WO2018171028A1 - Pta精制单元母液的回收利用方法 - Google Patents

Pta精制单元母液的回收利用方法 Download PDF

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WO2018171028A1
WO2018171028A1 PCT/CN2017/084350 CN2017084350W WO2018171028A1 WO 2018171028 A1 WO2018171028 A1 WO 2018171028A1 CN 2017084350 W CN2017084350 W CN 2017084350W WO 2018171028 A1 WO2018171028 A1 WO 2018171028A1
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Prior art keywords
stage
enters
flash
condensate
solvent
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PCT/CN2017/084350
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English (en)
French (fr)
Inventor
赵旭
申涛
王天宝
张万尧
路原睿
徐立龙
贾敏
韩东钊
谢晓玲
邱永宁
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天华化工机械及自动化研究设计院有限公司
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Priority to ES17901568T priority Critical patent/ES2886591T3/es
Priority to JP2019512993A priority patent/JP6672527B2/ja
Priority to EP17901568.0A priority patent/EP3505498B1/en
Priority to EA201991146A priority patent/EA201991146A1/ru
Priority to US16/330,230 priority patent/US10787411B2/en
Publication of WO2018171028A1 publication Critical patent/WO2018171028A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
    • C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/007—Energy recuperation; Heat pumps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/06—Flash distillation
    • B01D3/065—Multiple-effect flash distillation (more than two traps)
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/08—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in rotating vessels; Atomisation on rotating discs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/02—Treatment of water, waste water, or sewage by heating
    • C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/06—Flash evaporation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F2001/5218—Crystallization
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/34—Organic compounds containing oxygen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00—General aspects of water treatment
    • C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C63/00—Compounds having carboxyl groups bound to a carbon atoms of six-membered aromatic rings
    • C07C63/14—Monocyclic dicarboxylic acids
    • C07C63/15—Monocyclic dicarboxylic acids all carboxyl groups bound to carbon atoms of the six-membered aromatic ring
    • C07C63/26—1,4 - Benzenedicarboxylic acid
    • 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 invention relates to a method for recycling and recycling a mother liquid of a PTA refining unit, and more particularly relates to a method for recovering waste heat of a mother liquid of a PTA refining unit and a PT acid in a PTA industrial device, and is also suitable for low temperature waste heat recovery of waste water in other industries.
  • PT p-methylbenzoic acid
  • TA terephthalic acid
  • the temperature of the wastewater can be as high as 140 ⁇ 150 ° C
  • the current industry mainly uses a refined exhaust gas scrubbing system to treat it
  • the high temperature PTA mother liquor from the device first enters the atmospheric pressure flash tower, the high temperature mother liquor in the tower Flashing occurs
  • steam generated by flashing is discharged into the environment together with non-condensed steam such as H 2 and N 2 from the top of the atmospheric pressure flashing tower, and the mother liquor produced by flashing is cooled by air cooling, after cooling.
  • the PTA mother liquor is re-entered into a subsequent membrane processing system for use.
  • the object of the present invention is to provide a PTA mother liquor waste heat and PT acid recovery method by adopting an efficient multi-stage flashing technology, a low temperature waste heat power generation technology, a heat pump heating and cooling system.
  • Technology, low-temperature crystallization technology, etc. to achieve efficient multi-stage utilization of PTA mother liquor heat, through which the heat recovery of PTA mother liquor can be realized, and the shortcomings of existing industrial devices can be solved.
  • the invention provides a method for recycling and recycling a mother liquor of a PTA refining unit, comprising the following steps:
  • Multi-stage flash cooling step the PTA refining unit mother liquor enters the high efficiency multi-stage flash column (1), the high efficiency multi-stage flash column (1) comprises at least an N-stage flashing stage in which the high efficiency multi-stage flashing tower
  • the mother liquor of the PTA refining unit described in (1) is subjected to N-1 flashing;
  • the N-stage flashing section of the high efficiency multi-stage flash column (1) is a flash cooling section, the flash cooling section does not flash, and the flash cooling section is located at the N-2 stage flashing stage. Between the segment and the N-1 flash zone;
  • Residual heat utilization step the flash vapor generated by the first stage flash stage to the M stage flash stage enters the waste heat utilization unit;
  • PT acid crystallization recovery step the mother liquid produced in the N-1 stage flash stage enters the low temperature crystallization unit, and the PT acid crystal in the mother liquid of the PTA refining unit is recovered;
  • waste heat utilization unit preferably comprises a first waste heat utilization unit and a second waste heat utilization unit
  • the first waste heat utilization unit is preferably: a heating unit and/or a refrigeration unit into which the primary flash steam generated by the first stage flashing stage enters;
  • the second waste heat utilization unit is preferably a power generation unit into which the flash steam generated by the second stage flash stage to the M stage flash stage enters.
  • the heating unit preferably has the following steps:
  • the working fluid condensate is heated and evaporated by the first-stage flash steam from another part, and the condensed first-stage flash steam condensate enters into three
  • the vapor of the working fluid evaporated by heating enters into the heating absorber (24), and the concentrated lithium bromide solution is in an unsaturated state in the heating absorber (24), thereby transferring the working fluid vapor.
  • the refrigeration unit specifically takes the following steps:
  • the working fluid condensate entering the refrigerating evaporator (25) is evaporated under the action of low-temperature water heating, and the vapor generated by the evaporation enters into the refrigeration absorber (26), and the lithium bromide concentrated solution is in the refrigeration absorber. (26) is in an unsaturated state, so that the working fluid vapor is absorbed, and a large amount of heat released during the absorption process is cooled by the cooling circulating water, and the low temperature water after heat exchange in the refrigerating evaporator (25) is cooled, thereby obtaining Lower temperature chilled water;
  • the chilled water produced by the refrigerating evaporator (25) partially enters the air heat exchanger (36), cools the air at the inlet of the air compressor, and the chilled water after the heat exchange enters the chilled water buffer tank (37). And it is sent to the refrigeration evaporator (25) for recycling through the chilled water transfer pump (38), and another part of the chilled water enters the high efficiency multi-stage flash tower (1), and the flash steam is cooled.
  • the power generating unit specifically takes the following steps:
  • the second stage flash stage to the M stage flash stage are each connected with a heat exchanger, and each heat exchanger is connected in series at the same time, so that the steam generated by the high efficiency multistage flash tower (1) can be Gasification of the solvent in the heat exchanger;
  • the flash steam from the M-stage flash zone is indirectly exchanged with the solvent from the solvent transfer pump (8) in the primary heat exchanger connected thereto, and the vapor condensate after the heat exchange is discharged to the first stage.
  • the solvent heated by the previous step enters the lower heat exchanger in series with the primary heat exchanger, and the steam condensate after the heat exchange is discharged into the primary condensate buffer tank (9);
  • the vaporized solvent vapor enters the steam turbine (5) and pushes the steam turbine to work for power generation.
  • the solvent vapor after the work is then introduced into the solvent condenser (6), and the solvent condensate generated by the condensation enters the solvent buffer tank (7). And then transported to the primary heat exchanger by the solvent transfer pump (8), thereby completing the cycle of converting the residual heat of the PTA mother liquor into electrical energy;
  • the condensate in the primary condensate buffer tank (9) is transported to the subsequent system by the primary condensate transfer pump (10).
