WO2015142718A1 - Heads column overhead system - Google Patents

Heads column overhead system Download PDF

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Publication number
WO2015142718A1
WO2015142718A1 PCT/US2015/020709 US2015020709W WO2015142718A1 WO 2015142718 A1 WO2015142718 A1 WO 2015142718A1 US 2015020709 W US2015020709 W US 2015020709W WO 2015142718 A1 WO2015142718 A1 WO 2015142718A1
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WO
WIPO (PCT)
Prior art keywords
heads column
stream
tray
heads
column
Prior art date
Application number
PCT/US2015/020709
Other languages
English (en)
French (fr)
Inventor
Timothy Robert Mcdonel
Jay Robert COUCH
David Rudolph Wagner
Paul Trigg Wachtendorf
Original Assignee
Ineos Europe Ag
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ineos Europe Ag filed Critical Ineos Europe Ag
Priority to EA201691899A priority Critical patent/EA036895B8/ru
Publication of WO2015142718A1 publication Critical patent/WO2015142718A1/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C253/00Preparation of carboxylic acid nitriles
    • C07C253/32Separation; Purification; Stabilisation; Use of additives
    • C07C253/34Separation; Purification

Definitions

  • the invention relates to an improved process for the manufacture of acrylonitrile and methacrylonitrile.
  • the invention is directed to improved heads column overhead treatment of hydrogen cyanide (HCN).
  • U.S. Pat. Nos. 4,234,510; 3,885,928; 3,352,764; 3,198,750 and 3,044,966 are illustrative of typical recovery and purification processes for acrylonitrile and methacrylonitrile.
  • the acrylonitrile manufacturing process produces HCN co-product that is very toxic.
  • An approach is to use gravity flow to eliminate the need for pumps in HCN service.
  • fouling, particularly of trays, is often a problem in acrylonitrile plant HCN or heads columns.
  • an aspect of the disclosure is to provide a safe, effective and cost effective method and apparatus that overcomes or reduces the disadvantages of conventional processes.
  • the apparatus comprises a heads column and an overhead system.
  • the heads column is configured to receive a crude nitriles feed stream.
  • the heads column is configured to distill the crude nitriles feed stream while operating under a partial vacuum and produce a heads column overhead stream comprising HCN at the top of the heads column, and a bottom liquid stream comprising acrylonitrile product at the bottom of the heads column.
  • the overhead system comprises a condenser that is configured to condense the heads column overhead stream.
  • the apparatus comprises a glandless pump. The pump is configured to pump at least a portion of the heads column overhead stream after the heads column overheard stream is condensed in the condenser.
  • FIG. 1 is a schematic flow diagram of an embodiment in accordance with aspects of the disclosure as applied to the manufacture of acrylonitrile product.
  • FIG. 2 illustrates a flow diagram of a method in accordance with aspects of the disclosure.
  • FIG. 3 illustrates a flow diagram of a method in accordance with aspects of the disclsoure.
  • FIG. 4 is a schematic flow diagram of an alternative embodiment in accordance with aspects of the disclosure as applied to the manufacture of acrylonitrile product.
  • the recovery section of an acrylonitrile plant produces a crude nitriles feed stream, which is a mixture comprising acrylonitrile, HCN, and water.
  • a processing step in acrylonitrile purification is the removal of HCN co-product by distillation.
  • the distillation column that removes HCN from the crude nitriles feed stream is known as the HCN column, the heads column, or the heads drying column. Using this distillation column, HCN may be recovered as a high purity overhead product.
  • a glandless pump e.g., a magnetically coupled pump and/or a pump with no direct connection between the motor shaft and the impeller
  • a glandless pump By using a glandless pump, the risk of HCN leakage may be minimized because this type of pump has no drive seal that can leak and there is no heat transfer from the motor to the pumped fluid.
  • Apparatus 10 is downstream of a recovery column (not shown in FIG. 1) used in an acrylonitrile manufacturing process.
  • Apparatus 10 comprises a heads column 12 and an overhead system 14.
  • Heads column 12 is configured to distill the crude nitriles feed stream 1 and produce a heads column overhead stream 2, comprised mostly of HCN with trace amounts of acrylonitrile and water.
  • Crude nitriles feed stream 1 may include about 82 to about 90 weight percent acrylonitrile, and about 5 to about 13 weight percent HCN, with the balance of the composition being water.
  • components that may cause fouling will be dependent upon the types of inhibitors utilized.
  • Overhead system 14 comprises a condenser 16 that is configured to condense the heads column overhead stream 2.
  • Overhead system 14 comprises a glandless pump 18.
  • heads column 12 may be configured to distill crude nitriles feed stream 1 while operating under a partial vacuum.
  • heads column 12 may be configured to distill crude nitriles feed stream 1 while operating under a partial vacuum in the range of 0.044-0.090 MPa absolute.
  • heads column 12 distills crude nitriles feed stream 1 under a partial vacuum with a top pressure of about 0.075MPa absolute.
  • Fluid in heads column 12 may be heated by a spare reboiler (not shown in FIG. 1) that may be common for heating fluid in both the heads column 12 and fluid in the product column (not shown in FIG. 1) that is downstream of the heads column 12.
  • Lean water may be used as the heat source for the reboiler(s).
  • Heads column 12 comprises a plurality of trays. In an embodiment, heads column 12 comprises between fifty-two (52) and seventy-two (72) trays. In an embodiment, heads column 12 comprises sixty-two (62) trays. Heads column 12 may be configured to receive crude nitriles feed stream 1 at tray 28. In an embodiment, tray 28 may be the forty-second tray from the bottom of heads column 12. In an alternative embodiment, tray 28 may be the thirty-eighth tray from the bottom of heads column 12. In an alternative embodiment, tray 28 may be the forty-seventh tray from the bottom of heads column 12, and heads column 12 may comprise sixty-seven (67) trays. In an embodiment, the first through twenty bottom trays of heads column 12 dry the acrylonitrile product.
