TW201544156A - Heads column overhead system - Google Patents
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- TW201544156A TW201544156A TW104109003A TW104109003A TW201544156A TW 201544156 A TW201544156 A TW 201544156A TW 104109003 A TW104109003 A TW 104109003A TW 104109003 A TW104109003 A TW 104109003A TW 201544156 A TW201544156 A TW 201544156A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
Abstract
Description
本發明涉及一種用於製造丙烯腈和甲基丙烯腈的改進的方法。特別是,本發明涉及氰化氫(HCN)的改進的頭餾分塔(heads column)塔頂處理。 The present invention relates to an improved process for the manufacture of acrylonitrile and methacrylonitrile. In particular, the present invention relates to an improved heads column overhead treatment of hydrogen cyanide (HCN).
已知用於製造丙烯腈和甲基丙烯腈的多種方法和系統;參見例如,美國專利號6,107,509。如美國專利號6,107,509中記錄的,常規的方法通常涉及在已完成烴(選自丙烷、丙烯或異丁烯),氨和氧在催化劑存在下的直接反應後,通過以下方法回收和純化產生的丙烯腈/甲基丙烯腈:將含有丙烯腈/甲基丙烯腈的反應器流出物輸送至第一塔(驟冷),其中使用第一含水流冷卻反應器流出物,將經冷卻的含有丙烯腈/甲基丙烯腈的流出物輸送至第二塔(吸收器),其中經冷卻的流出物與第二含水流接觸以將丙烯腈/甲基丙烯腈吸收到第二含水流中,將含有丙烯腈/甲基丙烯腈的第二含水流從第二塔輸送至第一蒸餾塔(回收塔)用於使粗品丙烯腈/甲基丙烯腈與第二含水流分離,和將已分離 的粗品丙烯腈/甲基丙烯腈輸送至第二蒸餾塔(頭餾分塔)以從粗品丙烯腈/甲基丙烯腈除去至少一些雜質,和將部分純化的丙烯腈/甲基丙烯腈輸送至第三蒸餾塔(產物塔)以得到產物丙烯腈/甲基丙烯腈。美國專利號4,234,510;3,885,928;3,352,764;3,198,750和3,044,966說明丙烯腈和甲基丙烯腈的典型的回收和純化方法。 A variety of methods and systems are known for making acrylonitrile and methacrylonitrile; see, for example, U.S. Patent No. 6,107,509. As noted in U.S. Patent No. 6,107,509, the conventional method generally involves recovering and purifying the produced acrylonitrile by the following method after a completed hydrocarbon (selected from propane, propylene or isobutylene), direct reaction of ammonia and oxygen in the presence of a catalyst. /Methacrylonitrile: The reactor effluent containing acrylonitrile/methacrylonitrile is sent to a first column (quench) in which the reactor effluent is cooled using a first aqueous stream, and the cooled acrylonitrile is contained/ The methacrylonitrile effluent is passed to a second column (absorber) wherein the cooled effluent is contacted with a second aqueous stream to absorb acrylonitrile/methacrylonitrile into the second aqueous stream, which will contain acrylonitrile The second aqueous stream of /methacrylonitrile is transported from the second column to the first distillation column (recovery column) for separating the crude acrylonitrile/methacrylonitrile from the second aqueous stream, and will be separated The crude acrylonitrile/methacrylonitrile is sent to a second distillation column (heads column) to remove at least some impurities from the crude acrylonitrile/methacrylonitrile, and to deliver the partially purified acrylonitrile/methacrylonitrile to the first A tristillation column (product column) to give the product acrylonitrile/methacrylonitrile. Typical recovery and purification methods for acrylonitrile and methacrylonitrile are described in U.S. Patent Nos. 4,234,510; 3,885,928; 3,352,764; 3,198,750 and 3,044,966.
丙烯腈製造方法生產非常毒性的HCN副產物。在 設備操作或維修期間,為了使人暴露於HCN最小化,有用的是使可以處理HCN的設備具有低洩漏風險。一種方法是使用重力流動來消除在HCN使用(service)中對泵的需求。然而,在丙烯腈設備HCN塔或頭餾分塔中,污染(特別是塔板的污染)通常成為問題。 The acrylonitrile manufacturing process produces very toxic HCN by-products. in In order to minimize exposure of humans to HCN during operation or maintenance of the equipment, it is useful to have a low leakage risk for equipment that can handle HCN. One approach is to use gravity flow to eliminate the need for pumps in HCN service. However, in the acrylonitrile plant HCN column or heads column, contamination (especially tray fouling) is often a problem.
因此,本公開的一方面提供一種克服或減少常規方法的缺點的安全、有效和成本高效的方法和設備。 Accordingly, an aspect of the present disclosure provides a safe, efficient, and cost effective method and apparatus that overcomes or reduces the disadvantages of conventional methods.
在一方面,所述設備包含頭餾分塔和塔頂系統(overhead system)。所述頭餾分塔設置成接受粗品腈類原料流。所述頭餾分塔設置成在部分真空下操作的同時蒸餾粗品腈類原料流,並且生產在頭餾分塔頂部的包含HCN的頭餾分塔塔頂物流以及在頭餾分塔底部的包含丙烯腈產物的底部液體物流。所述塔頂系統包含設置成冷凝頭餾分塔塔頂物流的冷凝器。所述設備包含無密封墊的泵。所述泵設置成在冷凝器中冷凝頭餾分塔塔頂物流之後,泵送至少一 部分頭餾分塔塔頂物流。 In one aspect, the apparatus comprises a heads column and an overhead system. The heads column is configured to accept a crude nitrile feed stream. The heads column is arranged to distill a crude nitrile feed stream while operating under partial vacuum, and to produce a heads stream stream comprising HCN at the top of the heads column and an acrylonitrile product at the bottom of the heads column. Bottom liquid stream. The overhead system comprises a condenser arranged to condense the overhead stream of the heads column. The device comprises a pump without a gasket. The pump is arranged to pump at least one after condensing the head column overhead stream in the condenser Part of the heads fraction tower top stream.