  • the low temperature crystallization unit specifically has the following steps:
  • the N-2 stage flash zone in the high efficiency multi-stage flash column (1) is connected to a venturi ejector (12); the Nth stage flash in the high efficiency multi-stage flash column (1)
  • the section is a flash cooling section and is connected with a secondary condensate transfer pump (13);
  • the mother liquor produced in the flash stage of the N-1 stage enters the crystallization tank (15), and the PT acid is crystallized and precipitated in a large amount in the crystallization tank (15).
  • the liquid remaining in the crystallization tank containing a small amount of solid impurities is in the primary mother liquid transfer pump (16). Under the action of pressure, it enters a plurality of filters in series, the solid particles are intercepted and discharged through the bottom of the filter, and the filtered mother liquid enters into the mother liquid buffer tank (19), and is in the secondary mother liquid transfer pump. (20) enters the venturi ejector (12), condenses the flash steam from the N-2 stage flash zone, and condenses the condensate in the secondary condensate transfer pump (13) Transfer to the subsequent membrane processing system.
  • N is preferably 8
  • M is preferably 4.
  • the method for recovering and using the PTA refining unit mother liquid according to the present invention wherein the temperature of the PTA refining unit mother liquid is preferably 140 to 150 °C.
  • the method for recycling the mother liquid of the PTA refining unit according to the present invention wherein the mass concentration of the lithium bromide dilute solution is preferably 56% to 60%, and the mass concentration of the potassium bromide concentrated solution is preferably 60% to 64%.
  • the method for recycling the mother liquid of the PTA refining unit according to the present invention wherein the plurality of filters connected in series are preferably a primary filter (17), a secondary filter (18) connected in series, and the plurality of serially connected A filter cloth is preferably provided in the filter.
  • the mother liquid of the PTA refining unit enters the high-efficiency multi-stage flash column (1), the multi-stage flashing of the PTA refining unit mother liquid occurs, and the first-stage flashing stage (I) performs a first-stage flashing, and the generated flash steam enters.
  • the first-stage flashed condensate enters the secondary flash zone (II) for secondary flashing, and the flash steam generated by flashing enters the tertiary heat exchanger (2);
  • the second-stage flashed condensate enters the third-stage flash stage (III) for three-stage flashing, and the flash steam generated by flashing enters the secondary heat exchanger (3);
  • the third-stage flashing condensate enters the fourth-stage flashing stage (IV) for four-stage flashing, and the flash steam generated by flashing enters the first-stage heat exchanger (4);
  • the four-stage flashed condensate enters the fifth-stage flash stage (V) for five-stage flashing, and the flash steam generated by flashing enters the steam condenser (11) and condenses and condenses in the action of circulating cooling water. After the steam condensate enters the subsequent system;
  • the five-stage flashed condensate enters the six-stage flash stage (VI), and the flash steam generated by flashing enters the venturi ejector (12);
  • the condensate after the sixth stage flashing enters the seventh-stage flash stage (VII), and the flash steam generated by the flashing is condensed by the chilled water, and the condensed flash condensate is in the third-stage condensate transfer pump (14).
  • the chilled water buffer tank (37) used as hydration water for the preparation of chilled water;
  • the solvent heated by the primary heat exchanger (4) enters the secondary heat exchanger (3), and the steam condensate after the heat exchange is discharged into the primary condensate buffer tank (9);
  • the solvent heated by the secondary heat exchanger (3) enters the tertiary heat exchanger (2), the solvent is vaporized, and the steam condensate after the heat exchange is discharged into the primary condensate buffer tank (9) in;
  • the vaporized solvent vapor enters the steam turbine (5) and pushes the steam turbine to work for power generation.
  • the solvent vapor after the work is then introduced into the solvent condenser (6), and the solvent condensate generated by the condensation enters the solvent buffer tank (7). And then transported to the primary heat exchanger (4) by the solvent transfer pump (8), thereby completing the cycle of converting the residual heat of the PTA mother liquor into electrical energy;
  • the condensate in the primary condensate buffer tank (9) is transported to the subsequent system by the primary condensate transfer pump (10);
  • the PTA mother liquor after flashing through the seventh-stage flashing section (VII) enters the crystallization tank (15), and the PT acid is crystallized in a large amount in the crystallization tank (15), and the remaining liquid containing a small amount of solid impurities after crystallization is
  • the primary mother liquid transfer pump (16) is pressed into the plurality of series filters in sequence, the solid particles are intercepted, and discharged through the bottom of the filter, and the filtered mother liquid enters the mother liquid buffer tank (19), and Under the action of the secondary mother liquor transfer pump (20), it enters the venturi ejector (12), and the flash steam from the six-stage flash zone (VI) is condensed, and the condensed condensate is condensed in the second stage.
  • the liquid transfer pump (13) is transported to the subsequent membrane processing system;
  • One-stage flash steam from the high-efficiency multi-stage flash column (1) a part of which enters into the generator (21), the lithium bromide solution is heated and evaporated, and the steam condensate after heat exchange enters the third-stage condensate
  • the vapor generated by the evaporation enters into the condenser (22) and is condensed by the circulating cooling water, and the working fluid condensate generated by the condenser enters the heating evaporator through the working fluid circulation pump.
  • the working fluid condensate is heated and evaporated by the first-stage flash steam from another part, and the condensed first-stage flash steam condensate enters the third stage.
  • the heated vaporized working medium vapor enters the heating absorber (24), and the lithium bromide concentrated solution is in an unsaturated state in the heating absorber (24), thereby performing the working fluid vapor.
  • Absorption a large amount of heat is released during the absorption process, and the condensate from the fourth-stage condensate transfer pump (35) enters the heating absorber (24) and is heated, and the heated condensate enters the secondary condensation.
  • the liquid buffer tank (34) where flashing occurs, generating medium and low pressure steam, and entering the subsequent system Use
  • the working fluid condensate entering the refrigeration evaporator (25) is evaporated under the action of low temperature water heating, and the vapor of the working fluid vaporized enters into the refrigeration absorber (26), and the lithium bromide concentrated solution is in the refrigeration absorber.
  • (26) is in an unsaturated state, so that the working fluid vapor is absorbed, and a large amount of heat released during the absorption process is cooled by the cooling circulating water, and the low temperature water after heat exchange in the refrigerating evaporator (25) is cooled, thereby obtaining Lower temperature chilled water;
  • the chilled water produced by the refrigerating evaporator (25) partially enters the air heat exchanger (36), cools the air at the inlet of the air compressor, and the chilled water after the heat exchange enters the chilled water buffer tank (37) ), and is circulated to the refrigerating evaporator (25) through the chilled water transfer pump (38), and another part of the chilled water enters the high-efficiency multi-stage flash tower (1) and cools the seven-stage flash steam. .
  • a PTA refining unit mother liquor waste heat and PT acid recovery method the specific steps are as follows:
  • a PTA mother liquor from a certain upstream temperature enters the high-efficiency multi-stage flash tower 1 first, where the PTA mother liquor is first-stage flashed in the first-stage flashing section I, and the flash steam generated by flashing enters to occur.