  • the twenty-first through forty-second tray from bottom 34 of heads column 12 remove and purify HCN.
  • heads column 12 may be operated without drying function.
  • heads column 12 comprises between forty (40) and sixty-five (65) trays.
  • feed tray 28 may be between and including the twentieth and thirtieth tray from the bottom of the heads column.
  • Condenser 16 may be configured to receive cooled or refrigerated water (RW) stream 4. Refrigerated water stream 4 may comprise antifreeze and have an inlet temperature to condenser 16 of about -10 to 5 degrees Celsius. In an aspect, condenser 16 may be located near heads column 12, but not at the top of heads column 12. Condenser 16 may be configured, including an appropriate size, to accommodate the lower temperatures required for operation of heads column 12 under partial vacuum. Lower temperatures for operation of heads column 12 may be in the range of -10 to +10 degrees Celsius.
  • Glandless pump 18 may be used to pump condenser outlet stream 6 from condenser 16, comprised mostly of HCN. Condenser outlet stream 6 may split at junction 7 into reflux stream 3 and HCN co-product stream 5. In an aspect, HCN co-product stream 5 may be sent to HCN users, HCN storage, or disposal.
  • Reflux stream 3 may flow to heads column 12. The system may utilize a reflux ratio of about 2 to about 7, in another aspect, about 2 to about 6.5, and in another aspect, about 3 to about 6. In an aspect, reflux stream 3 may be received in the top tray 30 of heads column 12. In an embodiment, top tray 30 of heads column 12 may be the sixty- second tray from the bottom of heads column 12.
  • the flow of reflux stream 3 may be adjusted by a flow controller 8 that is configured to adjust a valve 9.
  • Flow controller 8 may be controlled by a temperature controller 20.
  • Temperature controller 20 may be located at an intermediate tray 32 of heads column 12 that is below top tray 30 of heads column 12.
  • controller 68 may be configured to process one or more signals corresponding to a measured parameter, e.g., the temperature measured by temperature controller 20.
  • Controller 68 may be configured to determine whether the measured parameter is above or below a predetermined parameter range, e.g., the temperature measured by temperature controller 20 is below or above a predetermined temperature range.
  • Controller 68 may be configured to adjust operation of one or more devices via communication lines or wireless communications (not shown in FIG.
  • controller 68 may be configured to adjust 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 configured to control operation of pump 18 and/or operation of valve 9, such as controlling the size of the opening of valve 9. Those skilled in the art will 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 and comprise flow controller 8.
  • Condenser 16 may comprise a condenser boot 22, and level controller 27.
  • Level controller 27 may be configured to control the level of condensed liquid in condenser boot 22. As shown in FIG. 1 , level controller 27 may be configured to control the level of condensed liquid in condenser boot 22 by adjusting the opening of product valve 25. As shown in FIG. 1, valve 25 may be located downstream of condenser 16.
  • controller 68 may be configured to process a signal corresponding to a measured parameter, e.g., the level of liquid in condenser boot 22 as measured by level controller 27. Controller 68 may be configured to determine whether the liquid level as measured by level controller 27 is above or below a predetermined liquid level range for condenser boot 22.
  • Controller 68 may be configured to adjust operation of one or more devices via communication lines or wireless communications (not shown in FIG. 1) if the measured liquid level in condenser boot 22 is above or below the predetermined liquid level range for condenser boot 22.
  • controller 68 may be configured to adjust the size of the opening of valve 25 when the measured liquid level in condenser boot 22 is above or below the predetermined liquid level range for condenser boot 22.
  • controller 68 or a similar controller may be located remote from level controller 27 (as shown in FIG. 1), or may be located at and comprise level controller 27.
  • Liquid stream 26 comprising acrylonitrile may be removed from the bottom of column 12.
  • Liquid stream 26 may be passed to a product column (not shown in FIG. 1).
  • liquid stream 26 may 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.
  • FIG. 4 is a schematic flow diagram of an alternative embodiment in accordance with aspects of the disclosure as applied to the manufacture of acrylonitrile product.
  • FIG. 4 is similar to the schematic flow diagram shown in FIG. 1.
  • flow controller 40 is in electronic communication with temperature controller 20 and valve 25.
  • flow controller 8 is in electronic communication with level controller 27 and valve 9.
  • controller 68 may be configured to process one or more signals corresponding to a measured parameter, e.g., the temperature measured by temperature controller 20. Controller 68 may be configured to determine whether the measured parameter is above or below a predetermined parameter range, e.g., the temperature measured by temperature controller 20 is below or above a predetermined temperature range. Controller 68 may be configured to adjust operation of one or more devices via communication lines or wireless communications (not shown in FIG. 4) if the measured parameter is below or above a predetermined parameter range. For example, controller 68 may be configured to adjust 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 configured to control operation of pump 18 and/or operation of valve 9 and/or operation of valve 25, such as controlling the size of the opening of valve 9 and/or valve 25. By controlling the size of the opening of valve 25, controller 68 controls the flow through valve 25 that otherwise may flow through valve 9.
  • controller 68 or a similar controller may be located remote from flow controller 8 and flow controller 40 (as shown in FIG. 4), or may be located at and comprise flow controller 8 and/or flow controller 40.