本公開的以上和其它方面、特徵和優點由其帶附 圖的實施方案的詳細說明而顯而易見,所述實施方案應結合附圖閱讀。 The above and other aspects, features, and advantages of the present disclosure are attached It will be apparent from the detailed description of the embodiments of the drawings that the description
1‧‧‧粗品腈類原料流 1‧‧‧ crude nitrile feedstock
2‧‧‧頭餾分塔塔頂物流 2‧‧‧ head fractionation tower top logistics
3‧‧‧回流物流 3‧‧‧Return Logistics
4‧‧‧水流 4‧‧‧Water flow
5‧‧‧HCN副產物物流 5‧‧‧HCN by-product logistics
6‧‧‧冷凝器出口物流 6‧‧‧Condenser export logistics
7‧‧‧接點 7‧‧‧Contacts
8‧‧‧控制器、流量控制器 8‧‧‧Controller, flow controller
9‧‧‧閥、控制閥 9‧‧‧Valves, Control Valves
10‧‧‧設備 10‧‧‧ Equipment
12‧‧‧頭餾分塔 12‧‧‧ heads tower
14‧‧‧塔頂系統 14‧‧‧Tower System
16‧‧‧冷凝器 16‧‧‧Condenser
18‧‧‧無密封墊的泵、控制泵 18‧‧‧No gasket pump, control pump
20‧‧‧溫度控制器 20‧‧‧ Temperature Controller
22‧‧‧料倉、冷凝器料倉 22‧‧‧ silo, condenser silo
25‧‧‧閥、產物閥 25‧‧‧Valve, product valve
26‧‧‧液體物流 26‧‧‧Liquid Logistics
27‧‧‧液位控制器 27‧‧‧Level controller
28‧‧‧塔板、頂部塔板 28‧‧‧Tray, top tray
30‧‧‧頂部塔板 30‧‧‧Top tray
32‧‧‧中間塔板 32‧‧‧Intermediate tray
34‧‧‧底部 34‧‧‧ bottom
40‧‧‧流量控制器 40‧‧‧Flow controller
68‧‧‧控制器 68‧‧‧ Controller
200、300‧‧‧方法 200, 300‧‧‧ method
201-205、301-305‧‧‧步驟 201-205, 301-305‧‧‧ steps
通過考慮附圖參考以下描述,可獲得對本發明的示例性實施方案及其優點的更完整的理解,其中相同的附圖標記指示相同的特徵,其中:圖1為應用於丙烯腈產物製造的根據本公開各方面的一個實施方案的示意性流程圖。 A more complete understanding of the exemplary embodiments of the invention and the advantages thereof, in which the A schematic flow diagram of one embodiment of various aspects of the present disclosure.
圖2說明根據本公開各方面的方法的流程圖。 2 illustrates a flow chart of a method in accordance with aspects of the present disclosure.
圖3說明根據本公開各方面的方法的流程圖。 FIG. 3 illustrates a flow chart of a method in accordance with aspects of the present disclosure.
圖4為應用於丙烯腈產物製造的根據本公開各方面的一個備選實施方案的示意性流程圖。 4 is a schematic flow diagram of an alternate embodiment for the manufacture of acrylonitrile products in accordance with aspects of the present disclosure.
丙烯腈設備的回收部分生產粗品腈類原料流,其為包含丙烯腈、HCN和水的混合物。在丙烯腈純化中的加工步驟為通過蒸餾除去HCN副產物。從粗品腈類原料流除去HCN的蒸餾塔稱為HCN塔、頭餾分塔或頭餾分乾燥塔。使用該蒸餾塔,可作為高純度塔頂產物回收HCN。 The recovered portion of the acrylonitrile plant produces a crude nitrile feed stream which is a mixture comprising acrylonitrile, HCN and water. The processing step in the purification of acrylonitrile is the removal of HCN by-products by distillation. The distillation column from which the HCN is removed from the crude nitrile feed stream is referred to as an HCN column, a heads column or a heads column drying column. Using this distillation column, HCN can be recovered as a high purity overhead product.
在丙烯腈設備HCN塔或頭餾分塔中,塔板污染通常成為問題。已發現降低HCN塔或頭餾分塔中的壓力,例如,在部分真空下運行HCN塔或頭餾分塔,顯著降低污染 並且延長在HCN塔或頭餾分塔的清潔之間的執行時間。然而,在減壓下操作HCN塔或頭餾分塔需要較低的冷凝溫度並且需要使用較大的冷凝器。結果是,設計用於真空使用的頭餾分塔的冷凝器通常太大而不能物理安裝在頭餾分塔的頂部或接近頂部。如果冷凝器向下安裝在接近頭餾分塔的支撐結構中,一個(或多個)泵可用於為頭餾分塔提供回流和/或將HCN副產物送至HCN使用者和/或HCN儲存和/或處置(disposal)。 In the acrylonitrile plant HCN column or heads column, tray fouling is often a problem. It has been found that reducing the pressure in the HCN or heads column, for example, operating the HCN or heads column under partial vacuum, significantly reduces pollution And extend the execution time between the cleaning of the HCN tower or the heads column. However, operating a HCN column or a heads column under reduced pressure requires a lower condensation temperature and requires the use of a larger condenser. As a result, the condenser of the heads column designed for vacuum use is typically too large to be physically mounted on top of or near the top of the heads column. If the condenser is installed down into the support structure near the heads column, one (or more) pumps can be used to provide reflux to the heads column and/or to deliver HCN by-products to HCN users and/or HCN storage and/or Or disposal (disposal).
