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JP4069645B2 - How to remove dirt from heat exchangers - Google Patents
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JP4069645B2 - How to remove dirt from heat exchangers - Google Patents

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Publication number
JP4069645B2
JP4069645B2 JP2002061611A JP2002061611A JP4069645B2 JP 4069645 B2 JP4069645 B2 JP 4069645B2 JP 2002061611 A JP2002061611 A JP 2002061611A JP 2002061611 A JP2002061611 A JP 2002061611A JP 4069645 B2 JP4069645 B2 JP 4069645B2
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Japan
Prior art keywords
heat exchanger
heavy
dirt
liquid containing
steam
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JP2002061611A
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JP2003262495A (en
Inventor
守 清野
重文 徳増
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Sumitomo Chemical Co Ltd
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Sumitomo Chemical Co Ltd
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Description

【0001】
【発明の属する技術分野】
本発明は、目的物と重質物を含む液から目的物を得る工程における、加熱型熱交換器の内部汚れを、該熱交換器の運転を継続しつつ除去し、長期に亘り熱交換能力を維持する方法に関する。
【0002】
【従来の技術】
加熱型熱交換器は、目的物と重質物を含む液から目的物を分離精製する蒸留操作等に用いられている。この場合、重質物の汚れ成分が熱交換器内部に付着し、熱交換器の伝熱能力が低下するために、しばしば熱交換器の操業を停止して内部汚れを除去する必要性があった。
【0003】
汚れを除去する方法としては、熱交換器の操業を一時停止して熱交換器の内容物を抜出して機器開放を行った後、熱交換器の内部を高圧水による洗浄、バフ研磨、メカクリーン研磨等を行って汚れを除去する方法をあげることができる。このような方法では、熱交換器の予備機への切り替え、機器の開放作業および汚れの除去作業等、多大の労力を要する他、作業の安全性、切り替えに伴うプラント操業上の安定性確保等の問題を抱えている。
【0004】
一方、熱交換器の停止を伴うが、機器の開放を行わずに熱交換器の内部を温水洗浄、アルカリ洗浄等の薬液洗浄を行う比較的作業量の少ない方法もある。しかし、この方法では汚れ除去が十分に行われず、操業再開後の熱交換能力の低下が早く、洗浄作業を頻繁に繰り返す必要性があるなどの問題があった。
【0005】
【発明が解決しようとする課題】
かかる現状において、本発明は加熱型熱交換器の運転停止等を伴うことなく、運転を継続しながら、熱交換能力を長期に亘って維持することができる、熱交換器の汚れ除去方法を提供することを目的とする。
【0006】
【課題を解決するための手段】
すなわち、本発明は、目的物と重質物を含む液であって、芳香族ペルオキシド類を分解することにより得られるジヒドロキシベンゼン類と重質物を含む液から目的物を蒸留により分離精製する化学プラントの工程において、前記目的物と重質物を含む液を加熱蒸発させる熱交換器内部に付着する前記重質物に基づく汚れを、熱交換器の運転を継続しつつ、熱交換器の内部にスチームを導入して汚れを除去する熱交換器の汚れ除去方法であって、熱交換器が縦型で、管が直管の多管式加熱型熱交換器熱交換器であり、ジヒドロキシベンゼン類と重質物を含む液は熱交換器内を下から上向きに通過し、スチームは熱交換器下部に設けられたノズルから該液中に導入される熱交換器の汚れ除去方法である。
【0007】
【発明の実施の形態】
本発明において、目的物と重質物を含む液とは、芳香族ペルオキシド類を分解することにより得られるジヒドロキシベンゼン類と重質物を含む液であって、重質物とは、目的物を分離精製する際に蒸留塔の底部等に設けられた加熱型熱交換器の内部に付着して、熱交換器の内部の汚れとなり、熱交換能力を阻害するものを言う。
【0008】
具体的には、分解工程における有機物質の重合物などの副反応物質、分解工程において用いた酸触媒を中和する際に生じる塩などの無機物を含めたものである。例えば、例示したレゾルシンプロセスの場合は、レゾルシン重合体、レゾルシンとヒドロキシメチルスチレン付加物等であり、その他酸触媒の中和操作等に伴って発生するNa2SO4等の無機物が重質物として熱交換器の汚れ成分となる。
【0009】
かかる目的物と重質物を含む液を、加熱型熱交換器によって加熱すると重質物が短期間に熱交換器内部に付着し、熱交換能力が低下して、熱交換器所定の能力を発揮できず、エネルギー損失のみではなく生産量の減少を招くなどプラント全体の安定的な操業にも支障をきたす。
【0010】
