JP6315869B2 - Atmospheric distillation equipment tower top oil gas heat exchange device and heat exchange method - Google Patents

Atmospheric distillation equipment tower top oil gas heat exchange device and heat exchange method Download PDF

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JP6315869B2
JP6315869B2 JP2017506929A JP2017506929A JP6315869B2 JP 6315869 B2 JP6315869 B2 JP 6315869B2 JP 2017506929 A JP2017506929 A JP 2017506929A JP 2017506929 A JP2017506929 A JP 2017506929A JP 6315869 B2 JP6315869 B2 JP 6315869B2
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water injection
housing
pipe
atmospheric
heat exchange
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JP2017532388A (en
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健良 王
健良 王
賢安 張
賢安 張
興苗 胡
興苗 胡
永▲ミャオ▼ 沈
永▲ミャオ▼ 沈
奎儿 周
奎儿 周
慧麗 馬
慧麗 馬
利江 劉
利江 劉
宇 王
宇 王
晨晨 馬
晨晨 馬
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鎮海石化建安工程有限公司
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28DHEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D7/00Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G9/00Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
    • C10G9/14Thermal non-catalytic cracking, in the absence of hydrogen, of hydrocarbon oils in pipes or coils with or without auxiliary means, e.g. digesters, soaking drums, expansion means
    • C10G9/18Apparatus
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28DHEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D7/00Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
    • F28D7/0066Multi-circuit heat-exchangers, e.g. integrating different heat exchange sections in the same unit or heat-exchangers for more than two fluids
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28FDETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F19/00Preventing the formation of deposits or corrosion, e.g. by using filters or scrapers
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28FDETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F21/00Constructions of heat-exchange apparatus characterised by the selection of particular materials
    • F28F21/08Constructions of heat-exchange apparatus characterised by the selection of particular materials of metal
    • F28F21/081Heat exchange elements made from metals or metal alloys
    • F28F21/086Heat exchange elements made from metals or metal alloys from titanium or titanium alloys
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28FDETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F27/00Control arrangements or safety devices specially adapted for heat-exchange or heat-transfer apparatus
    • F28F27/02Control arrangements or safety devices specially adapted for heat-exchange or heat-transfer apparatus for controlling the distribution of heat-exchange media between different channels
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28FDETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F9/00Casings; Header boxes; Auxiliary supports for elements; Auxiliary members within casings
    • F28F9/02Header boxes; End plates
    • F28F9/0246Arrangements for connecting header boxes with flow lines
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28GCLEANING OF INTERNAL OR EXTERNAL SURFACES OF HEAT-EXCHANGE OR HEAT-TRANSFER CONDUITS, e.g. WATER TUBES OR BOILERS
    • F28G9/00Cleaning by flushing or washing, e.g. with chemical solvents
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28DHEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D21/00Heat-exchange apparatus not covered by any of the groups F28D1/00 - F28D20/00
    • F28D2021/0019Other heat exchangers for particular applications; Heat exchange systems not otherwise provided for
    • F28D2021/0059Other heat exchangers for particular applications; Heat exchange systems not otherwise provided for for petrochemical plants
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28DHEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D7/00Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
    • F28D7/02Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits being helically coiled
    • F28D7/024Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits being helically coiled the conduits of only one medium being helically coiled tubes, the coils having a cylindrical configuration
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28DHEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D7/00Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
    • F28D7/16Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits being arranged in parallel spaced relation
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28FDETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F2265/00Safety or protection arrangements; Arrangements for preventing malfunction
    • F28F2265/22Safety or protection arrangements; Arrangements for preventing malfunction for draining

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  • Engineering & Computer Science (AREA)
  • Thermal Sciences (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Heat-Exchange Devices With Radiators And Conduit Assemblies (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Description

本発明は、化学工業設備及び化学工業技術に関し、具体的には常圧蒸留装置塔頂オイルガス熱交換装置及び熱交換方法に関する。   The present invention relates to chemical industrial equipment and chemical industrial technology, and more specifically to an atmospheric gas distillation tower top oil gas heat exchange device and a heat exchange method.