在本公開的一方面,無密封墊的泵(例如,磁性 偶聯的泵和/或在電機軸和葉輪之間沒有直接連接的泵)可用於頭餾分塔的塔頂系統。通過使用無密封墊的泵,HCN洩漏風險可最小化,因為這種類型的泵不具有可洩漏的驅動密封,並且不存在從電機到泵送的流體的傳熱。 In an aspect of the disclosure, a gasketless pump (eg, magnetic A coupled pump and/or a pump that has no direct connection between the motor shaft and the impeller can be used in the overhead system of the heads column. By using a sealless pump, the risk of HCN leakage can be minimized because this type of pump does not have a leaky drive seal and there is no heat transfer from the motor to the pumped fluid.
參考圖1詳細描述本公開的方法和設備。 The method and apparatus of the present disclosure are described in detail with reference to FIG.
設備10在用於丙烯腈製造方法的回收塔(在圖1中未顯示)的下游。設備10包含頭餾分塔12和塔頂系統14。頭餾分塔12設置成蒸餾粗品腈類原料流1,並且生產主要包含HCN以及痕量的丙烯腈和水的頭餾分塔塔頂物流2。粗品腈類原料流1可包括約82-約90重量%的丙烯腈,和約5-約13重量%的HCN,組合物的餘量為水。在該方面,可引起污染的組分取決於所用的抑制劑的類型。 Apparatus 10 is downstream of a recovery column (not shown in Figure 1) for the acrylonitrile manufacturing process. Apparatus 10 includes a heads column 12 and a top system 14. The heads column 12 is arranged to distill the crude nitrile feed stream 1 and produce a heads column overhead stream 2 comprising primarily HCN and traces of acrylonitrile and water. The crude nitrile feed stream 1 can comprise from about 82 to about 90 weight percent acrylonitrile, and from about 5 to about 13 weight percent HCN, with the balance of the composition being water. In this respect, the components that can cause contamination depend on the type of inhibitor used.
塔頂系統14包含設置成冷凝頭餾分塔塔頂物流2的冷凝器16。塔頂系統14包含無密封墊的泵18。在一方面,頭餾分塔12可設置成在部分真空下操作的同時蒸餾粗品腈 類原料流1。在一方面,頭餾分塔12可設置成在0.044-0.090MPa絕對壓力的部分真空下操作的同時蒸餾粗品腈類原料流1。在一種實施方案中,頭餾分塔12在頂部壓力為約0.075MPa絕對壓力的部分真空下蒸餾粗品腈類原料流1。頭餾分塔12中的流體可通過備用的再沸器(在圖1中未顯示)加熱,該再沸器可常用於加熱頭餾分塔12中的流體和在頭餾分塔12下游的產物塔(在圖1中未顯示)中的流體。貧水可用作一個(或多個)再沸器的熱源。 The overhead system 14 includes a condenser 16 that is configured to condense the heads column overhead stream 2. The overhead system 14 includes a pump 18 without a gasket. In one aspect, the heads column 12 can be configured to distill the crude nitrile while operating under partial vacuum. Class feed stream 1. In one aspect, the heads column 12 can be configured to distill the crude nitrile feed stream 1 while operating at a partial vacuum of 0.044-0.090 MPa absolute. In one embodiment, the heads column 12 distills the crude nitrile feed stream 1 under partial vacuum at a top pressure of about 0.075 MPa absolute. The fluid in the heads column 12 can be heated by a backup reboiler (not shown in Figure 1) which can be used to heat the fluid in the heads column 12 and the product column downstream of the heads column 12 ( The fluid in (not shown in Figure 1). Lean water can be used as a heat source for one (or more) reboilers.
頭餾分塔12包含多個塔板。在一種實施方案中, 頭餾分塔12包含五十二(52)-七十二(72)個塔板。在一種實施方案中,頭餾分塔12包含六十二(62)個塔板。頭餾分塔12可設置成在塔板28處接受粗品腈類原料流1。在一種實施方案中,塔板28可為距頭餾分塔12的底部第42個塔板。在一個備選的實施方案中,塔板28可為距頭餾分塔12的底部第38個塔板。在一個備選的實施方案中,塔板28可為距頭餾分塔12的底部第47個塔板,並且頭餾分塔12可包含六十七(67)個塔板。在一種實施方案中,頭餾分塔12的第1個-第20個底部塔板乾燥丙烯腈產物。在一種實施方案中,距頭餾分塔12的底部34第21個-第42個塔板除去和純化HCN。在一種實施方案中,頭餾分塔12可不帶乾燥功能操作。在一種實施方案中,頭餾分塔12包含四十(40)-六十五(65)個塔板。 在一種實施方案中,進料塔板28可在距頭餾分塔的底部第20個-第30個塔板之間,包括第20個塔板和第30個塔板。 The heads column 12 contains a plurality of trays. In one embodiment, The heads column 12 contains fifty-two (52)-seventy-two (72) trays. In one embodiment, the heads column 12 comprises sixty-two (62) trays. The heads column 12 can be configured to accept the crude nitrile feed stream 1 at the tray 28. In one embodiment, tray 28 can be the 42nd tray from the bottom of heads column 12. In an alternate embodiment, tray 28 can be the 38th tray from the bottom of heads column 12. In an alternate embodiment, tray 28 can be the 47th tray from the bottom of heads column 12, and heads column 12 can contain sixty-seven (67) trays. In one embodiment, the first to twentieth bottom trays of the heads column 12 are dried with an acrylonitrile product. In one embodiment, the 21st-42th tray from the bottom 34 of the heads column 12 removes and purifies the HCN. In one embodiment, the heads column 12 can be operated without a drying function. In one embodiment, the heads column 12 comprises forty (40) to sixty-five (65) trays. In one embodiment, the feed tray 28 can be between the 20th and 30th trays from the bottom of the heads column, including the 20th tray and the 30th tray.