熱交換器内部の汚れを除去するには、前記した如く、熱交換器を停止し、熱交換器の予備機への切り替え、機器の開放作業および汚れの除去作業等を行う等、多大の労力と化学プラントの操業自体に影響を及ぼす。そこで該工程にスチームを熱交換器に導入することにより、熱交換器を停止することなく運転継続したまま、熱交換器内部の汚れを除去することができ、熱交換能力を回復することができる。熱交換器への導入は、熱交換器下部にノズルを設けて導入し、熱交換器内部をスチームが通過できるようにするスチームはその工程あるいは後の工程で除去することができ、製品品質に影響を及ぼさない。
【0011】
本発明の一つの態様として、芳香族ペルオキシドを酸分解することにより得られるジヒドロキシベンゼン類と重質物を含む液からジヒドロキシベンゼン類を留出させる際に使用する多管式加熱型熱交換器が例示される。
【0012】
例えば、レゾルシンの製造プロセスにおいて、1,3−ジイソプロピルベンゼンを酸化して1,3−ジヒドロキシイソプロピルベンゼン等を含む液が得られ、この液から抽出、濃縮、分解等の工程を経てレゾルシン、アセトン、重質物を含むが得られる。この液からアセトン等の軽沸分を除去したレゾルシンおよび重質物を含む液からレゾルシンを精製回収する際に、縦型の多管式加熱型熱交換器で加熱、蒸留を行って重質物を除去する。
【0013】
重質物には、レゾルシン重合体、レゾルシンとヒドロキシメチルスチレン付加物等や、その他酸触媒の中和操作等に伴って発生するNa2SO4等の無機物が含まれることがある。
【0014】
重質物に基づく汚れが付着し、総括伝熱係数(以下Uと略す)が低下した多管式加熱型熱交換器の運転を停止して、1,300kg/cm2の高圧水で熱交換器の汚れを洗浄除去した後、熱交換器の運転を再開すると、当初のUは徐々に低下し、200日運転後は約1/3にまで低下する。この状態でUがさらに低下すると、プロセス全体の運転継続が困難となる。そこで熱交換器の運転を継続しながら、熱交換器下部のノズルから、該プロセスの後工程や目的製品であるレゾルシンの品質等に悪影響を及ぼさないスチームを導入しつつ運転を継続したところ、Uの低下はスチーム導入後すぐになくなり逆に次第にUが回復し始めた。14日後にはスチーム導入前の約2倍にまで回復し、プロセスの運転は順調に行われた。スチーム停止後は、回復したUは少なくとも約60日は回復した状態で持続するため、Uの状況を監視しつつスチームを必要に応じて熱交換器の下部ノズルから導入するだけでUを回復することが出来る。
【0015】
かかる方法によると、熱交換器の停止、予備機への切り替え、機器の開放作業および汚れの除去作業等多大の労力が不要であるばかりでなく、これらの作業に伴う作業の安全性、熱交換器切り替えに伴うプラント操業上の安定性の確保等が可能となる。
【0016】
【実施例】
実施例1
汚れが付着しUが約60Kcal/m2・Hr・degに低下した縦型の多管式加熱型熱交換器の運転を停止し、1,300kg/cm2の高圧水で熱交換器の汚れを洗浄除去した後、熱交換器の運転を再開した。運転再開直後のUは180Kcal/m2・Hr・deg.であった。運転継続と共にUは徐々に低下し、200日運転後は、Uは60Kcal/m2・Hr・deg.に低下した。そこで熱交換器の運転を継続しながら、熱交換器の底部に1kg/cm2(120℃)のスチームを16Kg/Hrで導入し運転を継続した。スチームの導入後は、Uの低下がなくなり次第にUが回復し始め、14日後には120Kcal/m2・Hr・deg.に回復した。スチームは14日目に停止したが、回復したUはその後約60日は持続することを確認できた。
【0017】
比較例1
汚れが付着しUが約60Kcal/m2・Hr・deg.に低下した縦型の多管式加熱型熱交換器の運転を停止し、100℃温水で洗浄を行い汚れの除去を行った。運転再開後Uは80Kcal/m2・Hr・deg.に回復していたが、約60日で60Kcal/m2・Hr・deg.にまで低下し、運転継続が出来なくなった。数回同様の運転停止、温水洗浄の操作を繰り返したが、いずれも60日以内でUは60Kcal/m2・Hr・deg.に低下し、安定的な連続運転はできなかった。
【0018】
【発明の効果】
本発明により、重質物に基づく汚れ成分が内部に付着して熱交換能力が低下する加熱型熱交換器の運転を継続しつつ、熱交換器内部にスチームを導入して汚れを除去することにより、汚れ成分を除去し熱交換能力を回復する事が出来る。この方法により、熱交換器の停止に伴うプラントの安定操業に対する悪影響がなく、熱交換器の汚れ除去作業に伴う安全確保等の問題も生じない、熱交換器の汚れ除去方法の提供が可能となった。
【図面の簡単な説明】
【図1】多管式加熱縦型熱交換器の一例を示す図である。
【符号の説明】
1…目的物および重質物を含む液の入口、2…スチームの入口、3…加熱媒体の出入口、4…重質物の抜出口、5…目的物の出口
[0001]
BACKGROUND OF THE INVENTION
The present invention removes the internal fouling of the heating heat exchanger in the process of obtaining the object from the liquid containing the object and the heavy material while continuing the operation of the heat exchanger, and has a long-term heat exchange capability. On how to maintain.
[0002]
[Prior art]
