US20120234516A1 - Energy recovery from mother liquid in paraxylene crystallization process - Google Patents

Energy recovery from mother liquid in paraxylene crystallization process Download PDF

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Publication number
US20120234516A1
US20120234516A1 US13/423,507 US201213423507A US2012234516A1 US 20120234516 A1 US20120234516 A1 US 20120234516A1 US 201213423507 A US201213423507 A US 201213423507A US 2012234516 A1 US2012234516 A1 US 2012234516A1
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United States
Prior art keywords
heat exchanger
mother liquor
crystallizer
energy
providing
Prior art date
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Abandoned
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US13/423,507
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English (en)
Inventor
Weihua Jin
Zhongyi Ding
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Sulzer GTC Technology US Inc
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GTC Technology US LLC
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Priority to US13/423,507 priority Critical patent/US20120234516A1/en
Assigned to GTC TECHNOLOGY US LLC reassignment GTC TECHNOLOGY US LLC ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: DING, ZHONGYI, JIN, WEIHUA
Publication of US20120234516A1 publication Critical patent/US20120234516A1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C15/00—Cyclic hydrocarbons containing only six-membered aromatic rings as cyclic parts
    • C07C15/02—Monocyclic hydrocarbons
    • C07C15/067—C8H10 hydrocarbons
    • C07C15/08—Xylenes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0004—Crystallisation cooling by heat exchange
    • B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • C07C7/14—Purification; Separation; Use of additives by crystallisation; Purification or separation of the crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D15/00—Heat-exchange apparatus with the intermediate heat-transfer medium in closed tubes passing into or through the conduit walls ; Heat-exchange apparatus employing intermediate heat-transfer medium or bodies
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals

Definitions

  • the claimed invention is directed to methods for recovering energy from a mother liquor stream in paraxylene crystallization processes.
  • the energy from the mother liquor is optimally utilized to reduce the refrigeration burden on the crystallization process.
  • Xylene isomers ortho-xylene (OX), meta-xylene (MX), and para-xylene (PX), and ethylbenzene (EB) are C8 aromatics from a reforming process or other petrochemical processes.
  • OX ortho-xylene
  • MX meta-xylene
  • PX para-xylene
  • EB ethylbenzene
  • MX meta-xylene
  • EB ethylbenzene
  • PX terephthalic acid
  • DMT dimethyl terephthalate
  • PX fibers, films and polyethylene terephthalate
  • PX crystallization is carried out at a temperature just above the eutectic point, which is about ⁇ 50° C. to about ⁇ 70° C. for an equilibrium xylene mixture feed.
  • the equilibrium of PX in C8 aromatics liquid (mother liquor) limits the efficiency of the crystallization process.
  • the solid PX crystals are typically separated from the mother liquor by filtration or centrifugation.
  • the mother liquor is separated from PX solid at low temperature.
  • the mother liquor from the process contains significant amount of refrigeration duty due to its low temperature and high flow rate.
  • This invention is related to the efficient energy recovery from the mother liquid in this low temperature crystallization process.
  • methods for recovering energy from mother liquor in paraxylene crystallization process comprise: 1) providing a crystallizer or heat exchanger to recover energy from low temperature mother liquor; 2) providing a second heat exchanger to recovery energy from intermediate temperature mother liquor; 3) providing a third heat exchanger to recovery energy from high temperature mother liquor.
  • the feed stream is the media on the other side of the heat exchangers/crystallizers that carries the energy, and the feed stream is cooled down by the mother liquor.
  • One option is to have a fourth heat exchanger for the feed stream between the first crystallizer/heat exchanger and second heat exchanger to further optimize the energy recovery.
  • FIG. 1 shows an illustrative energy recovery system from mother liquor
  • FIG. 2 shows an illustrative energy recovery system from mother liquor with an optional fourth heat exchanger between first crystallizer and second heat exchanger.
  • the main energy consumption is from the refrigeration station compressors, which are used to provide the low temperature refrigerant duty to cool the feed streams to desired temperature. It is desirable to minimize the refrigeration duty by recovering energy from different streams within the crystallization unit before discharge.
  • the lowest operating temperature is limited by the eutectic point, which is between ⁇ 50° C. and ⁇ 70° C.
  • the mother liquor is at this temperature before discharge. Because the equilibrium xylene feed contains only about 20% PX, the quantity of the mother liquor is significant. Therefore, there is significant amount of low temperature refrigeration duty available in the mother liquor. The optimum recovery of the energy from the mother liquor improves the energy efficiency of the process.
  • An embodiment of the invention is directed to a method for recovering energy from a mother liquor in a PX crystallization process, the method comprising providing a feed stream to a PX crystallization unit; providing a first crystallizer or heat exchanger to recover low temperature energy from low temperature mother liquor; providing a second heat exchanger to recovery energy from intermediate temperature mother liquor; providing a third heat exchanger to recovery energy from high temperature mother liquor; wherein the feed stream to the PX crystallization unit is cooled down by the energy extracted from the mother liquor.
  • Crystallizers or crystallization units are based on the use of vertical vessel, scraped-surface crystallizers, and wash columns.
  • the crystallizers create a slurry of high-purity para-xylene crystals in a mother liquor. This slurry is fed to wash columns where the crystals are separated from the mother liquor, and melted for the final product.
  • the low temperature mother liquor temperature is from ⁇ 50° C. to ⁇ 70° C.
  • the crystallizer is a screw type crystallizer, scrape surface crystallizer, or part of the crystallizer in the main PX crystallization section.
  • the crystallizer can be a single crystallizer, or multiple crystallizers operated in serial or in parallel.
  • the heat exchanger can be a shell/tube type heat exchanger, or more advantageously a double pipe heat exchanger.
  • a further embodiment of the invention is directed to a method for recovering energy from a mother liquor in PX crystallization process by providing a first crystallizer or heat exchanger to recover energy from low temperature mother liquor; providing a second heat exchanger to recovery energy from intermediate temperature mother liquor; providing a third heat exchanger to recovery energy from high temperature mother liquor; and providing a fourth heat exchanger to further reduce the temperature of feed stream, wherein the feed stream to the PX crystallization unit is cooled down by the energy extracted from the mother liquor.
  • a heat exchanger may be used to cool a feed stream.
  • the energy of mother liquor is first recovered in a first crystallizer or heat exchanger 101 .
  • the crystallizer can be a screw type crystallizer, or scrape surface crystallizer, or part or a portion of the crystallizers in the crystallization section shown in FIG. 1 . It can also be multiple crystallizers operated in serial or in parallel.
  • the reason to use a crystallizer is that when the temperature drops below the PX freezing point and PX crystals are formed, it is necessary to remove the crystals continuously to prevent the accumulation of solid that may cause plugging of the equipment.
  • mother liquor is warmed up from ⁇ 63° C. to ⁇ 54° C.
  • Mother liquor from 101 is further warmed up in a second heat exchanger 102 to recover additional energy for cooling the feed stream.
  • 102 can be a regular shell/tube type heat exchanger, or more advantageously a double pipe heat exchanger to minimize the equipment plugging problems.
  • Mother liquor from 102 is further warmed up in a third heat exchanger 103 to about 35° C. as illustrated in the example before exit from the PX crystallization process.
  • This warm stream is ready to be processed in the down stream units, such as a xylene isomerization unit.
  • Feed stream is cooled down from 40° C. to about ⁇ 17° C. in 103 as illustrated in the example. The energy from mother liquor is thus fully recovered.
  • a fourth heat exchanger 104 is introduced between the first crystallizer 101 and a second heat exchanger 102 .
  • the addition of the fourth heat exchanger is to utilize a high temperature energy source so that the energy from the mother liquor can be better utilized.
  • the shift of a high temperature energy source from a low temperature energy source means the overall refrigeration station power is decreased.
  • the cooling media for 104 can be a refrigerant from the refrigeration station, or other suitable media.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Water Supply & Treatment (AREA)
  • Combustion & Propulsion (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
US13/423,507 2011-03-18 2012-03-19 Energy recovery from mother liquid in paraxylene crystallization process Abandoned US20120234516A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US13/423,507 US20120234516A1 (en) 2011-03-18 2012-03-19 Energy recovery from mother liquid in paraxylene crystallization process