常圧蒸留装置及び減圧蒸留装置は、原油加工の第一工程として、各成分の沸点の違いに基づき、蒸留することによって、原油をナフサ、ジェット燃料、ディーゼル、灯油及び減圧残油などの留分に分ける。この蒸留技術のレベル、また装置の安定的且つ高効率の運転は後続装置の生産額と経済的効果に直接関係する。現在、世界の原油の品質は全体的に落ちている。世界的な軽質原油の産出量の減少に加え、硫黄含有量が上昇し続け、油の酸性が強くなっており、また、採掘難度も上がっている。これにより加工原油に大量の塩素を含む助剤が含まれることになる。よって、常圧蒸留装置及び減圧蒸留装置で高硫黄原油を加工する際、常圧蒸留装置塔頂オイルガス側のガス量が多く、ガス速度が速いため、アンモニウム塩結晶付着による腐蝕、HCl−HS−HO腐蝕、侵食、硫化鉄の詰まり等の現象が起こる。これにより、常圧蒸留装置塔頂熱交換装置の漏れや詰まりが頻繁に起こり、常圧蒸留装置及び減圧蒸留装置の長期的サイクルでの運転に大きな影響を及ぼす。また、下流装置での原料汚染を引き起こしやすく、下流の二次加工装置の正常な運転に影響を及ぼし、多大な経済損失をもたらす。装置の建設には、一般的に材料のグレードを上げ、腐蝕防止を高める「一脱三注」処理を行い、腐蝕の問題を緩和するのだが、依然として常圧蒸留装置塔頂熱交換装置における腐蝕や漏れの発生は比較的深刻である。常圧蒸留装置塔頂熱交換装置の多くは一般的な熱交換器であり、腐蝕防止のために、既にその材料のグレードを上げてはいるが、まだ比較的多くの熱交換器は長期的なサイクルで運転するすべがなく、管束の腐蝕や漏れを起こしやすい。溶接プレート式熱交換器を採用したものもあるが、材質のグレードは上がるものの、自身の抗波動性が比較的悪く、流路が比較的小さいため、流路の詰まりと漏れが発生しやすい。 Atmospheric distillation equipment and vacuum distillation equipment, as the first step of crude oil processing, distill crude oil into fractions such as naphtha, jet fuel, diesel, kerosene and vacuum residue by distilling based on the difference in boiling point of each component. Divide into This level of distillation technology, as well as the stable and efficient operation of the equipment, is directly related to the production value and economic effects of the subsequent equipment. Currently, the global quality of crude oil is declining overall. In addition to the reduction in global light crude oil production, the sulfur content continues to rise, the acidity of the oil has increased, and the difficulty of mining has increased. As a result, the processed crude oil contains an auxiliary containing a large amount of chlorine. Therefore, when processing high-sulfur crude oil with atmospheric distillation equipment and vacuum distillation equipment, the amount of gas on the atmospheric gas distillation tower top oil gas side is large and the gas velocity is fast, so corrosion due to ammonium salt crystal adhesion, HCl-H 2 S—H 2 O corrosion, erosion, iron sulfide clogging, and other phenomena occur. As a result, leakage and clogging of the atmospheric distillation apparatus tower top heat exchange apparatus frequently occur, which greatly affects the long-term operation of the atmospheric distillation apparatus and the vacuum distillation apparatus. Moreover, it is easy to cause raw material contamination in a downstream apparatus, affects the normal operation | movement of a downstream secondary processing apparatus, and brings about a great economic loss. In the construction of the equipment, the grade of the material is generally raised and “one-and-three-note injection” treatment that enhances the corrosion prevention is performed to alleviate the corrosion problem. However, the corrosion in the atmospheric pressure distillation tower top heat exchange equipment still remains. Occurrence and leakage are relatively serious. Atmospheric distillation equipment Many of the tower top heat exchangers are general heat exchangers, and have already been upgraded to prevent corrosion, but many heat exchangers are still long-term. It is easy to cause corrosion and leakage of the tube bundle. Although some have adopted a welded plate heat exchanger, although the grade of the material is improved, its own anti-wave resistance is relatively poor and the flow path is relatively small, so that the flow path is likely to be clogged and leaked.

本発明が解決しようとする技術的課題は、従来技術の現状に対し、有効的に熱交換器の詰まりを防ぐ常圧蒸留装置塔頂オイルガス熱交換装置を提供し、装置の腐蝕を防ぎ、運転サイクルを延ばし、運転コストの削減を図ることにある。   The technical problem to be solved by the present invention is to provide an atmospheric pressure distillation column top oil gas heat exchange device that effectively prevents clogging of the heat exchanger, and prevents corrosion of the device, against the current state of the prior art, The purpose is to extend the operation cycle and reduce the operation cost.

本発明が解決しようとするもう一つの技術的課題は、従来技術の現状に対し、有効的に熱交換器の詰まりを防ぐ常圧蒸留装置塔頂オイルガス熱交換方法を提供することである。   Another technical problem to be solved by the present invention is to provide a method for exchanging oil gas at the top of the atmospheric distillation apparatus that effectively prevents clogging of the heat exchanger as compared with the state of the art.