The heating type heat exchanger is used for a distillation operation or the like for separating and purifying a target product from a liquid containing the target product and a heavy product. In this case, the dirt component of the heavy material adheres to the inside of the heat exchanger, and the heat transfer capacity of the heat exchanger decreases, so it is often necessary to stop the operation of the heat exchanger and remove the internal dirt. .
[0003]
As a method of removing dirt, the operation of the heat exchanger is temporarily stopped, the contents of the heat exchanger are taken out and the equipment is opened, and then the inside of the heat exchanger is washed with high-pressure water, buffed, mechanically cleaned A method for removing dirt by polishing or the like can be given. Such a method requires a great deal of labor, such as switching to a spare heat exchanger, opening the equipment and removing dirt, as well as ensuring the safety of the operation and the operational stability of the plant associated with the switching. Have problems.
[0004]
On the other hand, although the heat exchanger is stopped, there is also a method with a relatively small work amount in which the inside of the heat exchanger is cleaned with chemicals such as warm water and alkali without opening the equipment. However, this method has a problem in that dirt is not sufficiently removed, the heat exchange capacity is rapidly reduced after the operation is resumed, and the cleaning operation needs to be repeated frequently.
[0005]
[Problems to be solved by the invention]
Under such circumstances, the present invention provides a heat exchanger dirt removal method capable of maintaining the heat exchange capacity over a long period of time while continuing the operation without stopping the operation of the heating heat exchanger. The purpose is to do.
[0006]
[Means for Solving the Problems]
That is, the present invention is a liquid containing a target product and a heavy product, and is a chemical plant for separating and purifying a target product by distillation from a liquid containing dihydroxybenzenes and a heavy product obtained by decomposing aromatic peroxides. In the process, introducing the steam inside the heat exchanger while continuing the operation of the heat exchanger to remove the dirt based on the heavy material adhering to the inside of the heat exchanger that heats and evaporates the liquid containing the target product and the heavy material Is a heat exchanger dirt removal method that removes dirt, and is a multi-tube heating heat exchanger heat exchanger in which the heat exchanger is vertical and the pipe is straight, and dihydroxybenzenes and heavy substances Is a method for removing dirt from a heat exchanger introduced into the liquid from a nozzle provided at the bottom of the heat exchanger.