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201161454337P 2011-03-18 2011-03-18
US13/423,507 US20120234516A1 (en) 2011-03-18 2012-03-19 Energy recovery from mother liquid in paraxylene crystallization process

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US20120234516A1 true US20120234516A1 (en) 2012-09-20

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US13/423,507 Abandoned US20120234516A1 (en) 2011-03-18 2012-03-19 Energy recovery from mother liquid in paraxylene crystallization process

Country Status (9)

Country Link
US (1) US20120234516A1 (ja)
EP (1) EP2686096A4 (ja)
JP (1) JP2014523797A (ja)
KR (1) KR101984770B1 (ja)
CN (2) CN103596670A (ja)
BR (1) BR112013023933A2 (ja)
RU (1) RU2604225C2 (ja)
TW (1) TW201240966A (ja)
WO (1) WO2012129155A1 (ja)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018217327A1 (en) * 2017-05-23 2018-11-29 Exxonmobil Chemical Patents Inc. Systems and methods for deep crystallization of xylene streams

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103880586B (zh) * 2012-12-19 2015-09-09 中国石油化工股份有限公司 对二甲苯的多级结晶方法
CN108905263A (zh) * 2018-07-13 2018-11-30 连云港康乐药业有限公司 一种扑热息痛细晶的生产方法

Citations (15)

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US2659763A (en) * 1950-09-16 1953-11-17 California Research Corp Xylene separation
US2778864A (en) * 1951-04-07 1957-01-22 Exxon Research Engineering Co Process for separating pure para xylene by complexing with antimony trichloride
US2827503A (en) * 1953-05-01 1958-03-18 Standard Oil Co Recovery of para-xylene from solutions containing the xylene isomers
US2866833A (en) * 1953-09-14 1958-12-30 Standard Oil Co Paraxylene purification system
US3119771A (en) * 1960-07-27 1964-01-28 Phillips Petroleum Co Desalting aqueous salt solutions by the formation of hydrocarbon hydrates and the purification thereof
US3177265A (en) * 1961-05-22 1965-04-06 Standard Oil Co Process for the recovery of paraxylene
US3364691A (en) * 1962-06-25 1968-01-23 Phillips Petroleum Co Crystallization
US3499946A (en) * 1966-09-01 1970-03-10 Mitsubishi Gas Chemical Co Method for separating m- and p-xylene from a mixture of xylenes
US3558731A (en) * 1968-09-18 1971-01-26 Shell Oil Co Paraxylene crystallization
US3916018A (en) * 1973-03-26 1975-10-28 Atlantic Richfield Co Separation of paraxylene
US4004886A (en) * 1969-12-12 1977-01-25 Stamicarbon B.V. Two stage continuous process and apparatus for crystallization
US4039617A (en) * 1975-06-17 1977-08-02 Allied Chemical Corporation Recovery of soda values and heat from sodium carbonate crystallizer purge liquors
US5329061A (en) * 1993-06-01 1994-07-12 Uop Crystallization process for para-xylene recovery using two-stage recovery section
US6565653B2 (en) * 2001-05-08 2003-05-20 Bp Corporation North America Inc. Energy efficient process for producing high purity paraxylene
US7857396B2 (en) * 2008-06-17 2010-12-28 Pinnacle Potash International, Ltd. Method and system for solution mining