  • the first-stage flashed condensate enters the secondary flash section II of the high-efficiency multi-stage flash tower 1, where the PTA mother liquor undergoes secondary flashing, flashing
  • the flash steam enters the third-stage heat exchanger 2;
  • the second-stage flashed condensate enters the third-stage flash stage III, where the PTA mother liquor undergoes a three-stage flash, and the flash steam generated by the flash enters
  • the secondary heat exchanger 3 the condensate after the third-stage flashing enters the fourth-stage flashing section IV, where the PTA mother liquor undergoes a four-stage flashing, and the flash steam generated by the flashing enters the primary heat exchanger 4; the condensate after the fourth
  • the action of water is condensed, and the condensed steam condensate enters the subsequent system; the condensate after the fifth-stage flashing enters the sixth-stage flash stage VI, The PTA mother liquor undergoes a six-stage flashing, and the flash steam generated by the flashing gas enters the venturi ejector 12; the condensed liquid after the sixth-stage flashing enters the seventh-stage flashing section VII, where the PTA mother liquor occurs seven.
  • the flashing steam generated by the flashing is condensed by the action of the chilled water, and the condensed flash condensate enters the chilled water buffer tank 37 by the action of the tertiary condensate transfer pump 14 to prepare the frozen Water hydration use.
  • the flash steam from the fourth stage flash stage IV is indirectly exchanged with the solvent from the solvent delivery pump 8 (using the R245fa solvent) in the primary heat exchanger 4, where the solvent is heated to a certain temperature,
  • the steam condensate after heat exchange is discharged into the primary condensate buffer tank 9;
  • the solvent heated by the primary heat exchanger 4 enters the secondary heat exchanger 3, where the solvent and the flash from the third stage
  • the flash steam of paragraph III undergoes indirect heat exchange, the solvent is further heated, and the steam condensate after heat exchange is discharged into the primary condensate buffer tank 9;
  • the solvent heated by the secondary heat exchanger 3 enters three In the heat exchanger 2, here, the solvent exchanges indirect heat with the flash steam from the secondary flash zone II, the solvent is vaporized, and the vapor condensate after the heat exchange is discharged into the primary condensate buffer tank.
  • the vaporized solvent vapor enters the steam turbine 5, and pushes the steam turbine to work for power generation, and the solvent vapor after the work is subsequently introduced into the solvent condenser 6, and is condensed by the cooling circulating water to condense the solvent.
  • the condensate enters the solvent buffer tank 7, and is transported by the solvent transfer pump 8. In a heat exchanger 4, thereby completing the cycle of the heat recovery portion into electrical energy in the PTA mother liquor.
  • the condensate in the primary condensate buffer tank 9 is transported to the subsequent system by the primary condensate transfer pump 10.
  • the PTA mother liquor after flashing in the seventh-stage flashing zone VII enters the crystallization tank 15. Since the temperature of the PTA mother liquor is low at this time, the PT acid is crystallized in a large amount in the crystallizing tank 15, and a small amount of solid impurities remain after crystallization.
  • the liquid enters the primary filter 17 and the secondary filter 18 in sequence under the action of the primary mother liquid delivery pump 16, and the filter is provided with a filter cloth, etc., and the solid particles are intercepted and passed through the bottom of the filter.
  • the discharged, filtered mother liquor enters the mother liquor buffer tank 19 and enters the venturi ejector 12 under the action of the secondary mother liquor transfer pump 20, where the flash steam from the six-stage flash zone VI is taken. Condensation is carried out, and the condensed condensate is transferred to the subsequent membrane processing system by the secondary condensate transfer pump 13.
  • d is from the first-stage flash steam in the high-efficiency multi-stage flash column 1, and a part of it enters the generator 21, where the lithium bromide solution at a certain concentration is heated and evaporated, and the steam condensate after the heat exchange enters the third stage.
  • the vapor generated by the evaporation enters the condenser 22 and is condensed by the circulating cooling water, and the working fluid condensate generated by the condenser enters the heating evaporator 23 through the working fluid circulation pump and In the refrigerating evaporator 25, in the heating evaporator, the working fluid condensate is heated and evaporated by the first-stage flash steam from another portion, and the condensed first-stage flash steam condensate enters the third-stage condensate buffer tank 39.
  • the heated vaporized working medium vapor enters the heating absorber 24, and the lithium bromide concentrated solution is in an unsaturated state in the heating absorber 24, thereby absorbing the working fluid vapor, and releasing a large amount of heat during the absorption process.
  • the condensate from the fourth-stage condensate transfer pump 35 enters the heating absorber 24 and is heated, and the heated condensate enters the secondary condensate buffer tank 34 where it is flashed to generate a certain temperature. Medium and low pressure steam, The system proceeds to subsequent use.
  • e enters the working fluid condensate in the refrigerating evaporator 25, and evaporates under the action of low-temperature water heating, and the vapor of the working fluid vaporized enters into the refrigerating absorber 26, and the concentrated lithium bromide solution is unsaturated in the refrigerating absorber 26.
  • the state is such that the working fluid vapor is absorbed, and a large amount of heat released during the absorption process is cooled by the cooling circulating water, and the low-temperature water after the heat exchange in the refrigerating evaporator 25 is cooled, thereby obtaining a chilled water having a lower temperature.
  • the chilled water generated by the refrigerating evaporator 25 is partially introduced into the air heat exchanger 36, and the air of the air compressor inlet is cooled, and the chilled water after the heat exchange enters the chilled water buffer tank 37 and passes through the chilled water.
  • the transfer pump 38 is sent to the refrigerating evaporator 25 for recycling, and the other portion of the chilled water enters the high efficiency multi-stage flash column 1 and cools the seven-stage flash steam.
  • the degree of vacuum of the system is maintained by the primary vacuum pump 41, the secondary vacuum pump 42, and the tertiary vacuum pump 43.
  • the invention uses the steam discharged into the environment to be comprehensively utilized in stages, and uses the waste heat in part of the PTA mother liquor for power generation, high-quality steam and chilled water to realize heat recovery.
  • low temperature crystallization technology is used to recover PT acid crystals in the PTA mother liquor, which reduces the influence of PT acid crystal on the subsequent system, and can provide crystallized process water to the subsequent membrane treatment system, and solves the membrane treatment system. Easy to block the problem.
  • the mother liquor treatment method provided by the invention not only has less equipment investment, but also can directly generate electricity by side by-product, and generate high-quality steam utilization, and the generated chilled water is used for cooling the air entering the air compressor, which is greatly reduced.
  • the power consumption of the air compressor reduces the operating cost of the PTA unit. Therefore, the mother liquor treatment method provided by the present invention can generate enormous economic benefits.
  • the mother liquor of the PTA refining unit at a temperature of 140-150 ° C first enters the first-stage flashing section I of the high-efficiency multi-stage flash column 1 and is decompressed and flashed in the PTA mother liquor, and the flashing produces about 100 ° C.
  • the saturated steam enters the subsequent generator 21 and the heating evaporator 23; the flashed 100 ° C PTA mother liquor enters the secondary flash zone II, and decompression flashing occurs, and flashing occurs.
  • the steam is in direct contact heat exchange with the chilled water from the refrigerating evaporator 25, the saturated steam is condensed, and the condensed condensate enters the chilled water buffer tank 37 by the action of the tertiary condensate transfer pump.
  • the circulating solvent is R245fa, and the saturated steam from 70°C in the fourth-stage flashing stage IV enters the primary heat exchanger 4, and performs indirect heat exchange with the solvent from the solvent transfer pump 8.