[0007]
DETAILED DESCRIPTION OF THE INVENTION
In the present invention, the liquid containing a target product and a heavy product is a liquid containing dihydroxybenzenes and a heavy product obtained by decomposing aromatic peroxides, and the heavy product separates and purifies the target product. At the same time, it adheres to the inside of the heating type heat exchanger provided at the bottom of the distillation column, etc., becomes dirty inside the heat exchanger, and inhibits the heat exchanging ability.
[0008]
Specifically, it includes a side reaction substance such as a polymer of an organic substance in the decomposition step and an inorganic substance such as a salt generated when neutralizing the acid catalyst used in the decomposition step. For example, in the case of the resorcinol process exemplified, resorcin polymer, resorcin and hydroxymethylstyrene adduct, etc., and other inorganic substances such as Na 2 SO 4 generated by the neutralization operation of the acid catalyst, etc. It becomes a dirty component of the exchanger.
[0009]
When a liquid containing such a target product and a heavy material is heated by a heating type heat exchanger, the heavy material adheres to the inside of the heat exchanger in a short period of time, and the heat exchange capacity is reduced, and the predetermined capacity of the heat exchanger can be exhibited. In addition, not only energy loss but also a decrease in production volume will cause problems in the stable operation of the entire plant.
[0010]
In order to remove the dirt inside the heat exchanger, as described above, the heat exchanger is stopped, the heat exchanger is switched to a spare machine, the equipment is opened, the dirt is removed, etc. And the operation of the chemical plant itself. Therefore, by introducing steam into the heat exchanger in the process, dirt inside the heat exchanger can be removed while the operation is continued without stopping the heat exchanger, and the heat exchange capability can be restored. . Introduction into the heat exchanger, and introduced a nozzle provided in the lower heat exchanger, an internal heat exchanger and a steam to pass through. Steam can be removed in that process or in a later process and does not affect product quality .
[0011]
One embodiment of the present invention is a multi-tube heating heat exchanger used when dihydroxybenzenes are distilled from a liquid containing dihydroxybenzenes and heavy substances obtained by acidolysis of aromatic peroxide. Is done.
[0012]
For example, in the resorcin production process, 1,3-diisopropylbenzene is oxidized to obtain a liquid containing 1,3-dihydroxyisopropylbenzene, etc., and this liquid is subjected to steps of extraction, concentration, decomposition, etc., and resorcin, acetone, Contains heavy material. When resorcin is refined and recovered from a liquid containing resorcin and heavy substances from which light boiling components such as acetone have been removed from this liquid, the heavy substances are removed by heating and distillation in a vertical multi-tube heating heat exchanger. To do.
[0013]
The heavy substance may contain a resorcin polymer, a resorcin and hydroxymethylstyrene adduct, and other inorganic substances such as Na 2 SO 4 generated by neutralization operation of an acid catalyst.
[0014]
Stops the operation of the multi-tube heating heat exchanger with dirt and heavy soil adherence and reduced overall heat transfer coefficient (hereinafter abbreviated as U), and heat exchanger with high pressure water of 1,300kg / cm 2 When the operation of the heat exchanger is resumed after washing and removing the dirt, the initial U gradually decreases and decreases to about 1/3 after 200 days of operation. If U further decreases in this state, it becomes difficult to continue operation of the entire process. Therefore, while continuing the operation of the heat exchanger, the operation was continued while introducing steam that did not adversely affect the quality of the subsequent process of the process and the resorcinol as the target product from the nozzle at the bottom of the heat exchanger. However, U began to recover gradually. After 14 days, the process recovered to about twice that before the introduction of steam, and the process was running smoothly. After the steam is stopped, the recovered U will remain recovered for at least about 60 days. Therefore, the U can be recovered simply by introducing steam from the lower nozzle of the heat exchanger as needed while monitoring the U status. I can do it.
[0015]
According to this method, not only a great effort such as stopping the heat exchanger, switching to a spare machine, opening the equipment and removing dirt is unnecessary, but also the safety of the work accompanying these work, heat exchange. It is possible to ensure the stability of plant operation associated with the switching of the equipment.