上述の技術的課題を解決するために本発明が採用した手段は次の通りである。当該常圧蒸留装置塔頂オイルガス熱交換装置は、熱交換器を含む。前記熱交換器は、筐体と、筐体内に位置する上管プレート及び下管プレートと、上管プレート及び下管プレートに支えられた伝熱管と、を含む。各前記伝熱管の入口は、前記筐体の底部に設けられた管通路入口と接続される。各前記伝熱管の出口は前記筐体の頂部に設けられた管通路出口と接続される。前記管通路入口及び管通路出口は、原油と繋がれる。また、前記筐体の上部には、常圧蒸留装置塔頂オイルガス配管と接続される筐体通路入口が設けられる。前記筐体の下部には筐体通路出口が設けられる。この常圧蒸留装置塔頂オイルガス熱交換装置の特徴は以下の通りである。   Means employed by the present invention to solve the above technical problem are as follows. The atmospheric pressure distillation column top oil gas heat exchanger includes a heat exchanger. The heat exchanger includes a housing, an upper tube plate and a lower tube plate located in the housing, and a heat transfer tube supported by the upper tube plate and the lower tube plate. The inlet of each heat transfer tube is connected to a tube passage inlet provided at the bottom of the housing. The outlet of each heat transfer tube is connected to a tube passage outlet provided at the top of the housing. The pipe passage inlet and the pipe passage outlet are connected to crude oil. Moreover, the upper part of the said housing | casing is provided with the housing | casing channel | path inlet connected with an atmospheric pressure distillation apparatus tower top oil gas piping. A housing passage outlet is provided at the lower portion of the housing. The features of the atmospheric gas distillation tower top oil gas heat exchanger are as follows.

前記筐体内の上部には、外部注水配管と接続される環状注水管がさらに設けられる。前記環状注水管には筐体内部と連通する複数の水孔が設けられる。前記常圧蒸留装置塔頂オイルガス配管は第1注水配管と第3注水配管を介し、前記外部注水配管に接続される。前記第1注水配管と第3注水配管にはそれぞれ第1電磁弁と第2電磁弁が設けられる。前記環状注水管は第2注水配管を介して外部注水配管と接続される。   An annular water injection pipe connected to an external water injection pipe is further provided in the upper part of the housing. The annular water injection pipe is provided with a plurality of water holes communicating with the inside of the housing. The atmospheric pressure distillation tower top oil gas pipe is connected to the external water injection pipe via a first water injection pipe and a third water injection pipe. A first electromagnetic valve and a second electromagnetic valve are provided in the first water injection pipe and the third water injection pipe, respectively. The annular water injection pipe is connected to an external water injection pipe via a second water injection pipe.

より好ましくは、以下のようにしてもよい。前記筐体に注水口を設け、前記外部注水配管と前記環状注水管を、前記注水口を介して連通させる。前記環状注水管を前記上管プレートの下方且つ前記上管プレートの近傍に位置させる。前記上管プレートと下管プレートの間に位置する伝熱管が前記筐体の中心軸に沿って巻かれるように設ける。前記筐体の頂部にさらに、点検修理時に筐体内の頂部のガスを排出する排気口を前記筐体の内部と連通させて設け、前記筐体の底部に、点検修理時に筐体内の底部の液体を排出する排液口を設ける。各前記伝熱管は純チタン製の伝熱管にする。   More preferably, it may be as follows. A water inlet is provided in the casing, and the external water inlet pipe and the annular water inlet pipe are communicated with each other via the water inlet. The annular water injection pipe is positioned below the upper pipe plate and in the vicinity of the upper pipe plate. A heat transfer tube located between the upper tube plate and the lower tube plate is provided so as to be wound along the central axis of the housing. The top of the casing is further provided with an exhaust port for exhausting the gas at the top of the casing at the time of inspection / repair to communicate with the inside of the casing. A drain outlet is provided to discharge the water. Each of the heat transfer tubes is a heat transfer tube made of pure titanium.

上述の各手段に記載の常圧蒸留装置塔頂オイルガス熱交換装置を用いた熱交換方法は、以下のステップを含むことを特徴とする。   The heat exchange method using the atmospheric distillation apparatus tower top oil gas heat exchange apparatus described in the above means includes the following steps.

原油は前記熱交換器の伝熱管に入る。常圧蒸留装置塔頂オイルガスは第1注水に混ざった後、前記熱交換器の筐体内に入り、原油と熱交換を行った後、熱交換器から排出されて下流へ流れる。ここで、前記原油と前記常圧蒸留装置塔頂オイルガスの流量比は、4〜5:1であり、前記第1注水量は常圧蒸留装置塔頂オイルガス流量の2〜3%である。前記常圧蒸留装置塔頂オイルガスの温度は120℃〜150℃で、圧力は0.10〜0.15MPaGである。前記第1注水の温度は30〜50℃であり、圧力は2.0〜2.5MPaG、熱交換後の筐体通路出口の温度は80〜85℃である。   Crude oil enters the heat exchanger tubes of the heat exchanger. The oil gas at the top of the atmospheric distillation unit is mixed with the first water injection, then enters the housing of the heat exchanger, exchanges heat with the crude oil, and then is discharged from the heat exchanger and flows downstream. Here, the flow rate ratio between the crude oil and the atmospheric distillation apparatus overhead oil gas is 4-5: 1, and the first water injection amount is 2-3% of the atmospheric distillation apparatus overhead oil gas flow. . The temperature of the atmospheric gas at the top of the atmospheric distillation apparatus is 120 ° C. to 150 ° C., and the pressure is 0.10 to 0.15 MPaG. The temperature of the first water injection is 30 to 50 ° C., the pressure is 2.0 to 2.5 MPaG, and the temperature of the housing passage outlet after heat exchange is 80 to 85 ° C.