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US2795634A (en) * 1953-05-01 1957-06-11 Standard Oil Co Recovery of ortho-and para-xylenes from c8 aromatic mixtures
GB1080360A (en) * 1965-07-20 1967-08-23 Ici Ltd Improvements in and relating to crystallisation processes
DE2509182A1 (de) * 1974-03-11 1975-10-02 Standard Oil Co Einstufiges kristallisationsverfahren zur gewinnung von hochgereinigtem p-xylol
JPH08208561A (ja) * 1994-11-16 1996-08-13 Mitsubishi Chem Corp テレフタル酸の製造方法
JPH10120601A (ja) * 1996-10-23 1998-05-12 Mitsubishi Chem Corp パラキシレンの分離方法
RU2221755C2 (ru) * 2002-04-01 2004-01-20 Сукманский Олег Борисович Способ получения неорганического бурового реагента и установка для его осуществления

Patent Citations (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2659763A (en) * 1950-09-16 1953-11-17 California Research Corp Xylene separation
US2778864A (en) * 1951-04-07 1957-01-22 Exxon Research Engineering Co Process for separating pure para xylene by complexing with antimony trichloride
US2827503A (en) * 1953-05-01 1958-03-18 Standard Oil Co Recovery of para-xylene from solutions containing the xylene isomers
US2866833A (en) * 1953-09-14 1958-12-30 Standard Oil Co Paraxylene purification system
US3119771A (en) * 1960-07-27 1964-01-28 Phillips Petroleum Co Desalting aqueous salt solutions by the formation of hydrocarbon hydrates and the purification thereof
US3177265A (en) * 1961-05-22 1965-04-06 Standard Oil Co Process for the recovery of paraxylene
US3364691A (en) * 1962-06-25 1968-01-23 Phillips Petroleum Co Crystallization
US3499946A (en) * 1966-09-01 1970-03-10 Mitsubishi Gas Chemical Co Method for separating m- and p-xylene from a mixture of xylenes
US3558731A (en) * 1968-09-18 1971-01-26 Shell Oil Co Paraxylene crystallization
US4004886A (en) * 1969-12-12 1977-01-25 Stamicarbon B.V. Two stage continuous process and apparatus for crystallization
US3916018A (en) * 1973-03-26 1975-10-28 Atlantic Richfield Co Separation of paraxylene
US4039617A (en) * 1975-06-17 1977-08-02 Allied Chemical Corporation Recovery of soda values and heat from sodium carbonate crystallizer purge liquors
US5329061A (en) * 1993-06-01 1994-07-12 Uop Crystallization process for para-xylene recovery using two-stage recovery section
US6565653B2 (en) * 2001-05-08 2003-05-20 Bp Corporation North America Inc. Energy efficient process for producing high purity paraxylene
US7857396B2 (en) * 2008-06-17 2010-12-28 Pinnacle Potash International, Ltd. Method and system for solution mining

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018217327A1 (en) * 2017-05-23 2018-11-29 Exxonmobil Chemical Patents Inc. Systems and methods for deep crystallization of xylene streams
US11332422B2 (en) 2017-05-23 2022-05-17 Exxonmobil Chemical Patents Inc. Systems and methods for deep crystallization of xylene streams

Also Published As

Publication number Publication date
EP2686096A4 (en) 2014-09-10
KR101984770B1 (ko) 2019-05-31
RU2604225C2 (ru) 2016-12-10
KR20140016335A (ko) 2014-02-07
WO2012129155A1 (en) 2012-09-27
CN111454117A8 (zh) 2020-10-02
TW201240966A (en) 2012-10-16
CN103596670A (zh) 2014-02-19
CN111454117A (zh) 2020-07-28
JP2014523797A (ja) 2014-09-18
EP2686096A1 (en) 2014-01-22
BR112013023933A2 (pt) 2016-12-13
RU2013144438A (ru) 2015-04-27

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