  • the solvent is heated to 55-60 ° C, and the steam condensate after the heat exchange enters into the primary condensate buffer tank 9; the solvent heated by the primary heat exchanger 4 enters the secondary heat exchanger 3, Therefore, indirect heat exchange with the saturated steam from about 80 ° C in the third-stage flash zone III, the solvent is heated to 65-70 ° C, and the steam condensate after the heat exchange enters the first-stage condensate buffer tank 9;
  • the solvent heated by the secondary heat exchanger 3 enters the tertiary heat exchanger 2, where indirect heat exchange with the saturated steam from about 90 ° C in the secondary flash zone II, the solvent is evaporated, resulting in The solvent vapor at 75 to 85 ° C enters the primary condensate buffer tank 9 after the heat exchange.
  • the solvent vapor of 75-85 °C enters the steam turbine 5, and pushes the steam turbine to work for power generation.
  • the solvent vapor after work is about 45-50 ° C, and enters the solvent condenser 6, which is condensed by circulating cooling water, after condensation
  • the solvent condensate enters the solvent buffer tank 7 and enters the primary heat exchanger 4 under the action of the solvent circulation pump 8, thereby completing the cycle of low-temperature waste heat power generation.
  • the steam condensate in the primary condensate buffer tank 9 is delivered to the subsequent system by the primary condensate transfer pump 10.
  • the PTA mother liquor from 25 ° C in the seven-stage flash zone VII enters the crystallization tank 15, where the PT acid in the PTA mother liquor is largely crystallized, and the crystallized PTA mother liquor is subsequently transferred to the primary mother liquor transfer pump 16 Under the action, it enters the primary filter 17 and the secondary filter 18 in sequence, and removes the solid impurities contained in the PTA mother liquor.
  • the filtered PTA mother liquor enters the mother liquor buffer tank 19 and enters through the secondary mother liquor delivery pump 20.
  • the PTA mother liquor at 25 ° C condenses the 40 ° C saturated steam in the six-stage flash zone VI, and the resulting condensate enters the flash cooling section VIII, and Under the action of the condensate transfer pump, it enters the subsequent membrane treatment system (the VIII is located between the VI and the VII, the flash does not occur in this section, and the other seven stages are flashed).
  • the working fluid vapor enters the condenser 22, and the working fluid vapor exchanges indirect heat with the cooling circulating water to obtain a steam condensate of about 40 ° C, that is, the working fluid condensate, which passes through A part of the working fluid circulation pump enters into the heating evaporator 23, and a part enters into the refrigeration evaporator 25.
  • the working fluid condensate evaporates at a temperature of 100 ° C, and evaporation yields about 90.
  • the working fluid vapor of °C in order to ensure the smooth progress of the evaporation, the working fluid condensate is forcedly circulated and evaporated by the secondary working fluid circulation pump 31, and the working fluid vapor generated by the heating evaporator 23 enters the heating absorber 24,
  • the concentration of the lithium bromide solution is 60% to 64%, and the lithium bromide solution is in an unsaturated state, so that the working fluid vapor can be absorbed.
  • the working fluid vapor releases a large amount of heat from the four-stage condensate transfer pump.
  • the condensate in 35 enters the heating absorber 24, and absorbs the released heat, and the temperature of the condensate rises to 135-140 ° C, and then the heated condensate enters the secondary condensate buffer tank 34 and occurs Flashing, generating about 130 ° C of saturated steam into the subsequent system utilization, 56% ⁇ 60% of the lithium bromide solution after the generator 21 is evaporated, producing 60% ⁇ 64% lithium bromide solution, and in the role of the first-stage lithium bromide circulation pump 29 Enter In the first-stage solvent heat exchanger 27, 60% to 64% of the lithium bromide solution generates 56% to 60% of the lithium bromide solution after the heating absorber absorbs the working fluid vapor, and enters the first-stage solvent heat exchanger 27, Here, indirect heat exchange is performed with the lithium bromide solution from the generator to complete the heating process of the heat pump.
  • the 40°C working fluid condensate entering the refrigerating evaporator 25 absorbs the heat of the low-temperature water of about 15° C. from the chilled water transfer pump 38, and the working fluid condensate is evaporated to generate a working fluid vapor of 5° C.
  • the working fluid condensate is forced to circulate and evaporate through the three-stage working fluid circulation pump 32, and the chilled water of 5 to 10 ° C is generated by the low temperature water of 15 ° C after absorbing heat, resulting in 5
  • the working medium vapor of °C enters the refrigeration absorber 26, where the lithium bromide solution having a concentration of 60% to 64% absorbs the working medium vapor, and the heat released during the absorption process is cooled by circulating cooling water and absorbed.
  • the subsequent 56% to 60% lithium bromide solution is indirectly exchanged with the 60 to 64% potassium bromide solution from the evaporator 21 in the secondary solvent exchanger 28 to complete the heat pump refrigeration process.
  • the chilled water from 5 to 10 ° C in the refrigerating evaporator 25 is partially introduced into the air heat exchanger 36, and the air entering the air compressor is cooled from 25 ° C to 15 ° C, and the heat is exchanged.
  • the water enters the chilled water buffer tank 37, is sent to the refrigerating evaporator 25 for recycling through the chilled water transfer pump 38, and the other portion of the chilled water enters the seven-stage flashing section to condense the 25 ° C saturated steam generated by the flashing. .
  • the 100 ° C saturated steam to the generator 21 and the heating evaporator 23 is passed through the condenser to the tertiary condensate buffer tank 39 and is sent to the subsequent system for use by the five-stage condensate transfer pump 40.