第2注水は連続的に前記環状注水管6に入り、各前記水孔61から前記筐体内に吹き出す。前記第2注水の流量と第1注水の流量の比は3〜4:1、第2注水の温度は30〜50℃である。   The second water injection continuously enters the annular water injection pipe 6 and blows out from the water holes 61 into the housing. The ratio of the flow rate of the second water injection to the flow rate of the first water injection is 3-4: 1, and the temperature of the second water injection is 30-50 ° C.

第3注水は間歇的に常圧蒸留装置塔頂オイルガス配管2に入り、筐体通路入口から筐体通路に入る。前記第3注水と第1注水の流量比は8〜12:1であり、第3注水の温度は30〜50℃であり、注水時間は25〜35分、注水サイクルは80〜100分である。   The third water injection intermittently enters the atmospheric gas distillation tower top oil gas pipe 2 and enters the housing passage from the housing passage entrance. The flow rate ratio of the third water injection and the first water injection is 8-12: 1, the temperature of the third water injection is 30-50 ° C., the water injection time is 25-35 minutes, and the water injection cycle is 80-100 minutes. .

従来技術と比べ、本発明が提供する常圧蒸留装置塔頂オイルガス熱交換装置及び熱交換方法は、オイルガス配管に対して配水し、水が環状注水管を通って筐体を洗い流すことで、有効的に熱交換率を高めている。また、着垢抑制性能も良好で、HCl−HS−HO腐蝕や着垢による腐蝕を防ぐ性能も高い。アンモニウム塩の結晶付着による腐蝕や、硫化鉄の詰まりなどの解消困難な現象を防ぐので、常圧蒸留装置塔頂オイルガス/原油の熱交換器において、腐蝕や漏れ、通路の詰まり等が生じやすいことが原因となって頻繁に起きる閉塞や漏れ、さらには装置の交換などの問題を解決できる。また、圧力損失が小さく、運転も安定しており、装置を安全に運転できるサイクルを大幅に伸ばすことができる。 Compared to the prior art, the atmospheric distillation apparatus tower top oil gas heat exchange device and heat exchange method provided by the present invention distribute water to the oil gas pipe, and the water is washed through the annular water injection pipe to wash the casing. , Effectively increasing the heat exchange rate. Moreover, the anti-sticking performance is also good, and the performance of preventing corrosion due to HCl-H 2 S—H 2 O corrosion and sticking is also high. Prevents corrosion caused by ammonium salt crystals and clogging of iron sulfide, which is difficult to eliminate, so corrosion, leakage, passage clogging, etc. easily occur in the oil gas / crude heat exchanger at the top of the atmospheric distillation unit. This can solve problems such as frequent blockages and leaks, and device replacement. In addition, the pressure loss is small, the operation is stable, and the cycle in which the apparatus can be operated safely can be greatly extended.

本発明の実施例にかかる熱交換器の正面図である。It is a front view of the heat exchanger concerning the Example of this invention. 本発明の実施例にかかる工程フロー図である。It is a process flow figure concerning the Example of this invention. 図1のA方向から見た図である。It is the figure seen from A direction of FIG. 図1のB方向から見た図である。It is the figure seen from the B direction of FIG. 図1の縦断面図である。It is a longitudinal cross-sectional view of FIG.

以下、図面及び実施例と合わせながら本発明について更に詳しく説明する。   Hereinafter, the present invention will be described in more detail with reference to the drawings and examples.

図1から図5に示すように、常圧蒸留装置塔頂オイルガス熱交換装置は、熱交換器1を含む。熱交換器1は筐体11を含む。筐体11の頂部には、各伝熱管5と連通する管通路出口18、第2注水配管32と連通する注水口15、筐体内と連通する排気口10、熱交換器の上ヘッドの側壁に設けられた筐体通路入口12が間隔をあけて設けられている。筐体11の底部には、各伝熱管5と連通する管通路入口13と、筐体内に連通する筐体通路出口14と、排液口19が間隔をあけて設けられている。   As shown in FIGS. 1 to 5, the atmospheric distillation apparatus top oil gas heat exchanger includes a heat exchanger 1. The heat exchanger 1 includes a housing 11. At the top of the housing 11, a pipe passage outlet 18 that communicates with each heat transfer tube 5, a water injection port 15 that communicates with the second water injection pipe 32, an exhaust port 10 that communicates with the interior of the housing, and a side wall of the upper head of the heat exchanger The provided housing passage inlets 12 are provided at intervals. At the bottom of the housing 11, a tube passage inlet 13 that communicates with each heat transfer tube 5, a housing passage outlet 14 that communicates within the housing, and a drainage port 19 are provided at intervals.