冷凝器16可設置成接受冷卻的或冷凍的水(RW) 流4。冷凍的水流4可包含防凍劑,並且通向冷凝器16的入口溫度為約-10至5℃。在一方面,冷凝器16可位於接近頭餾分塔12,但是不在頭餾分塔12的頂部。冷凝器16(包括適當的尺寸)可設置成適應在部分真空下操作頭餾分塔12所需的較低的溫度。用於操作頭餾分塔12的較低的溫度可為-10至+10℃。 The condenser 16 can be configured to accept cooled or frozen water (RW) Stream 4. The chilled water stream 4 may contain an antifreeze and the inlet temperature to the condenser 16 is between about -10 and 5 °C. In one aspect, the condenser 16 can be located near the heads column 12, but not at the top of the heads column 12. The condenser 16 (including suitable dimensions) can be configured to accommodate the lower temperatures required to operate the heads column 12 under partial vacuum. The lower temperature for operating the heads column 12 can range from -10 to +10 °C.
無密封墊的泵18可用於泵送來自冷凝器16的主 要包含HCN的冷凝器出口物流6。冷凝器出口物流6可在接點7處分成回流物流3和HCN副產物物流5。在一方面,可將HCN副產物物流5送至HCN使用者、HCN儲存或處置。 A gasketless pump 18 can be used to pump the main from the condenser 16 The condenser outlet stream 6 of HCN is to be included. The condenser outlet stream 6 can be separated at point 7 into a reflux stream 3 and an HCN byproduct stream 5. In one aspect, the HCN by-product stream 5 can be sent to an HCN user, HCN for storage or disposal.
回流物流3可流向頭餾分塔12。系統可利用約2- 約7的回流比,在另一方面,約2-約6.5的回流比,在另一方面,約3-約6的回流比。在一方面,可在頭餾分塔12的頂部塔板30中接受回流物流3。在一種實施方案中,頭餾分塔12的頂部塔板30可為距頭餾分塔12的底部第62個塔板。在一方面,可通過設置成調節閥9的流量控制器8來調節回流物流3的流量。流量控制器8可通過溫度控制器20來控制。溫度控制器20可位於低於頭餾分塔12的頂部塔板30的頭餾分塔12的中間塔板32處。在一方面,控制器68可設置成處理對應於測量參數(例如,通過溫度控制器20測量的溫度)的一個或多個信號。控制器68可設置成確定測量參數是高於還是低於預定的參數範圍,例如,通過溫度控制器20測量的溫度低於或高於預定的溫度範圍。如果測量的參數低於或高於預定的參數範圍,控制器68可設置成經由通訊線路或 無線通訊(在圖1中未顯示)調節一個或多個裝置的操作。例如,當通過溫度控制器20測量的溫度低於或高於預定的溫度範圍時,控制器68可設置成調節流向頭餾分塔12的回流物流3的量。控制器68可設置成控制泵18的操作和/或閥9的操作,例如控制閥9的開孔的尺寸。本領域技術人員認識到,控制器68或類似的控制器可位於遠離流量控制器8(如在圖1中所示),或者可位於流量控制器8處並且包括流量控制器8。 The reflux stream 3 can be passed to the heads column 12. The system can utilize about 2 A reflux ratio of about 7, on the other hand, a reflux ratio of from about 2 to about 6.5, and on the other hand, a reflux ratio of from about 3 to about 6. In one aspect, the reflux stream 3 can be received in the top tray 30 of the heads column 12. In one embodiment, the top tray 30 of the heads column 12 can be the 62nd tray from the bottom of the heads column 12. In one aspect, the flow rate of the reflux stream 3 can be adjusted by a flow controller 8 provided as a regulating valve 9. The flow controller 8 can be controlled by the temperature controller 20. The temperature controller 20 can be located at an intermediate tray 32 below the heads column 12 of the top tray 30 of the heads column 12. In an aspect, the controller 68 can be configured to process one or more signals corresponding to the measured parameters (eg, the temperature measured by the temperature controller 20). The controller 68 can be arranged to determine whether the measured parameter is above or below a predetermined range of parameters, for example, the temperature measured by the temperature controller 20 is below or above a predetermined temperature range. If the measured parameter is below or above a predetermined parameter range, the controller 68 can be set to be via a communication line or Wireless communication (not shown in Figure 1) regulates the operation of one or more devices. For example, controller 68 may be configured to regulate the amount of reflux stream 3 flowing to heads column 12 when the temperature measured by temperature controller 20 is below or above a predetermined temperature range. Controller 68 may be arranged to control the operation of pump 18 and/or the operation of valve 9, such as the size of the opening of control valve 9. Those skilled in the art recognize that controller 68 or a similar controller may be located remote from flow controller 8 (as shown in FIG. 1) or may be located at flow controller 8 and include flow controller 8.