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Abstract

本发明涉及一种PTA精制单元母液的回收利用方法。本发明通过采用高效多级闪蒸技术、低温余热发电技术、热泵制热与制冷技术、低温结晶技术等，实现PTA母液余热及PT酸的回收，将PTA母液中的热量进行有效利用，并解决了PT酸的结晶对后续系统的影响，减小了对环境的污染，并能产生巨大的经济效益。

Description

PTA精制单元母液的回收利用方法 技术领域
本发明涉及PTA精制单元母液的回收利用方法，更具体涉及到PTA工业装置中PTA精制单元母液余热及PT酸回收的方法，同样适用于其他行业中废水的低温余热回收。
背景技术
在PTA(精制对苯二甲酸)生产装置中，PTA精制过程中往往会产生大量的含有PT(对甲基苯甲酸)酸、TA(对苯二甲酸)固体、H2、N2等不凝气的废水，废水的温度可高达140～150℃，目前工业中主要采用精制尾气洗涤系统对其进行处理，来自装置中的高温PTA母液首先进入到常压闪蒸塔中，高温母液在塔内发生闪蒸，闪蒸产生的蒸汽与H2、N2等不凝汽一同由常压闪蒸塔的塔顶排放入环境，闪蒸产生的母液再通过空冷的方式进行降温，经降温后的PTA母液再进入到后续的膜处理系统进行使用。
上述的现有工业装置PTA母液的处理方法主要存在以下问题：
(1)闪蒸产生的蒸汽排入环境，造成废水中携带的大量热量直接排入到大气中，导致能量的大量浪费。
(2)蒸汽直接排入到大气，在生产区域形成“白龙”的现象，并且蒸汽中含有PT酸等酸性物质，对环境造成了严重的污染。
(3)PTA母液冷却后进入到膜处理系统，由于PT酸固体颗粒的析出，容易造成膜处理系统的堵塞。
发明内容
为了解决现有PTA母液处理装置的问题，本发明的目的在于提供一种PTA母液余热及PT酸回收的方法，该方法通过采用高效多级闪蒸技术、低温余热发电技术、热泵制热与制冷技术、低温结晶技术等，实现PTA母液热量的高效多级利用，通过此方法可实现PTA母液中热量的回收利用，解决现有工业装置的不足。
本发明的目的是这样实现的：
本发明提供一种PTA精制单元母液的回收利用方法，包括如下步骤：
多级闪蒸冷却步骤：PTA精制单元母液进入高效多级闪蒸塔(1)中，所述高效多级闪蒸塔(1)包含至少N级闪蒸段，在所述高效多级闪蒸塔
(1)中所述PTA精制单元母液发生N-1级闪蒸；
所述高效多级闪蒸塔(1)中第N级闪蒸段为闪蒸冷却段，所述闪蒸冷却段不发生闪蒸，且所述闪蒸冷却段位于第N-2级闪蒸段与第N-1级闪蒸段之间；
余热利用步骤：用于第一级闪蒸段至第M级闪蒸段产生的闪蒸蒸气进入余热利用单元；
PT酸结晶回收步骤：用于第N-1级闪蒸段产生的母液进入低温结晶单元，将PTA精制单元母液中的PT酸结晶回收；
其中，N＝4～8，M＝1～4；N＞M，N与M皆为整数。
本发明所述的PTA精制单元母液的回收利用方法，其中：所述余热利用单元优选包括第一余热利用单元和第二余热利用单元；
所述第一余热利用单元优选为：第一级闪蒸段产生的一级闪蒸蒸汽所进入的制热单元和/或制冷单元；
所述第二余热利用单元优选为：第二级闪蒸段至第M级闪蒸段产生的闪蒸蒸气所进入的发电单元。
本发明所述的PTA精制单元母液的回收利用方法，其中：
所述制热单元中优选具体发生如下步骤：
来自高效多级闪蒸塔(1)中的一级闪蒸蒸汽，一部分进入到发生器(21)中，溴化锂稀溶液被加热蒸发，换热后的蒸汽凝液进入到三级凝液缓冲罐(39)中，蒸发产生的蒸汽进入到冷凝器(22)中，并在循环冷却水的作用下冷凝，冷凝器产生的工质凝液通过工质循环泵分别进入到制热蒸发器(23)和制冷蒸发器(25)中，在制热蒸发器(23)中，工质凝液被来自另一部分的一级闪蒸蒸汽加热蒸发，冷凝后的一级闪蒸蒸汽凝液进入到三级凝液缓冲罐(39)中，被加热蒸发的工质蒸汽进入到制热吸收器(24)中，溴化锂浓溶液在制热吸收器(24)中处于不饱和状态，从而将工质蒸汽进行吸收，在吸收过程中放出大量的热量，来自四级凝液输送泵(35)的凝液进入 到制热吸收器(24)中，并被加热，加热后的凝液进入到二级凝液缓冲罐(34)中，并在此发生闪蒸，产生中、低压蒸汽，并进入到后续系统利用。
本发明所述的PTA精制单元母液的回收利用方法，其中：
所述制冷单元优选具体发生了如下步骤：
进入到所述制冷蒸发器(25)中的工质凝液，在低温水加热的作用下进行蒸发，蒸发产生的工质蒸汽进入到制冷吸收器(26)中，溴化锂浓溶液在制冷吸收器(26)中处于不饱和状态，从而将工质蒸汽进行吸收，在吸收过程中放出的大量热量由冷却循环水进行冷却，在制冷蒸发器(25)中换热后的低温水降温，从而获得温度更低的冷冻水；
由制冷蒸发器(25)产生的冷冻水，一部分进入到空气换热器(36)中，将空气压缩机进口的空气进行冷却，换热后的冷冻水进入到冷冻水缓冲罐(37)中，并通过冷冻水输送泵(38)输送至制冷蒸发器(25)中循环使用，另一部分冷冻水进入到高效多级闪蒸塔(1)中，并对闪蒸蒸汽进行冷却。
本发明所述的PTA精制单元母液的回收利用方法，其中：
所述发电单元优选具体发生了如下步骤：
第二级闪蒸段至第M级闪蒸段均分别各自连接有换热器，且各个换热器之间同时进行串联连接，以使得高效多级闪蒸塔(1)产生的蒸汽能够将换热器中的溶剂气化；
来自第M级闪蒸段的闪蒸蒸汽与来自溶剂输送泵(8)的溶剂在与其相连接的一级换热器中进行间接换热，经换热后的蒸汽凝液排入到一级凝液缓冲罐(9)中；
经上一步骤加热后的溶剂进入到与一级换热器串联的下一级换热器中，经换热后的蒸汽凝液排入到一级凝液缓冲罐(9)中；
重复上述溶剂与闪蒸段的闪蒸蒸汽的换热步骤；
经气化后的溶剂蒸汽进入到汽轮机(5)中，并推动汽轮机做功发电，做功后的溶剂蒸汽随后进入到溶剂冷凝器(6)中，冷凝产生的溶剂凝液进入到溶剂缓冲罐(7)中，再通过溶剂输送泵(8)的作用下输送至一级换热器中，从而完成PTA母液中部分的余热转化成电能的循环过程；
一级凝液缓冲罐(9)中的凝液在一级凝液输送泵(10)的作用下输送至后续系统使用。
本发明所述的PTA精制单元母液的回收利用方法，其中：
所述低温结晶单元优选具体发生了如下步骤：
所述高效多级闪蒸塔(1)中的第N-2级闪蒸段连接有文丘里引射器(12)；所述高效多级闪蒸塔(1)中的第N级闪蒸段为闪蒸冷却段，且连接有二级凝液输送泵(13)；