筐体11内にはさらに、上管プレート16と下管プレート17が設けられている。   An upper tube plate 16 and a lower tube plate 17 are further provided in the housing 11.

伝熱管5は、複数あり、全て純チタン製の伝熱管である。これにより伝熱管の腐蝕防止性能を保証している。各伝熱管の上端、下端は、それぞれ上管プレート16、下管プレート17に固定され、各伝熱管の上管プレート16と下管プレート17の間の部分は、筐体11の中心軸に沿って螺旋状に巻かれて設けられており、これにより熱交換効率を高めている。   There are a plurality of heat transfer tubes 5, all of which are pure titanium heat transfer tubes. This guarantees the corrosion prevention performance of the heat transfer tube. The upper and lower ends of each heat transfer tube are fixed to the upper tube plate 16 and the lower tube plate 17, respectively, and the portion between the upper tube plate 16 and the lower tube plate 17 of each heat transfer tube is along the central axis of the housing 11. In this way, the heat exchange efficiency is enhanced.

環状注水管6は、筐体11内の、且つ上管プレート16付近の下方に位置するよう設けられている。環状注水管6の管壁には筐体内と連通する複数の水孔61が均一に分布している。環状注水管6の入口は注水口15を介して第二注水配管32と接続されている。   The annular water injection pipe 6 is provided so as to be positioned in the housing 11 and below the upper pipe plate 16. A plurality of water holes 61 communicating with the inside of the housing are uniformly distributed on the tube wall of the annular water injection tube 6. The inlet of the annular water injection pipe 6 is connected to the second water injection pipe 32 via the water injection port 15.

筐体通路入口12は常圧蒸留装置塔頂オイルガス配管2と接続される。常圧蒸留装置塔頂オイルガス配管2には、第1注水配管31と第3注水配管33とが接続され、第1注水配管31と第3注水配管33はともに外部注水配管3と接続されている。また、第一注水配管31と第3注水配管33にはそれぞれ第1電磁弁34と第2電磁弁35が設けられている。   The housing passage inlet 12 is connected to the atmospheric gas distillation apparatus top oil gas pipe 2. A first water injection pipe 31 and a third water injection pipe 33 are connected to the atmospheric gas distillation tower top oil gas pipe 2, and both the first water injection pipe 31 and the third water injection pipe 33 are connected to the external water injection pipe 3. Yes. The first water injection pipe 31 and the third water injection pipe 33 are provided with a first electromagnetic valve 34 and a second electromagnetic valve 35, respectively.

第1注水配管31を介して常圧蒸留装置塔頂オイルガス配管2に対し水を補給し、電磁弁により水の流量を調節する。第3注水配管は常圧蒸留装置塔頂オイルガス配管2に対し、間歇的に注水するために用いられ、大量の水で筐体通路を洗い流しやすくする。   Water is replenished to the atmospheric gas distillation tower top oil gas pipe 2 through the first water injection pipe 31, and the flow rate of water is adjusted by a solenoid valve. The third water injection pipe is used to intermittently inject water into the atmospheric gas distillation tower top oil gas pipe 2 and facilitates washing of the housing passage with a large amount of water.

第1注水配管31と第3注水配管33はともに外部注水配管3と接続しており、また第1注水配管31と第3注水配管33にはそれぞれ電磁弁が設けられている。2つの電磁弁は制御システム(図示せず)と繋がっており、制御システムによって2つの電磁弁の開閉及び弁開度を制御し、各注水配管の注水を制御する。   Both the first water injection pipe 31 and the third water injection pipe 33 are connected to the external water injection pipe 3, and the first water injection pipe 31 and the third water injection pipe 33 are each provided with a solenoid valve. The two solenoid valves are connected to a control system (not shown), and the control system controls the opening and closing of the two solenoid valves and the valve opening, thereby controlling the water injection of each water injection pipe.

上述の常圧蒸留装置塔頂オイルガス熱交換装置を用いた熱交換方法は、以下のステップを含む。   The heat exchange method using the above-mentioned atmospheric distillation apparatus tower top oil gas heat exchange apparatus includes the following steps.

原油は原油配管7を通って管通路入口から各伝熱管内に入る。常圧蒸留塔8からきた常圧蒸留装置塔頂オイルガスは第1注水に混ざった後、筐体通路入口から熱交換器の筐体内に入り、原油と熱交換を行った後、筐体通路出口から排出され、下流に流れる。常圧蒸留装置塔頂オイルガスの流量は43860kg/h、温度は125℃、圧力は0.11MPaGであり、熱交換後の出口温度は82℃である。第1注水量は1000kg/hであり、温度は40℃である。原油の流量は192400kg/hであり、入口温度は32℃、圧力は2.1MPaG、熱交換後の出口温度は72℃である。   Crude oil enters the heat transfer pipes through the crude oil pipe 7 from the pipe passage inlet. After the atmospheric gas distillation tower top oil gas from the atmospheric distillation tower 8 is mixed with the first water injection, it enters the inside of the heat exchanger through the inlet of the casing passage, exchanges heat with crude oil, and then the casing passage. It is discharged from the outlet and flows downstream. The flow rate of the oil gas at the top of the atmospheric distillation apparatus tower is 43860 kg / h, the temperature is 125 ° C., the pressure is 0.11 MPaG, and the outlet temperature after heat exchange is 82 ° C. The first water injection amount is 1000 kg / h, and the temperature is 40 ° C. The flow rate of crude oil is 192400 kg / h, the inlet temperature is 32 ° C., the pressure is 2.1 MPaG, and the outlet temperature after heat exchange is 72 ° C.