冷凝器16可包含冷凝器料倉(boot)22和液位控制 器27。液位控制器27可設置成控制冷凝器料倉22中冷凝的液體的液位。如在圖1中所示,液位控制器27可設置成通過調節產物閥25的開孔而控制冷凝器料倉22中冷凝的液體的液位。如在圖1中所示,閥25可位於冷凝器16的下游。在一種實施方案中,控制器68可設置成處理對應於測量參數(例如,通過液位控制器27測量的冷凝器料倉22中液體的液位)的信號。控制器68可設置成確定通過液位控制器27測量的液體液位是高於還是低於冷凝器料倉22的預定液體液位範圍。如果在冷凝器料倉22中測量的液體液位高於或低於冷凝器料倉22的預定的液體液位範圍,控制器68可設置成經由通訊線路或無線通訊(在圖1中未顯示)調節一個或多個裝置的操作。例如,當在冷凝器料倉22中測量的液體液位高於或低於冷凝器料倉22的預定的液體液位範圍時,控制器68可設置成調節閥25的開孔的尺寸。本領域技術人員認識到,控制器68或類似的控制器可位於遠離液位控制器27(如 在圖1中所示),或者可位於液位控制器27處並且包括液位控制器27。 The condenser 16 can include a condenser bin 22 and level control 27. The level controller 27 can be configured to control the level of liquid condensed in the condenser bin 22. As shown in FIG. 1, the level controller 27 can be configured to control the level of liquid condensed in the condenser bin 22 by adjusting the opening of the product valve 25. As shown in FIG. 1, valve 25 can be located downstream of condenser 16. In one embodiment, the controller 68 can be configured to process signals corresponding to measurement parameters (eg, the level of liquid in the condenser bin 22 as measured by the level controller 27). The controller 68 can be arranged to determine whether the liquid level measured by the level controller 27 is above or below a predetermined liquid level range of the condenser bin 22. If the liquid level measured in the condenser bin 22 is above or below the predetermined liquid level range of the condenser bin 22, the controller 68 can be configured to communicate via a communication line or wirelessly (not shown in FIG. 1) Adjusting the operation of one or more devices. For example, controller 68 may be configured to adjust the size of the opening of valve 25 when the liquid level measured in condenser bin 22 is above or below a predetermined liquid level range of condenser bin 22. Those skilled in the art recognize that the controller 68 or similar controller can be located remotely from the level controller 27 (eg, Also shown in FIG. 1 or may be located at level controller 27 and include level controller 27.
包含丙烯腈的液體物流26可從塔12的底部除 去。可將液體物流26通向產物塔(在圖1中未顯示)。或者,可將液體物流26通向乾燥塔,例如在包含頭餾分塔、乾燥塔和產物塔的3-塔純化系統中的乾燥塔。 A liquid stream 26 comprising acrylonitrile can be removed from the bottom of column 12 go with. Liquid stream 26 can be passed to the product column (not shown in Figure 1). Alternatively, liquid stream 26 can be passed to a drying column, such as a drying column in a 3-column purification system comprising a heads column, a drying column, and a product column.
圖4為根據應用於丙烯腈產物製造的本公開的方 面的一個備選實施方案的示意性流程圖。圖4與示於圖1的示意性流程圖類似。如在圖4中所示,流量控制器40與溫度控制器20和閥25電子連通。如在圖4中所示,流量控制器8與液位控制器27和閥9電子連通。 Figure 4 is a side view of the present disclosure applied to the manufacture of acrylonitrile products. A schematic flow diagram of an alternate embodiment of a face. Figure 4 is similar to the schematic flow diagram shown in Figure 1. As shown in FIG. 4, flow controller 40 is in electronic communication with temperature controller 20 and valve 25. As shown in FIG. 4, the flow controller 8 is in electronic communication with the level controller 27 and the valve 9.
像在圖1中那樣,在圖4中,控制器68可設置成處 理對應於測量參數(例如,通過溫度控制器20測量的溫度)的一個或多個信號。控制器68可設置成確定測量參數是高於還是低於預定的參數範圍,例如,通過溫度控制器20測量的溫度低於或高於預定的溫度範圍。如果測量的參數低於或高於預定的參數範圍,控制器68可設置成經由通訊線路或無線通訊(在圖4中未顯示)調節一個或多個裝置的操作。例如,當通過溫度控制器20測量的溫度低於或高於預定的溫度範圍時,控制器68可設置成調節流向頭餾分塔12的回流物流3的量。控制器68可設置成控制泵18的操作和/或閥9的操作和/或閥25的操作,例如控制閥9和/或閥25的開孔的尺寸。通過控制閥25的開孔的尺寸,控制器68控制否則可流經閥9的經過閥25的流量。本領域技術人員認識到, 控制器68或類似的控制器可位於遠離流量控制器8和流量控制器40(如在圖4中所示),或者可位於流量控制器8和/或流量控制器40處並且包括流量控制器8和/或流量控制器40。 As in Figure 1, in Figure 4, the controller 68 can be set up in place One or more signals corresponding to the measured parameters (eg, the temperature measured by temperature controller 20). The controller 68 can be arranged to determine whether the measured parameter is above or below a predetermined range of parameters, for example, the temperature measured by the temperature controller 20 is below or above a predetermined temperature range. If the measured parameter is below or above a predetermined parameter range, the controller 68 can be configured to adjust the operation of one or more devices via a communication line or wireless communication (not shown in Figure 4). For example, controller 68 may be configured to regulate the amount of reflux stream 3 flowing to heads column 12 when the temperature measured by temperature controller 20 is below or above a predetermined temperature range. Controller 68 may be arranged to control the operation of pump 18 and/or the operation of valve 9 and/or the operation of valve 25, such as the size of the opening of control valve 9 and/or valve 25. By controlling the size of the opening of the valve 25, the controller 68 controls the flow through the valve 25 that would otherwise flow through the valve 9. Those skilled in the art recognize that Controller 68 or similar controller may be located remote from flow controller 8 and flow controller 40 (as shown in Figure 4), or may be located at flow controller 8 and/or flow controller 40 and include a flow controller 8 and/or flow controller 40.