第N-1级闪蒸段产生的母液进入结晶罐(15)中，PT酸在结晶罐(15)中大量结晶析出，结晶后剩余的含有少量固体杂质的液体在一级母液输送泵(16)加压的作用下依次进入多个串联的过滤器中，固体颗粒被截留下来，并通过过滤器底部排出，过滤后的母液进入到母液缓冲罐(19)中，并在二级母液输送泵(20)的作用下进入到文丘里引射器(12)中，将来自第N-2级闪蒸段的闪蒸蒸汽进行冷凝，冷凝后的凝液在二级凝液输送泵(13)的作用下输送至后续的膜处理系统。
本发明所述的PTA精制单元母液的回收利用方法，其中：N优选为8，M优选为4。
本发明所述的PTA精制单元母液的回收利用方法，其中：所述PTA精制单元母液的温度优选为140～150℃。
本发明所述的PTA精制单元母液的回收利用方法，其中：所述溶剂输送泵(8)的溶剂优选采用R245fa溶剂。
本发明所述的PTA精制单元母液的回收利用方法，其中：所述溴化锂稀溶液的质量浓度优选为56％～60％，所述溴化钾浓溶液的质量浓度优选为60％～64％。
本发明所述的PTA精制单元母液的回收利用方法，其中：所述多个串联的过滤器优选为一级过滤器(17)、二级过滤器(18)串联，且所述多个串联的过滤器中优选设置有滤布。
本发明所述的PTA精制单元母液的回收利用方法，其中：N为8，M为4时，具体步骤可以详述如下：
a.首先PTA精制单元母液进入高效多级闪蒸塔(1)中，PTA精制单元母液发生多级闪蒸，在一级闪蒸段(I)进行一级闪蒸，产生的闪蒸蒸汽进入发生器(21)和制热蒸发器(23)；
一级闪蒸后的凝液进入二级闪蒸段(II)进行二级闪蒸，闪蒸产生的闪蒸蒸汽进入三级换热器(2)；
二级闪蒸后的凝液进入三级闪蒸段(III)进行三级闪蒸，闪蒸产生的闪蒸蒸汽进入二级换热器(3)；
三级闪蒸后的凝液进入四级闪蒸段(IV)进行四级闪蒸，闪蒸产生的闪蒸蒸汽进入一级换热器(4)中；
四级闪蒸后的凝液进入五级闪蒸段(V)进行五级闪蒸，闪蒸产生的闪蒸蒸汽进入蒸汽冷凝器(11)中，并在循环冷却水的作用进行冷凝，冷凝后的蒸汽凝液进入到后续系统使用；
五级闪蒸后的凝液进入六级闪蒸段(VI)，闪蒸产生的闪蒸蒸汽进入文丘里引射器(12)中；
六级闪蒸后的凝液进入七级闪蒸段(VII)，闪蒸产生的闪蒸蒸汽在冷冻水的作用下进行冷凝，冷凝后的闪蒸凝液在三级凝液输送泵(14)的作用下进入冷冻水缓冲罐(37)中，作为制取冷冻水的补水使用；
b.来自四级闪蒸段(IV)的闪蒸蒸汽与来自溶剂输送泵(8)的溶剂在一级换热器(4)中进行间接换热，经换热后的蒸汽凝液排入到一级凝液缓冲罐(9)中；
经一级换热器(4)加热后的溶剂进入到二级换热器(3)中，经换热后的蒸汽凝液排入到一级凝液缓冲罐(9)中；
经二级换热器(3)加热后的溶剂进入到三级换热器(2)中，溶剂被气化，经换热后的蒸汽凝液排入到一级凝液缓冲罐(9)中；
经气化后的溶剂蒸汽进入到汽轮机(5)中，并推动汽轮机做功发电，做功后的溶剂蒸汽随后进入到溶剂冷凝器(6)中，冷凝产生的溶剂凝液进入到溶剂缓冲罐(7)中，再通过溶剂输送泵(8)的作用下输送至一级换热器(4)中，从而完成PTA母液中部分的余热转化成电能的循环过程；
一级凝液缓冲罐(9)中的凝液在一级凝液输送泵(10)的作用下输送至后续系统使用；
c.经七级闪蒸段(VII)闪蒸后的PTA母液进入到结晶罐(15)中，PT酸在结晶罐(15)中大量结晶析出，结晶后剩余的含有少量固体杂质的液体在一级母液输送泵(16)加压的作用下依次进入多个串联过滤器中，固体颗粒被截留下来，并通过过滤器底部排出，过滤后的母液进入到母液缓冲罐(19)中，并在二级母液输送泵(20)的作用下进入到文丘里引射器(12)中，将来自六级闪蒸段(VI)的闪蒸蒸汽进行冷凝，冷凝后的凝液在二级凝液输送泵(13)的作用下输送至后续的膜处理系统；
d.来自高效多级闪蒸塔(1)中的一级闪蒸蒸汽，一部分进入到发生器(21)中，溴化锂稀溶液被加热蒸发，换热后的蒸汽凝液进入到三级凝液缓冲罐(39)中，蒸发产生的蒸汽进入到冷凝器(22)中，并在循环冷却水的作用下冷凝，冷凝器产生的工质凝液通过工质循环泵分别进入到制热蒸发器(23)和制冷蒸发器(25)中，在制热蒸发器中，工质凝液被来自另一部分的一级闪蒸蒸汽加热蒸发，冷凝后的一级闪蒸蒸汽凝液进入到三级凝液缓冲罐(39)中，被加热蒸发的工质蒸汽进入到制热吸收器(24)中，溴化锂浓溶液在制热吸收器(24)中处于不饱和状态，从而将工质蒸汽进行吸收，在吸收过程中放出了大量的热量，来自四级凝液输送泵(35)的凝液进入到制热吸收器(24)中，并被加热，加热后的凝液进入到二级凝液缓冲罐(34)中，并在此发生闪蒸，产生中、低压蒸汽，并进入到后续系统利用；
e.进入到制冷蒸发器(25)中的工质凝液，在低温水加热的作用下进行蒸发，蒸发产生的工质蒸汽进入到制冷吸收器(26)中，溴化锂浓溶液在制冷吸收器(26)中处于不饱和状态，从而将工质蒸汽进行吸收，在吸收过程中放出的大量热量由冷却循环水进行冷却，在制冷蒸发器(25)中换热后的低温水降温，从而获得温度更低的冷冻水；
f.由制冷蒸发器(25)产生的冷冻水，一部分进入到空气换热器(36)中，将空气压缩机进口的空气进行冷却，换热后的冷冻水进入到冷冻水缓冲罐(37)中，并通过冷冻水输送泵(38)输送至制冷蒸发器(25)中循环使用，另一部分冷冻水进入到高效多级闪蒸塔(1)中，并对七级闪蒸蒸汽进行冷却。
本发明还可以叙述如下：
一种PTA精制单元母液余热及PT酸回收方法，具体步骤如下：
a来自上游的一定温度下的PTA母液首先进入到高效多级闪蒸塔1中，在此，PTA母液在一级闪蒸段I进行一级闪蒸，闪蒸产生的闪蒸蒸汽进入到发生器21和制热蒸发器23中；一级闪蒸后的凝液进入到高效多级闪蒸塔1的二级闪蒸段II，在此，PTA母液发生二级闪蒸，闪蒸产生的闪蒸蒸汽进入到三级换热器2中；二级闪蒸后的凝液进入到三级闪蒸段III，在此，PTA母液发生三级闪蒸，闪蒸产生的闪蒸蒸汽进入到二级换热器3中；三级闪蒸后的凝液进入到四级闪蒸段IV，在此，PTA母液发生四级闪蒸，闪蒸产生的闪蒸蒸汽进入到一级换热器4中；四级闪蒸后的凝液进入到五级闪蒸段V，在此，PTA母液发生五级闪蒸，闪蒸产生的闪蒸蒸汽进入到蒸汽冷凝器11中，并在循环冷却水的作用进行冷凝，冷凝后的蒸汽凝液进入到后续系统使用；五级闪蒸后的凝液进入到六级闪蒸段VI，在此，PTA母液发生六级闪蒸，闪蒸产生的闪蒸蒸汽进入到文丘里引射器12中；六级闪蒸后的凝液进入到七级闪蒸段VII，在此，PTA母液发生七级闪蒸，闪蒸产生的闪蒸蒸汽在冷冻水的作用下进行冷凝，冷凝后的闪蒸凝液在三级凝液输送泵14的作用进入到冷冻水缓冲罐37中，作为制取冷冻水的补水使用。