[0016]
【Example】
Example 1
Stops the operation of the vertical multi-tube heating heat exchanger with dirt and U decreasing to about 60 Kcal / m 2 · Hr · deg, and stains the heat exchanger with 1,300 kg / cm 2 high pressure water After washing out, the heat exchanger was restarted. Immediately after resuming operation, U is 180 Kcal / m 2 · Hr · deg. Met. As the operation continues, U gradually decreases. After 200 days of operation, U is 60 Kcal / m 2 · Hr · deg. Declined. Therefore, while continuing the operation of the heat exchanger, steam of 1 kg / cm 2 (120 ° C.) was introduced at the bottom of the heat exchanger at 16 kg / hr, and the operation was continued. After the introduction of steam, U began to recover gradually after the decrease in U, and after 14 days it recovered to 120 Kcal / m 2 · Hr · deg. The steam stopped on the 14th day, but it was confirmed that the recovered U would continue for about 60 days thereafter.
[0017]
Comparative Example 1
The operation of the vertical multi-tube heating heat exchanger with dirt attached and U lowered to about 60 Kcal / m 2 · Hr · deg. Was stopped, and the dirt was removed by washing with 100 ° C hot water. After the operation resumption U was recovered to 80Kcal / m 2 · Hr · deg . , But dropped to 60Kcal / m 2 · Hr · deg . In about 60 days, is no longer able to continue operation. The same operation stop and warm water washing were repeated several times, but in both cases, U decreased to 60 Kcal / m 2 · Hr · deg. Within 60 days, and stable continuous operation was not possible.
[0018]
【The invention's effect】
By removing dirt by introducing steam into the heat exchanger while continuing the operation of the heating type heat exchanger in which dirt components based on heavy substances adhere to the inside and the heat exchange capacity is reduced by the present invention. , Removes dirt components and restores heat exchange capacity. By this method, it is possible to provide a heat exchanger dirt removal method that does not adversely affect the stable operation of the plant due to the stoppage of the heat exchanger and does not cause problems such as ensuring safety associated with the heat exchanger dirt removal work. became.
[Brief description of the drawings]
FIG. 1 is a view showing an example of a multi-tube heating vertical heat exchanger.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 ... Inlet of the liquid containing a target object and a heavy material, 2 ... Steam inlet, 3 ... Heating medium inlet / outlet, 4 ... Heavy material outlet / outlet, 5 ... Outlet of target object

Claims (2)

目的物と重質物を含む液であって、芳香族ペルオキシド類を分解することにより得られるジヒドロキシベンゼン類と重質物を含む液から目的物を蒸留により分離精製する化学プラントの工程において、前記目的物と重質物を含む液を加熱蒸発させる熱交換器内部に付着する前記重質物に基づく汚れを、熱交換器の運転を継続しつつ、熱交換器の内部にスチームを導入して汚れを除去する熱交換器の汚れ除去方法であって、熱交換器が縦型で、管が直管の多管式加熱型熱交換器熱交換器であり、ジヒドロキシベンゼン類と重質物を含む液は熱交換器内を下から上向きに通過し、スチームは熱交換器下部に設けられたノズルから該液中に導入される熱交換器の汚れ除去方法。In a process of a chemical plant for separating and purifying a target product by distillation from a liquid containing dihydroxybenzenes obtained by decomposing aromatic peroxides and a heavy product, the liquid containing the target product and a heavy product. The contamination based on the heavy material adhering to the inside of the heat exchanger that heats and evaporates the liquid containing the heavy material is removed by introducing steam into the heat exchanger while continuing the operation of the heat exchanger. This is a method for removing dirt from a heat exchanger, which is a multi-tube heating heat exchanger with a vertical heat exchanger and a straight pipe, and heat exchange is performed for liquids containing dihydroxybenzenes and heavy substances. A method of removing dirt from a heat exchanger, wherein steam passes through the chamber upward from the bottom, and steam is introduced into the liquid from a nozzle provided at a lower portion of the heat exchanger. 前記ジヒドロキシベンゼン類がレゾルシンである請求項1記載の熱交換器の汚れ除去方法。  The method for removing dirt from a heat exchanger according to claim 1, wherein the dihydroxybenzene is resorcin.
JP2002061611A 2002-03-07 2002-03-07 How to remove dirt from heat exchangers Expired - Fee Related JP4069645B2 (en)

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