1 (en) 2001-12-04 2002-12-04 Process for producing (meth)acrylic acids
US10/859,221 US7348455B2 (en) 2001-12-04 2004-06-03 Process for producing (meth)acrylic acids
US11/674,247 US20070129571A1 (en) 2001-12-04 2007-02-13 Process for producing (meth)acrylic acids

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EP1740283A4 (en) * 2003-12-02 2008-03-12 Sylvan Source Inc Fully automated water processing control system
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