b来自四级闪蒸段IV的闪蒸蒸汽与来自溶剂输送泵8的溶剂(采用R245fa溶剂)在一级换热器4中进行间接换热，在此，溶剂被加热至一定的温度，经换热后的蒸汽凝液排入到一级凝液缓冲罐9中；经一级换热器4加热后的溶剂进入到二级换热器3中，在此，溶剂与来自三级闪蒸段III的闪蒸蒸汽进行间接换热，溶剂被进一步加热，经换热后的蒸汽凝液排入到一级凝液缓冲罐9中；经二级换热器3加热后的溶剂进入到三级换热器2中，在此，溶剂与来自二级闪蒸段II的闪蒸蒸汽进行间接换热，溶剂被气化，经换热后的蒸汽凝液排入到一级凝液缓冲罐9中；经气化后的溶剂蒸汽进入到汽轮机5中，并推动汽轮机做功发电，做功后的溶剂蒸汽随后进入到溶剂冷凝器6中，并在冷却循环水的作用下冷凝，冷凝产生的溶剂凝液进入到溶剂缓冲罐7中，再通过溶剂输送泵8的作用下输送至一级换热器4中，从而完成PTA母液中部分的余热转化成电能的循环过程。一级凝液缓冲罐9中的凝液在一级凝液输送泵10的作用下输送至后续系统使用。
c经七级闪蒸段VII闪蒸后的PTA母液进入到结晶罐15中，由于此时的PTA母液温度较低，PT酸在结晶罐15中大量结晶析出，结晶后剩余的含有少量固体杂质的液体在一级母液输送泵16加压的作用下依次进入到一级过滤器17、二级过滤器18中，过滤器中设置有滤布等，固体颗粒被截留下来，并通过过滤器底部排出，过滤后的母液进入到母液缓冲罐19中，并在二级母液输送泵20的作用下进入到文丘里引射器12中，在此，将来自六级闪蒸段VI的闪蒸蒸汽进行冷凝，冷凝后的凝液在二级凝液输送泵13的作用下输送至后续的膜处理系统。
d来自高效多级闪蒸塔1中的一级闪蒸蒸汽，一部分进入到发生器21中，在此，一定浓度下的溴化锂稀溶液被加热蒸发，换热后的蒸汽凝液进入到三级凝液缓冲罐39中，蒸发产生的蒸汽进入到冷凝器22中，并在循环冷却水的作用下冷凝，冷凝器产生的工质凝液通过工质循环泵分别进入到制热蒸发器23和制冷蒸发器25中，在制热蒸发器中，工质凝液被来自另一部分的一级闪蒸蒸汽加热蒸发，冷凝后的一级闪蒸蒸汽凝液进入到三级凝液缓冲罐39中，被加热蒸发的工质蒸汽进入到制热吸收器24中，溴化锂浓溶液在制热吸收器24中处于不饱和状态，从而将工质蒸汽进行吸收，在吸收过程中放出了大量的热量，来自四级凝液输送泵35的凝液进入到制热吸收器24中，并被加热，加热后的凝液进入到二级凝液缓冲罐34中，并在此发生闪蒸，产生一定温度下的中、低压蒸汽，并进入到后续系统利用。
e进入到制冷蒸发器25中的工质凝液，在低温水加热的作用下进行蒸发，蒸发产生的工质蒸汽进入到制冷吸收器26中，溴化锂浓溶液在制冷吸收器26中处于不饱和状态，从而将工质蒸汽进行吸收，在吸收过程中放出的大量热量由冷却循环水进行冷却，在制冷蒸发器25中换热后的低温水降温，从而获得温度更低的冷冻水。
f由制冷蒸发器25产生的冷冻水，一部分进入到空气换热器36中，将空气压缩机进口的空气进行冷却，换热后的冷冻水进入到冷冻水缓冲罐37中，并通过冷冻水输送泵38输送至制冷蒸发器25中循环使用，另一部分冷冻水进入到高效多级闪蒸塔1中，并对七级闪蒸蒸汽进行冷却。本系统的真空度由一级真空泵41、二级真空泵42、三级真空泵43来进行维持。
本发明的有益效果：
1、本发明将原有排入环境中的蒸汽，进行分级综合利用，将部分PTA母液中的余热用于发电、制取高品质蒸汽及制取冷冻水，实现了热量的回收利用。
2、本发明中采用低温结晶技术，将PTA母液中的PT酸结晶回收，减少了PT酸结晶对后续系统的影响，并能够向后续的膜处理系统提供结晶的工艺水，解决了膜处理系统易堵的问题。
3、本发明中将原有排入环境的蒸汽进行回收利用，解决了环境污染的问题。
4、本发明提供的母液处理方法，不仅设备投资较少，而且能够直接副产发电，产生高品质的蒸汽利用，产生的冷冻水用于将进入空气压缩机的空气进行冷却，大幅度降低了空气压缩机的电耗，降低了PTA装置的运行成本。因此，本发明所提供的母液处理方法，能够产生巨大的经济效益。
附图说明
图1、图2为本发明的工艺流程图；
其中，附图标记：
1高效多级闪蒸塔
2三级换热器
3二级换热器
4一级换热器
5汽轮机
6溶剂冷凝器
7溶剂缓冲罐
8溶剂输送泵
9一级凝液缓冲罐
10一级凝液输送泵
11蒸汽冷凝器
12文丘里引射器
13二级凝液输送泵
14三级凝液输送泵
15结晶罐
16一级母液输送泵
17一级过滤器
18二级过滤器
19母液缓冲罐
20二级母液输送泵
21发生器
22冷凝器
23制热蒸发器
24制热吸收器
25制冷蒸发器
26制冷吸收器
27一级溶剂热交换器
28二级溶剂热交换器
29一级溴化锂循环泵
30一级工质循环泵
31二级工质循环泵
32三级工质循环泵
33二级溴化锂循环泵
34二级凝液缓冲罐
35四级凝液输送泵
36空气换热器
37冷冻水缓冲罐
38冷冻水输送泵
39三级凝液缓冲罐
40五级凝液输送泵
41一级真空泵
42二级真空泵
43三级真空泵
I一级闪蒸段
II二级闪蒸段
III三级闪蒸段
IV四级闪蒸段
V五级闪蒸段
VI六级闪蒸段
VII七级闪蒸段
VIII闪蒸冷却段。
具体实施方式
以下对本发明的实施例作详细说明：本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和过程，但本发明的保护范围不限于下述的实施例，下列实施例中未注明具体条件的实验方法，通常按照常规条件。
结合附图1、2，以N为8，M为4为例，对本发明的具体实施方式进一步描述：
(1)温度为140～150℃的PTA精制单元的母液，首先进入到高效多级闪蒸塔1的一级闪蒸段I中，在PTA母液发生减压闪蒸，闪蒸产生约100℃的饱和蒸汽，并进入到后续的发生器21和制热蒸发器23中；闪蒸后的100℃的PTA母液进入到二级闪蒸段II中，并发生减压闪蒸，闪蒸产生约90℃的饱和蒸汽，并进入到三级换热器2中；闪蒸后的90℃的PTA母液进入到三级闪蒸段III中，并发生减压闪蒸，闪蒸产生约80℃的饱和蒸汽，并进入到二级换热器3中；闪蒸后的80℃的PTA母液进入到四级闪蒸段IV中，并发生减压闪蒸，闪蒸产生约70℃的饱和蒸汽，并进入到一级换热器4中；闪蒸后的70℃的PTA母液进入到五级闪蒸段V中，并发生减压闪蒸，闪蒸产生约60℃的饱和蒸汽进入到蒸汽冷凝器11中，并使用冷却循环水对其进行冷凝，冷凝后的蒸汽凝液进入到后续系统；闪蒸后的60℃的PTA母液进入到六级闪蒸段VI中，并发生减压闪蒸，闪蒸约40℃的饱和蒸汽，并进入到文丘里引射器12中；闪蒸后的40℃的PTA母液进入到七级闪蒸段VII中，并发生减压闪蒸，闪蒸产生约25℃的饱和蒸汽，在此，产生的饱和蒸 汽与来自制冷蒸发器25中的冷冻水进行直接接触换热，饱和蒸汽被冷凝，冷凝后的凝液通过三级凝液输送泵的作用下进入到冷冻水缓冲罐37中。