第2注水は連続的に環状注水管6に入り、各水孔61から筐体内に吹き出される。第2注水は水量が3000kg〜4000kg/h、温度が40℃になるよう制御される。   The second water injection continuously enters the annular water injection pipe 6 and is blown out from each water hole 61 into the housing. The second water injection is controlled so that the amount of water is 3000 kg to 4000 kg / h and the temperature is 40 ° C.

第3注水は間歇的に常圧蒸留装置塔頂オイルガス配管2に入り、前記第3注水量が10000kg/h、温度が40℃、注水時間が30分、注水サイクルが90分になるよう制御される。第1注水と第3注水の流量及び注水時間は2つの対応する電磁弁により制御される。   The third water injection is intermittently entered into the oil gas pipe 2 at the top of the atmospheric distillation unit, and the third water injection amount is 10,000 kg / h, the temperature is 40 ° C., the water injection time is 30 minutes, and the water injection cycle is 90 minutes. Is done. The flow rate and the water injection time of the first water injection and the third water injection are controlled by two corresponding solenoid valves.

装置を停止して点検や修理をする際、装置内の媒質を完全に排出する必要がある。排気口10を開けて筐体の上部にたまった常圧蒸留装置塔頂オイルガスを排出する。装置を分解した後、洗浄し、排気口10から洗浄液を注入して、排液口19から洗浄液を排出する。   When the apparatus is stopped and inspected or repaired, it is necessary to completely discharge the medium in the apparatus. The exhaust port 10 is opened to discharge the oil gas at the top of the atmospheric distillation apparatus that has accumulated in the upper part of the housing. After disassembling the apparatus, the apparatus is cleaned, the cleaning liquid is injected from the exhaust port 10, and the cleaning liquid is discharged from the drain port 19.

従来の一般的な常圧蒸留装置塔頂熱交換装置の使用寿命は約1〜2年であり、腐蝕や漏れが起こった後は全体を交換したり、管束を交換したりする必要がある。通路が詰まるため、頻繁に洗浄を行わなければならない。本発明の熱交換装置及び熱交換方法によれば、装置本体に良好な腐蝕抑制性能や着垢抑制性能を与えることができる。2期の運転サイクルである8年内に、着垢による詰まり、腐蝕、漏れなどの問題が生じない。よって、装置の交換や点検修理、メンテナンスにかかる費用を大幅に節約することができる。   The service life of the conventional general atmospheric distillation apparatus tower top heat exchanger is about 1 to 2 years, and after corrosion or leakage, it is necessary to replace the whole or replace the tube bundle. Because the passage is clogged, frequent cleaning is required. According to the heat exchange apparatus and the heat exchange method of the present invention, it is possible to give the apparatus main body good corrosion inhibition performance and scaling inhibition performance. There will be no problems such as clogging, corrosion, or leakage due to settling within 8 years, which is the second operation cycle. Therefore, it is possible to greatly save the cost for device replacement, inspection and repair, and maintenance.

Claims (7)