像在圖1中那樣,在圖4中,控制器68可設置成處理對應於測量參數(例如,通過液位控制器27測量的冷凝器料倉22中液體的液位)的信號。控制器68可設置成確定通過液位控制器27測量的液體液位是高於還是低於冷凝器料倉22的預定液體液位範圍。如果測量的參數低於或高於預定的參數範圍,控制器68可設置成經由通訊線路或無線通訊(在圖4中未顯示)調節一個或多個裝置的操作。例如,當通過液位控制器27測量的冷凝器料倉22中的液體液位低於或高於預定的液體液位範圍時,控制器68可設置成調節流向頭餾分塔12的回流物流3的量。控制器68可設置成控制泵18的操作和/或閥9的操作和/或閥25的操作,例如控制閥9和/或閥25的開孔的尺寸。通過控制閥9的開孔的尺寸,控制器68控制否則可流經閥25的經過閥9的流量。本領域技術人員認識到,控制器68或類似的控制器可位於遠離流量控制器8和流量控制器40(如在圖4中所示),或者可位於流量控制器8和/或流量控制器40處並且包括控制器8和/或流量控制器40 As in FIG. 1, in FIG. 4, controller 68 may be arranged to process signals corresponding to measurement parameters (eg, the level of liquid in condenser bin 22 as measured by level controller 27). The controller 68 can be arranged to determine whether the liquid level measured by the level controller 27 is above or below a predetermined liquid level range of the condenser bin 22. If the measured parameter is below or above a predetermined parameter range, the controller 68 can be configured to adjust the operation of one or more devices via a communication line or wireless communication (not shown in Figure 4). For example, when the liquid level in the condenser bin 22 as measured by the level controller 27 is below or above a predetermined liquid level range, the controller 68 can be configured to regulate the reflux stream 3 to the heads column 12 The amount. Controller 68 may be arranged to control the operation of pump 18 and/or the operation of valve 9 and/or the operation of valve 25, such as the size of the opening of control valve 9 and/or valve 25. By controlling the size of the opening of the valve 9, the controller 68 controls the flow through the valve 9 that would otherwise flow through the valve 25. Those skilled in the art recognize that controller 68 or a similar controller may be located remote from flow controller 8 and flow controller 40 (as shown in Figure 4), or may be located at flow controller 8 and/or flow controller 40 and includes controller 8 and/or flow controller 40
圖2說明根據本公開的方面的方法200的流程圖。方法200可使用前面描述的設備進行。在步驟201中,發生在包含多個塔板的頭餾分塔中接受粗品腈類原料流。在步驟201中,可在距頭餾分塔底部第38-第47個塔板的塔 板處發生在頭餾分塔中接受粗品腈類原料流。在步驟202中,發生在部分真空下在頭餾分塔中蒸餾粗品腈類原料流,以生產在頭餾分塔頂部的包含HCN的頭餾分塔塔頂物流以及在頭餾分塔底部的包含丙烯腈產物的底部液體物流。在步驟203中,發生在冷凝器中冷凝頭餾分塔塔頂物流。在步驟204中,在冷凝器中冷凝後,發生使用泵將至少一部分頭餾分塔塔頂物流作為回流物流泵送至頭餾分塔和/或泵送至HCN儲存、HCN使用者或處置中的至少一個。在步驟205中,發生在頭餾分塔中接受回流物流。如上所述,關於設備的本公開的各方面,在步驟205中,可在頭餾分塔的頂部塔板處發生在頭餾分塔中接受回流物流。 FIG. 2 illustrates a flow chart of a method 200 in accordance with aspects of the present disclosure. Method 200 can be performed using the apparatus described above. In step 201, a crude nitrile feed stream is received in a heads column comprising a plurality of trays. In step 201, a tower from the 38th to the 47th tray at the bottom of the heads column The plate takes place in the heads column to accept the crude nitrile feed stream. In step 202, a crude nitrile feed stream is distilled in a heads column under partial vacuum to produce a heads stream stream comprising HCN at the top of the heads column and an acrylonitrile product at the bottom of the heads column. The bottom liquid stream. In step 203, a condensation heads overhead stream is produced in the condenser. In step 204, after condensing in the condenser, at least a portion of the heads column overhead stream is pumped as a reflux stream to the heads column and/or pumped to the HCN storage, HCN user or treatment using a pump. One. In step 205, a reflux stream is received in the heads column. As noted above, with respect to aspects of the present disclosure of the apparatus, in step 205, a reflux stream can be received in the heads column at the top tray of the heads column.