  • controller 68 may be configured to process a signal corresponding to a measured parameter, e.g., the level of liquid in condenser boot 22 as measured by level controller 27. Controller 68 may be configured to determine whether the liquid level as measured by level controller 27 is above or below a predetermined liquid level range for condenser boot 22. Controller 68 may be configured to adjust operation of one or more devices via communication lines or wireless communications (not shown in FIG. 4) if the measured parameter is below or above a predetermined parameter range. For example, controller 68 may be configured to adjust the amount of reflux stream 3 flowing to heads column 12 when the liquid level in condenser boot 22 measured by level controller 27 is below or above a predetermined liquid level range.
  • Controller 68 may be configured to control operation of pump 18 and/or operation of valve 9 and/or operation of valve 25, such as controlling the size of the opening of valve 9 and/or valve 25. By controlling the size of the opening of valve 9, controller 68 controls the flow through valve 9 that otherwise may flow through valve 25.
  • controller 68 or a similar controller may be located remote from flow controller 8 and flow controller 40 (as shown in FIG. 4), or may be located at and comprise flow controller 8 and/or flow controller 40.
  • FIG. 2 illustrates a flow diagram of a method 200 in accordance with aspects of the disclosure.
  • Method 200 may be carried out using apparatus previously described.
  • step 201 receiving a crude nitriles feed stream in a heads column comprising a plurality of trays occurs.
  • step 201 the receiving the crude nitriles feed stream in the heads column may occur at a tray that is in the range of the thirty-eighth to the forty-seventh tray from the bottom of the heads column.
  • step 202 distilling the crude nitriles feed stream in the heads column under a partial vacuum to produce a heads column overhead stream comprising HCN at the top of the heads column, and a bottom liquid stream comprising acrylonitrile product at the bottom of the heads column occurs.
  • step 203 condensing the heads column overhead stream in a condenser occurs.
  • step 204 after being condensed in the condenser, pumping at least a portion of the heads column overhead stream using a pump to the heads column as a reflux stream and/or to at least one of HCN storage, a user of HCN, or disposal occurs.
  • step 205 receiving the reflux stream in the heads column occurs. As noted above regarding aspects of the disclosure of apparatus, in step 205, the receiving the reflux stream in the heads column may occur at the top tray of the heads column.
  • Method 200 may further comprise additional steps (not shown in FIG. 2).
  • method 200 may further comprise a step of determining the temperature of fluid at a predetermined tray located between the top tray and the tray receiving the crude nitriles feed stream of the heads column.
  • Method 200 may further comprise a step of adjusting the flow of the reflux stream to the heads column to maintain the temperature of fluid at the predetermined tray within a predetermined temperature range.
  • Method 200 may further comprise a step of controlling the level of condensed liquid in boot 22 of condenser 16 within a predetermined level range, and this step may performed by adjusting at least one valve located downstream of condenser 16.
  • FIG. 3 illustrates a flow diagram of a method 300 in accordance with aspects of the disclosure.
  • Method 300 may be similar to method 200.
  • step 301 receiving a crude nitriles feed stream in a heads column comprising a plurality of trays occurs.
  • the receiving the crude nitriles feed stream in the heads column may occur at a tray that is in the range of the thirty-eighth to the forty- seventh tray from the bottom of the heads column.
  • step 302 distilling the crude nitriles feed stream in the heads column under a partial vacuum to produce a heads column overhead stream comprising HCN at the top of the heads column, and a bottom liquid stream comprising acrylonitrile product at the bottom of the heads column occurs.
  • step 303 condensing the heads column overhead stream in a condenser occurs.
  • step 304 after being condensed in the condenser, sending at least a portion of the heads column overhead stream to the heads column as a reflux stream and/or to at least one of HCN storage, a user of HCN, or disposal occurs.
  • the sending at least a portion of the heads column overhead stream to the heads column as a reflux stream may or may not include pumping of the reflux stream.
  • step 305 receiving the reflux stream in the heads column occurs. As noted above regarding aspects of the disclosure of apparatus, in step 305, the receiving the reflux stream in the heads column may occur at the top tray of the heads column.
  • Method 300 may further comprise additional steps (not shown in FIG. 3). For example method 300 may further comprise a step of determining the temperature of fluid at a first predetermined tray and a second predetermined tray, the first and second predetermined trays each located between the top tray and the tray receiving the crude nitriles feed stream of the heads column. Method 300 may further comprise a step of adjusting the flow of the reflux stream to the heads column to maintain the temperature of fluid at the first predetermined tray within a first predetermined temperature range and adjusting the flow of the reflux stream to maintain the temperature of fluid at the second predetermined tray within a second predetermined temperature range.
  • the first predetermined temperature range is below a temperature at which the fluid at the first predetermined temperature range would begin to cause fouling at the first predetermined tray.
  • Method 300 may further comprise a step of controlling the level of condensed liquid in boot 22 of condenser 16 within a predetermined level range, and this step may performed by adjusting at least one valve located downstream of condenser 16.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
PCT/US2015/020709 2014-03-21 2015-03-16 Heads column overhead system WO2015142718A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EA201691899A EA036895B8 (ru) 2014-03-21 2015-03-16 Система верхнего погона колонны головного погона