熱交換器(1)を含み、前記熱交換器は、筐体(11)と、前記筐体(11)内に位置する上管プレート(16)及び下管プレート(17)と、前記上管プレート及び前記下管プレートに支えられた伝熱管(5)と、を含み、各前記伝熱管(5)の入口は前記筐体の底部に設けられた管通路入口(13)と接続され、各前記伝熱管(5)の出口は前記筐体の頂部に設けられた管通路出口(18)と接続され、
前記管通路入口及び前記管通路出口は原油と繋がれ、また、前記筐体(11)の上部には常圧蒸留装置塔頂オイルガス配管(2)と接続される筐体通路入口が設けられ、前記筐体の下部に筐体通路出口が設けられる、常圧蒸留装置塔頂オイルガス熱交換装置であって、
前記筐体(11)内の上部には、外部注水配管(3)と接続される環状注水管(6)がさらに設けられ、前記環状注水管(6)に前記筐体の内部と連通する複数の水孔(61)が設けられ、
前記常圧蒸留装置塔頂オイルガス配管(2)は第1注水配管(31)と第3注水配管(33)を介して前記外部注水配管(3)に接続され、
前記第1注水配管(31)と前記第3注水配管(33)にはそれぞれ第1電磁弁(34)と第2電磁弁(35)が設けられ、
前記環状注水管(6)は第2注水配管(32)を介して前記外部注水配管(3)と接続される、
ことを特徴とする常圧蒸留装置塔頂オイルガス熱交換装置。
The heat exchanger includes a housing (11), an upper tube plate (16) and a lower tube plate (17) located in the housing (11), and the upper tube. A heat transfer tube (5) supported by the plate and the lower tube plate, and an inlet of each of the heat transfer tubes (5) is connected to a tube passage inlet (13) provided at the bottom of the casing, The outlet of the heat transfer tube (5) is connected to a tube passage outlet (18) provided at the top of the housing,
The pipe passage inlet and the pipe passage outlet are connected to crude oil, and a housing passage inlet connected to the atmospheric distillation tower top oil gas pipe (2) is provided at an upper portion of the housing (11). An atmospheric pressure distillation apparatus tower top oil gas heat exchange device in which a housing passage outlet is provided at a lower portion of the housing,
An annular water injection pipe (6) connected to an external water injection pipe (3) is further provided in the upper part of the housing (11), and a plurality of pipes communicating with the inside of the housing are connected to the annular water injection pipe (6). Water holes (61) are provided,
The atmospheric distillation apparatus tower top oil gas pipe (2) is connected to the external water injection pipe (3) via a first water injection pipe (31) and a third water injection pipe (33),
A first solenoid valve (34) and a second solenoid valve (35) are provided in the first water injection pipe (31) and the third water injection pipe (33), respectively.
The annular water injection pipe (6) is connected to the external water injection pipe (3) via a second water injection pipe (32).
An atmospheric gas distillation tower top oil gas heat exchanger.
前記筐体(11)に注水口(15)を設け、前記外部注水配管(3)と前記環状注水管(6)が、前記注水口(5)を介して連通することを特徴とする請求項1に記載の常圧蒸留装置塔頂オイルガス熱交換装置。   The water injection port (15) is provided in the housing (11), and the external water injection pipe (3) and the annular water injection pipe (6) communicate with each other through the water injection port (5). The atmospheric oil distillation heat exchanger of the top of the atmospheric distillation apparatus according to 1. 前記環状注水管()は前記上管プレート(16)の下方且つ前記上管プレート(16)近傍に位置することを特徴とする、請求項1又は2に記載の常圧蒸留装置塔頂オイルガス熱交換装置。 The atmospheric distillation apparatus top oil according to claim 1 or 2, wherein the annular water injection pipe ( 6 ) is located below the upper pipe plate (16) and in the vicinity of the upper pipe plate (16). Gas heat exchange device. 前記上管プレート(16)と前記下管プレート(17)の間に位置する前記伝熱管(5)は、前記筐体(11)の中心軸に沿って巻かれるように設けられることを特徴とする、請求項3に記載の常圧蒸留装置塔頂オイルガス熱交換装置。   The heat transfer tube (5) positioned between the upper tube plate (16) and the lower tube plate (17) is provided so as to be wound along a central axis of the housing (11). The atmospheric pressure distillation apparatus top oil gas heat exchanger according to claim 3. 前記筐体(11)の頂部にはさらに、点検修理時に前記筐体内の頂部のガスを排出する排気口(10)が前記筐体の内部と連通して設けられており、前記筐体(11)の底部には、点検修理時に前記筐体内の底部の液体を排出する排液口(19)が設けられていることを特徴とする、請求項3に記載の常圧蒸留装置塔頂オイルガス熱交換装置。   The top of the casing (11) is further provided with an exhaust port (10) for exhausting the gas at the top in the casing at the time of inspection / repair, and communicates with the inside of the casing. The bottom gas outlet (19) is provided with a drainage port (19) for discharging the liquid at the bottom in the casing during inspection and repair. Heat exchange device. 各前記伝熱管は純チタン製の伝熱管であることを特徴とする、請求項3に記載の常圧蒸留装置塔頂オイルガス熱交換装置。   4. The atmospheric distillation apparatus top oil gas heat exchange device according to claim 3, wherein each of the heat transfer tubes is a heat transfer tube made of pure titanium. 請求項1から6のいずれかひとつに記載の常圧蒸留装置塔頂オイルガス熱交換装置を用いた熱交換方法であって、
原油は前記熱交換器の前記伝熱管に入り、常圧蒸留装置塔頂オイルガスは第1注水に混ざった後、前記熱交換器の前記筐体内に入り、前記原油と熱交換を行った後、前記熱交換器から排出されて下流へ流れるが、ここで、前記原油と前記常圧蒸留装置塔頂オイルガスの流量比は4〜5:1であり、前記第1注水量は前記常圧蒸留装置塔頂オイルガス流量の2〜3%であって、前記常圧蒸留装置塔頂オイルガスの温度は120℃〜150℃、圧力は0.10〜0.15MPaGであり、前記第1注水の温度は30〜50℃、圧力は2.0〜2.5MPaGであり、熱交換後の前記筐体通路出口の温度は80〜85℃であるステップと、
第2注水は連続的に前記環状注水管(6)に入って各前記水孔(61)から前記筐体内に吹き出し、前記第2注水の流量と前記第1注水の流量の比は3〜4:1、前記第2注水の温度は30〜50℃であるステップと、
第3注水は間歇的に前記常圧蒸留装置塔頂オイルガス配管に入って前記筐体通路入口から前記筐体通路に入り、前記第3注水と前記第1注水の流量比は8〜12:1であり、前記第3注水の温度は30〜50℃であり、注水時間は25〜35分、注水サイクルは80〜100分であるステップと、を含むことを特徴とする、常圧蒸留装置塔頂オイルガス熱交換装置を用いた熱交換方法。
A heat exchange method using the atmospheric distillation apparatus tower top oil gas heat exchange device according to any one of claims 1 to 6,
After the crude oil enters the heat transfer tube of the heat exchanger, the oil gas at the top of the atmospheric distillation apparatus is mixed with the first water injection, and then enters the housing of the heat exchanger and performs heat exchange with the crude oil. , Discharged from the heat exchanger and flowing downstream, wherein the flow rate ratio of the crude oil and the atmospheric oil at the top of the atmospheric distillation unit is 4 to 5: 1, and the first water injection amount is the atmospheric pressure. 2 to 3% of the distillation apparatus tower top oil gas flow rate, the temperature of the atmospheric distillation tower top oil gas is 120 ° C to 150 ° C, the pressure is 0.10 to 0.15 MPaG, and the first water injection The temperature is 30-50 ° C., the pressure is 2.0-2.5 MPaG, and the temperature of the housing passage outlet after heat exchange is 80-85 ° C.,
The second water injection continuously enters the annular water injection pipe (6) and blows out from the water holes (61) into the housing, and the ratio of the flow rate of the second water injection to the flow rate of the first water injection is 3-4. 1: the temperature of the second water injection is 30-50 ℃,
The third water injection intermittently enters the atmospheric gas distillation tower top oil gas pipe ( 2 ) and enters the housing passage from the housing passage inlet, and the flow ratio of the third water injection to the first water injection is 8 The temperature of the third water injection is 30 to 50 ° C., the water injection time is 25 to 35 minutes, and the water injection cycle is 80 to 100 minutes. A heat exchange method using an oil gas heat exchanger at the top of a pressure distillation apparatus.
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CN110373222B (en) * 2019-07-29 2024-06-14 镇海石化建安工程股份有限公司 Atmospheric and vacuum heat exchange system with winding tube type heat exchanger and heat exchange process
CN114440698A (en) * 2020-11-05 2022-05-06 南京科技职业学院 Method for reducing burning-through of furnace door of tubular furnace by degreasing and alkali washing heat exchanger
CN115597402B (en) * 2022-09-30 2023-08-04 镇海石化建安工程股份有限公司 Heat exchange assembly and heat exchange process for hydrogenation unit
CN118517932B (en) * 2024-07-23 2024-10-01 江苏润睿生物科技有限公司 Heat exchanger based on sealing leakage-proof pipe fitting and heat exchange method for oleic acid production