方法200還可包括另外的步驟(在圖2中未顯示)。例如方法200還可包括在位於頭餾分塔的頂部塔板和接受粗品腈類原料流的塔板之間的預定塔板處測定流體的溫度的步驟。方法200還可包括調節通向頭餾分塔的回流物流的流量以保持流體在預定塔板處的溫度在預定的溫度範圍內的步驟。方法200還可包括控制冷凝器16的料倉22中冷凝的液體的液位在預定的液位範圍的步驟,並且該步驟可通過調節至少一個位於冷凝器16下游的閥而進行 Method 200 can also include additional steps (not shown in Figure 2). For example, the method 200 can further include the step of determining the temperature of the fluid at a predetermined tray between the top tray of the heads column and the tray receiving the crude nitrile feed stream. The method 200 can also include the step of adjusting the flow rate of the reflux stream to the heads column to maintain the temperature of the fluid at the predetermined tray within a predetermined temperature range. The method 200 can also include the step of controlling the level of liquid condensed in the silo 22 of the condenser 16 to be within a predetermined level range, and the step can be performed by adjusting at least one valve located downstream of the condenser 16
圖3說明根據本公開的方面的方法300的流程圖。方法300可與方法200類似。在步驟301中,發生在包含多個塔板的頭餾分塔中接受粗品腈類原料流。在步驟301中,在頭餾分塔中接受粗品腈類原料流可在距頭餾分塔底部第38-第47個塔板的塔板處發生。在步驟302中,發生在 部分真空下在頭餾分塔中蒸餾粗品腈類原料流,以生產在頭餾分塔頂部的包含HCN的頭餾分塔塔頂物流以及在頭餾分塔底部的包含丙烯腈產物的底部液體物流。在步驟303中,發生在冷凝器中冷凝頭餾分塔塔頂物流。在步驟304中,在冷凝器中冷凝後,發生將至少一部分頭餾分塔塔頂物流作為回流物流送至頭餾分塔和/或送至HCN儲存、HCN使用者或處置中的至少一個。將至少一部分頭餾分塔塔頂物流作為回流物流送至頭餾分塔可能包括或者可能不包括泵送回流物流。在步驟305中,發生在頭餾分塔中接受回流物流。如上所述,關於設備的本公開的各方面,在步驟305中,在頭餾分塔中接受回流物流可在頭餾分塔的頂部塔板處發生。 FIG. 3 illustrates a flow chart of a method 300 in accordance with aspects of the present disclosure. Method 300 can be similar to method 200. In step 301, a crude nitrile feed stream is received in a heads column comprising a plurality of trays. In step 301, the accepting of the crude nitrile feed stream in the heads column can occur at the trays from the 38th to the 47th trays at the bottom of the heads column. In step 302, what happens in The crude nitrile feed stream is distilled in a heads column under partial vacuum to produce a HCN-containing heads overhead stream at the top of the heads column and a bottoms liquid stream comprising the acrylonitrile product at the bottom of the heads column. In step 303, a condensation heads overhead stream is produced in the condenser. In step 304, after condensing in the condenser, at least one of the at least a portion of the heads column overhead stream is sent as a reflux stream to the heads column and/or to the HCN storage, HCN user or treatment. Feeding at least a portion of the heads column overhead stream as a reflux stream to the heads column may or may not include pumping the reflux stream. In step 305, a reflux stream is received in the heads column. As noted above, with respect to aspects of the present disclosure of the apparatus, in step 305, receiving a reflux stream in the heads column can occur at the top tray of the heads column.
方法300還可包括另外的步驟(在圖3中未顯 示)。例如方法300還可包括在第一預定塔板和第二預定塔板處測定流體的溫度的步驟,第一和第二預定塔板各自位於頭餾分塔的頂部塔板和接受粗品腈類原料流的塔板之間。方法300還可包括調節通向頭餾分塔的回流物流的流量以保持流體在第一預定塔板處的溫度在第一預定的溫度範圍內,以及調節回流物流的流量以保持流體在第二預定塔板處的溫度在第二預定的溫度範圍內的步驟。在一方面,第一預定的溫度範圍低於流體在第一預定溫度範圍將開始引起在第一預定塔板處污染的溫度。在一方面,第二預定的溫度範圍低於流體在第二預定溫度範圍將開始引起在第二預定塔板處污染的溫度。方法300還可包括將冷凝器16的 料倉22中冷凝的液體的液位控制在預定的液位範圍內的步驟,並且該步驟可通過調節至少一個位於冷凝器16下游的閥而進行。 Method 300 can also include additional steps (not shown in Figure 3) Show). For example, method 300 can further include the steps of determining the temperature of the fluid at the first predetermined tray and the second predetermined tray, each of the first and second predetermined trays being located at the top tray of the heads column and receiving the crude nitrile feed stream Between the trays. The method 300 can also include adjusting a flow rate of the reflux stream to the heads column to maintain the temperature of the fluid at the first predetermined tray within a first predetermined temperature range, and adjusting the flow of the reflux stream to maintain the fluid at the second predetermined The step of the temperature at the tray being within a second predetermined temperature range. In one aspect, the first predetermined temperature range is lower than a temperature at which the fluid will begin to cause contamination at the first predetermined tray in the first predetermined temperature range. In one aspect, the second predetermined temperature range is lower than a temperature at which the fluid will begin to cause contamination at the second predetermined tray in the second predetermined temperature range. Method 300 can also include the condenser 16 The level of liquid condensed in the silo 22 is controlled within a predetermined range of liquid levels, and this step can be performed by adjusting at least one valve located downstream of the condenser 16.
雖然在前面的說明書中已關於其某些優選的實施方案描述了本公開,並且就說明的目的,已描述許多細節,對於本領域技術人員來說顯而易見的是,本公開容許另外的實施方案,並且在不偏離本公開的基本原則的情況下,本文描述的某些細節可顯著變化。應理解的是,在不偏離本公開的精神和範圍或不偏離申請專利範圍的情況下,本公開的特徵容許修改、變化、改變或替代。例如,各部件的尺寸、數量、大小和形狀可改變,以適應具體的應用。因此,本文說明和描述的具體實施方案僅出於說明的目的。 Although the present disclosure has been described in connection with certain preferred embodiments thereof, and the details of the invention have been described, it will be apparent to those skilled in the art that And certain details described herein may vary significantly without departing from the basic principles of the disclosure. It is to be understood that the features of the present disclosure are susceptible to modifications, variations, alterations, and substitutions, without departing from the spirit and scope of the disclosure. For example, the size, number, size, and shape of the various components can be varied to suit a particular application. Accordingly, the specific embodiments illustrated and described herein are for illustrative purposes only.
