WO2012129155A1 - Energy recovery from mother liquid in paraxylene crystallization process - Google Patents
Energy recovery from mother liquid in paraxylene crystallization process Download PDFInfo
- Publication number
- WO2012129155A1 WO2012129155A1 PCT/US2012/029621 US2012029621W WO2012129155A1 WO 2012129155 A1 WO2012129155 A1 WO 2012129155A1 US 2012029621 W US2012029621 W US 2012029621W WO 2012129155 A1 WO2012129155 A1 WO 2012129155A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- heat exchanger
- mother liquor
- crystallizer
- energy
- providing
- Prior art date
Links
Classifications
-
- 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
-
- 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
- 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
- the melting points of PX, MX, OX, and EB are 13.3 °C, - 47.9 °C, -25.2 °C, and -95.0 °C respectively, and the system does not form solid solutions above the eutectic temperature.
- the crystals are essentially pure PX.
- Several commercial crystallization processes have been developed to separate PX from its isomer mixture. PX crystals are typically produced in two or more crystallization stages, with PX recovery of about 60-65% per pass. In commercial practice, 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.
- 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;
- Crystallizers or crystallization units are based on the use of vertical vessel
- 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 the low temperature mother liquor
- 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. In the example illustrated in FIG.
- mother liquor is warmed up from -63 °C to -54 °C in 101, and the feed stream is cooled down from -35 °C to -40 °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.
- FIG. 2 which is similar to the method illustrated in FIG. 1 except 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.
Abstract
Description
Claims
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP12760638.2A EP2686096A4 (en) | 2011-03-18 | 2012-03-19 | Energy recovery from mother liquid in paraxylene crystallization process |
CN201280014294.2A CN103596670A (en) | 2011-03-18 | 2012-03-19 | Energy recovery from mother liquid in paraxylene crystallization process |
RU2013144438/05A RU2604225C2 (en) | 2011-03-18 | 2012-03-19 | Heat exchange using mother liquid in para-xylene crystallization process |
BR112013023933A BR112013023933A2 (en) | 2011-03-18 | 2012-03-19 | energy recovery of the mother liquor in the paraxylene crystallization process |
KR1020137027183A KR101984770B1 (en) | 2011-03-18 | 2012-03-19 | Energy recovery from mother liquid in paraxylene crystallization process |
JP2013558231A JP2014523797A (en) | 2011-03-18 | 2012-03-19 | Energy recovery from mother liquor of para-xylene crystallization process |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US201161454337P | 2011-03-18 | 2011-03-18 | |
US61/454,337 | 2011-03-18 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2012129155A1 true WO2012129155A1 (en) | 2012-09-27 |
Family
ID=46827530
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US2012/029621 WO2012129155A1 (en) | 2011-03-18 | 2012-03-19 | Energy recovery from mother liquid in paraxylene crystallization process |
Country Status (9)
Country | Link |
---|---|
US (1) | US20120234516A1 (en) |
EP (1) | EP2686096A4 (en) |
JP (1) | JP2014523797A (en) |
KR (1) | KR101984770B1 (en) |
CN (2) | CN111454117A (en) |
BR (1) | BR112013023933A2 (en) |
RU (1) | RU2604225C2 (en) |
TW (1) | TW201240966A (en) |
WO (1) | WO2012129155A1 (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103880586B (en) * | 2012-12-19 | 2015-09-09 | 中国石油化工股份有限公司 | The multistage crystallization method of p-Xylol |
US11332422B2 (en) | 2017-05-23 | 2022-05-17 | Exxonmobil Chemical Patents Inc. | Systems and methods for deep crystallization of xylene streams |
CN108905263A (en) * | 2018-07-13 | 2018-11-30 | 连云港康乐药业有限公司 | A kind of production method of paracetamol fine grain |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3558731A (en) * | 1968-09-18 | 1971-01-26 | Shell Oil Co | Paraxylene crystallization |
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 |
Family Cites Families (18)
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 |
US2795634A (en) * | 1953-05-01 | 1957-06-11 | Standard Oil Co | Recovery of ortho-and para-xylenes from c8 aromatic mixtures |
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 |
NL125644C (en) * | 1961-05-22 | |||
US3364691A (en) * | 1962-06-25 | 1968-01-23 | Phillips Petroleum Co | Crystallization |
GB1080360A (en) * | 1965-07-20 | 1967-08-23 | Ici Ltd | Improvements in and relating to crystallisation processes |
US3499946A (en) * | 1966-09-01 | 1970-03-10 | Mitsubishi Gas Chemical Co | Method for separating m- and p-xylene from a mixture of xylenes |
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 |
DE2509182A1 (en) * | 1974-03-11 | 1975-10-02 | Standard Oil Co | ONE-STAGE CRYSTALLIZATION PROCESS FOR THE RECOVERY OF HIGHLY PURIFIED P-XYLOL |
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 |
JPH08208561A (en) * | 1994-11-16 | 1996-08-13 | Mitsubishi Chem Corp | Production of terephthalic acid |
JPH10120601A (en) * | 1996-10-23 | 1998-05-12 | Mitsubishi Chem Corp | Separation of para-xylene |
RU2221755C2 (en) * | 2002-04-01 | 2004-01-20 | Сукманский Олег Борисович | Method to produce inorganic boring reagent and installation for its implementation |
-
2012
- 2012-03-16 TW TW101109178A patent/TW201240966A/en unknown
- 2012-03-19 CN CN202010186803.6A patent/CN111454117A/en active Pending
- 2012-03-19 WO PCT/US2012/029621 patent/WO2012129155A1/en active Application Filing
- 2012-03-19 EP EP12760638.2A patent/EP2686096A4/en not_active Withdrawn
- 2012-03-19 CN CN201280014294.2A patent/CN103596670A/en active Pending
- 2012-03-19 KR KR1020137027183A patent/KR101984770B1/en active IP Right Grant
- 2012-03-19 BR BR112013023933A patent/BR112013023933A2/en not_active IP Right Cessation
- 2012-03-19 US US13/423,507 patent/US20120234516A1/en not_active Abandoned
- 2012-03-19 JP JP2013558231A patent/JP2014523797A/en active Pending
- 2012-03-19 RU RU2013144438/05A patent/RU2604225C2/en active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3558731A (en) * | 1968-09-18 | 1971-01-26 | Shell Oil Co | Paraxylene crystallization |
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 |
Non-Patent Citations (1)
Title |
---|
See also references of EP2686096A4 * |
Also Published As
Publication number | Publication date |
---|---|
RU2013144438A (en) | 2015-04-27 |
RU2604225C2 (en) | 2016-12-10 |
CN111454117A (en) | 2020-07-28 |
EP2686096A1 (en) | 2014-01-22 |
EP2686096A4 (en) | 2014-09-10 |
CN111454117A8 (en) | 2020-10-02 |
KR20140016335A (en) | 2014-02-07 |
US20120234516A1 (en) | 2012-09-20 |
BR112013023933A2 (en) | 2016-12-13 |
TW201240966A (en) | 2012-10-16 |
KR101984770B1 (en) | 2019-05-31 |
CN103596670A (en) | 2014-02-19 |
JP2014523797A (en) | 2014-09-18 |
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