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201410107192.6 2014-03-21
CN201410107192.6A CN104922926A (zh) 2014-03-21 2014-03-21 头馏分塔塔顶系统

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EA (1) EA036895B8 (zh)
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Cited By (3)

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CN105366692A (zh) * 2015-12-04 2016-03-02 中国天辰工程有限公司 一种制取高纯液态氰化氢工艺及系统
EP3604222A1 (en) * 2018-07-30 2020-02-05 Evonik Operations GmbH Process for the purification of hydrogen cyanide
RU2800707C2 (ru) * 2018-07-30 2023-07-26 Эвоник Оперейшенс ГмбХ Способ очистки цианистого водорода

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CN106699599A (zh) * 2015-11-16 2017-05-24 英尼奥斯欧洲股份公司 头馏分塔泵循环

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Publication number Priority date Publication date Assignee Title
CN105366692A (zh) * 2015-12-04 2016-03-02 中国天辰工程有限公司 一种制取高纯液态氰化氢工艺及系统
EP3604222A1 (en) * 2018-07-30 2020-02-05 Evonik Operations GmbH Process for the purification of hydrogen cyanide
WO2020025322A1 (en) * 2018-07-30 2020-02-06 Evonik Operations Gmbh Process for the purification of hydrogen cyanide
KR20210034658A (ko) * 2018-07-30 2021-03-30 에보니크 오퍼레이션즈 게엠베하 시안화수소의 정제 방법
JP2021533064A (ja) * 2018-07-30 2021-12-02 エボニック オペレーションズ ゲーエムベーハー シアン化水素の精製方法
RU2800707C2 (ru) * 2018-07-30 2023-07-26 Эвоник Оперейшенс ГмбХ Способ очистки цианистого водорода
JP7413350B2 (ja) 2018-07-30 2024-01-15 エボニック オペレーションズ ゲーエムベーハー シアン化水素の精製方法
US11939281B2 (en) 2018-07-30 2024-03-26 Evonik Operations Gmbh Process for the purification of hydrogen cyanide
KR102670277B1 (ko) 2018-07-30 2024-05-30 에보니크 오퍼레이션즈 게엠베하 시안화수소의 정제 방법

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Publication number Publication date
EA036895B8 (ru) 2021-02-16
TW201544156A (zh) 2015-12-01
EA036895B1 (ru) 2021-01-12
CN104922926A (zh) 2015-09-23
TWI639461B (zh) 2018-11-01
EA201691899A1 (ru) 2017-02-28

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