1‧‧‧粗品腈類原料流 1‧‧‧ crude nitrile feedstock
2‧‧‧頭餾分塔塔頂物流 2‧‧‧ head fractionation tower top logistics
3‧‧‧回流物流 3‧‧‧Return Logistics
4‧‧‧水流 4‧‧‧Water flow
5‧‧‧HCN副產物物流 5‧‧‧HCN by-product logistics
6‧‧‧冷凝器出口物流 6‧‧‧Condenser export logistics
7‧‧‧接點 7‧‧‧Contacts
8‧‧‧控制器、流量控制器 8‧‧‧Controller, flow controller
9‧‧‧閥、控制閥 9‧‧‧Valves, Control Valves
12‧‧‧頭餾分塔 12‧‧‧ heads tower
14‧‧‧塔頂系統 14‧‧‧Tower System
16‧‧‧冷凝器 16‧‧‧Condenser
18‧‧‧無密封墊的泵、控制泵 18‧‧‧No gasket pump, control pump
20‧‧‧溫度控制器 20‧‧‧ Temperature Controller
22‧‧‧料倉、冷凝器料倉 22‧‧‧ silo, condenser silo
25‧‧‧閥、產物閥 25‧‧‧Valve, product valve
26‧‧‧液體物流 26‧‧‧Liquid Logistics
27‧‧‧液位控制器 27‧‧‧Level controller
28‧‧‧塔板、頂部塔板 28‧‧‧Tray, top tray
30‧‧‧頂部塔板 30‧‧‧Top tray
32‧‧‧中間塔板 32‧‧‧Intermediate tray
34‧‧‧底部 34‧‧‧ bottom
68‧‧‧控制器 68‧‧‧ Controller
Claims (32)
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??201410107192.6 | 2014-03-21 | ||
CN201410107192.6A CN104922926A (en) | 2014-03-21 | 2014-03-21 | Head fraction tower tower-top system |
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TW201544156A true TW201544156A (en) | 2015-12-01 |
TWI639461B TWI639461B (en) | 2018-11-01 |
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TW104109003A TWI639461B (en) | 2014-03-21 | 2015-03-20 | Heads column overhead system |
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CN (1) | CN104922926A (en) |
EA (1) | EA036895B8 (en) |
TW (1) | TWI639461B (en) |
WO (1) | WO2015142718A1 (en) |
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CN114870421A (en) * | 2015-11-16 | 2022-08-09 | 英尼奥斯欧洲股份公司 | Head fraction column pump cycle |
CN105366692B (en) * | 2015-12-04 | 2018-03-30 | 中国天辰工程有限公司 | A kind of high purity liquid HCN and system |
EP3604222A1 (en) * | 2018-07-30 | 2020-02-05 | Evonik Operations GmbH | Process for the purification of hydrogen cyanide |
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US3044966A (en) | 1959-08-05 | 1962-07-17 | Standard Oil Co | Attrition resistant oxidation catalysts |
US3196085A (en) * | 1962-02-12 | 1965-07-20 | Du Pont | Process for purifying acrylonitrile |
US3198750A (en) | 1962-12-26 | 1965-08-03 | Standard Oil Co | Mixed antimony oxide-uranium oxide oxidation catalyst |
US3352764A (en) | 1966-05-02 | 1967-11-14 | Standard Oil Co | Absorption and distillation process for separating crude unsaturated nitriles from acetonitrile with selective solvent recycle |
US4234510A (en) | 1973-06-07 | 1980-11-18 | Standard Oil Company | Recovery of acrylonitrile or methacrylonitrile by condensation |
US3885928A (en) | 1973-06-18 | 1975-05-27 | Standard Oil Co Ohio | Acrylonitrile and methacrylonitrile recovery and purification system |
CN1016404B (en) * | 1988-06-06 | 1992-04-29 | 天津大学 | Rectification of mixts. with high freezing pt. and installation thereof |
US6107509A (en) | 1999-03-31 | 2000-08-22 | The Standard Oil Company | Process for the recovery of acrylonitrile and methacrylontrile |
JP4430788B2 (en) * | 2000-06-02 | 2010-03-10 | 株式会社日本触媒 | Distillation tower startup method |
DE10046609A1 (en) * | 2000-09-20 | 2002-04-04 | Basf Ag | Method and device for the separation of C5 + cuts by distillation |
CN1220660C (en) * | 2002-12-10 | 2005-09-28 | 扬子石油化工股份有限公司 | Intelligent control method for ethylene rectifying tower of ethylene equipment |
CN101549211B (en) * | 2009-04-21 | 2011-07-20 | 西安交通大学 | Energy-saving and modification method for heat pump distillation and device thereof |
JP5605921B2 (en) * | 2010-12-27 | 2014-10-15 | 旭化成ケミカルズ株式会社 | Purification method of acrylonitrile |
CN202289528U (en) * | 2011-10-11 | 2012-07-04 | 浙江大学宁波理工学院 | Rectification experimental apparatus capable of safely showing flooding phenomenon in plate tower |
CN204246864U (en) * | 2014-03-21 | 2015-04-08 | 英尼奥斯欧洲股份公司 | Head fraction column overhead system |
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EA036895B8 (en) | 2021-02-16 |
EA036895B1 (en) | 2021-01-12 |
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