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE566112A (en) * 1957-05-21
JPS5849482Y2 (en) * 1977-06-20 1983-11-11 川崎重工業株式会社 Fire pipe type water heater
JPS5849482A (en) * 1981-09-19 1983-03-23 株式会社 サタケ Grain selecting apparatus
JPH09159393A (en) * 1995-12-08 1997-06-20 Tokyo Gesuido Energ Kk Method of promoting peeling off of deposit on inside wall of tube of heat exchanger
US6283133B1 (en) * 1997-08-18 2001-09-04 Jgc Corporation Method for cleaning heavy hydrocarbon scale adhered to heat exchanger and piping structure for cleaning
CN202902937U (en) * 2012-11-02 2013-04-24 镇海石化建安工程有限公司 Heat exchanger structure
CN103453782B (en) * 2013-09-18 2015-01-28 南京都乐制冷设备有限公司 Three-in-one shell and tube oil-gas heat exchanger
CN103673693A (en) * 2013-12-10 2014-03-26 山东蓝星清洗防腐公司 Novel crude oil normal-pressure tower top oil-gas heat exchanger
CN104697293A (en) 2015-03-03 2015-06-10 李丽芬 Miraflor drying method
CN104697393A (en) * 2015-03-16 2015-06-10 北京中科华誉热泵设备制造有限公司 Shell tube dry type evaporator with spraying type cleaning structure
CN204478881U (en) * 2015-03-17 2015-07-15 江苏国信淮安燃气发电有限责任公司 The secondary heat exchange water tank of water-bath stove heating system
CN204987954U (en) * 2015-07-30 2016-01-20 镇海石化建安工程有限公司 Ordinary pressure top of tower oil gas heat transfer device

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