(2)低温余热发电系统中，循环溶剂采用R245fa，来自四级闪蒸段IV中的70℃的饱和蒸汽进入到一级换热器4中，与来自溶剂输送泵8的溶剂进行间接换热，溶剂被加热至55～60℃，换热后的蒸汽凝液进入到一级凝液缓冲罐9中；经一级换热器4加热后的溶剂进入到二级换热器3中，在此，与来自三级闪蒸段III中的80℃左右的饱和蒸汽进行间接换热，溶剂被加热至65～70℃，换热后的蒸汽凝液进入到一级凝液缓冲罐9中；经二级换热器3加热后的溶剂进入到三级换热器2中，在此，与来自二级闪蒸段II中的90℃左右的饱和蒸汽进行间接换热，溶剂被蒸发，产生75～85℃的溶剂蒸汽，换热后的蒸汽凝液进入到一级凝液缓冲罐9中。75～85℃的溶剂蒸汽进入到汽轮机5中，并推动汽轮机做功发电，做功后的溶剂蒸汽约45～50℃，并进入到溶剂冷凝器6中，采用循环冷却水对其进行冷凝，冷凝后的溶剂凝液进入到溶剂缓冲罐7中，并在溶剂循环泵8的作用下进入到一级换热器4中，从而完成低温余热发电的循环过程。一级凝液缓冲罐9中的蒸汽凝液在一级凝液输送泵10的作用下输送至后续系统。
(3)来自七级闪蒸段VII中的25℃的PTA母液进入到结晶罐15中，在此，PTA母液中的PT酸大量结晶，结晶后的PTA母液随后在一级母液输送泵16的作用下依次进入到一级过滤器17、二级过滤器18中，将PTA母液中含有的固体杂质除去，过滤后的PTA母液进入到母液缓冲罐19中，并通过二级母液输送泵20进入到文丘里引射器12中，在此，25℃的PTA母液将六级闪蒸段VI中的40℃的饱和蒸汽进行冷凝，产生的冷凝液进入到闪蒸冷却段VIII中，并在二级凝液输送泵的作用下进入到后续的膜处理系统(第VIII位于第VI和第VII之间，此段不发生闪蒸，其余七段均发生闪蒸)。
(4)来自一级闪蒸段I的100℃的饱和蒸汽，一部分进入到发生器21中作为热源使用，另一部分进入到制热蒸发器23中作为热源使用，热泵制热、制冷技术中采用溴化钾溶液作为循环溶剂，水蒸汽作为工质，在发生器21中，浓度为56％～60％的溴化钾溶液被100℃的饱和蒸汽加热，溴化锂溶液蒸发，并产生80～90℃的工质蒸汽进入到冷凝器22中，工质蒸汽在此与冷却循环水进行间接换热，获得40℃左右的蒸汽凝液，即工质凝液，其通 过一级工质循环泵一部分进入到制热蒸发器23中，一部分进入到制冷蒸发器25中，在制热蒸发器23中，工质凝液在100℃热源的作用蒸发，蒸发产生约90℃的工质蒸汽，为了保证蒸发的顺利进行，工质凝液通过二级工质循环泵31进行强制循环蒸发，由制热蒸发器23产生的工质蒸汽进入到制热吸收器24中，在此，溴化锂溶液的浓度为60％～64％，溴化锂溶液处于非饱和状态，因此能够将工质蒸汽进行吸收，在此过程中，工质蒸汽放出大量的热量，来自四级凝液输送泵35中的凝液进入到制热吸收器24中，并将放出的热量吸收，凝液温度升高至135～140℃，随后加热的凝液进入到二级凝液缓冲罐34中，并发生闪蒸，产生约130℃的饱和蒸汽进入后续系统利用，56％～60％的溴化锂溶液在发生器21蒸发后，产生60％～64％的溴化锂溶液，并在一级溴化锂循环泵29的作用下进入到一级溶剂热交换器27中，60％～64％的溴化锂溶液在制热吸收器吸收工质蒸汽后，产生56％～60％的溴化锂溶液，并进入到一级溶剂热交换器27中，在此，与来自发生器的溴化锂溶液进行间接换热，从而完成热泵的制热过程。
(5)进入到制冷蒸发器25中的40℃的工质凝液，吸收来自冷冻水输送泵38的15℃左右的低温水的热量，工质凝液被蒸发，产生5℃的工质蒸汽，为了保证工质凝液被顺利蒸发，工质凝液通过三级工质循环泵32强制循环蒸发，经吸收热量后的15℃的低温水，产生5～10℃的冷冻水，产生的5℃的工质蒸汽进入到制冷吸收器26中，在此，浓度为60％～64％的溴化锂溶液将工质蒸汽吸收，吸收过程中放出的热量，采用循环冷却水对其进行冷却，经吸收后的56％～60％的溴化锂溶液与来自蒸发器21中的60～64％的溴化钾溶液在二级溶剂交换器28中进行间接换热，从而完成热泵的制冷过程。
(6)来自制冷蒸发器25中的5～10℃的冷冻水，一部分进入到空气换热器36中，将进入到空气压缩机的空气由25℃冷却至15℃左右，换热后的冷冻水进入到冷冻水缓冲罐37中，并通过冷冻水输送泵38输送至制冷蒸发器25中循环使用，另一部分冷冻水进入到七级闪蒸段，将闪蒸产生的25℃饱和蒸汽进行冷凝。去往发生器21和制热蒸发器23中的100℃饱和蒸汽，经冷凝器进入到三级凝液缓冲罐39中，并在五级凝液输送泵40的作用下输送至后续系统使用。

Claims (12)

  1. 一种PTA精制单元母液的回收利用方法，包括如下步骤：
    多级闪蒸冷却步骤：PTA精制单元母液进入高效多级闪蒸塔(1)中，所述高效多级闪蒸塔(1)包含至少N级闪蒸段，在所述高效多级闪蒸塔(1)中所述PTA精制单元母液发生N-1级闪蒸；
    所述高效多级闪蒸塔(1)中第N级闪蒸段为闪蒸冷却段，所述闪蒸冷却段不发生闪蒸，且所述闪蒸冷却段位于第N-2级闪蒸段与第N-1级闪蒸段之间；
    余热利用步骤：用于第一级闪蒸段至第M级闪蒸段产生的闪蒸蒸气进入余热利用单元；
    PT酸结晶回收步骤：用于第N-1级闪蒸段产生的母液进入低温结晶单元，将PTA精制单元母液中的PT酸结晶回收；
    其中，N＝4～8，M＝1～4；N＞M，N与M皆为整数。
  2. 根据权利要求1所述的PTA精制单元母液的回收利用方法，其特征在于：所述余热利用单元包括第一余热利用单元和第二余热利用单元；
    所述第一余热利用单元为：第一级闪蒸段产生的一级闪蒸蒸汽所进入的制热单元和/或制冷单元；
    所述第二余热利用单元为：第二级闪蒸段至第M级闪蒸段产生的闪蒸蒸气所进入的发电单元。
  3. 根据权利要求2所述的PTA精制单元母液的回收利用方法，其特征在于：
    所述制热单元中具体发生如下步骤：
    来自高效多级闪蒸塔(1)中的一级闪蒸蒸汽，一部分进入到发生器(21)中，溴化锂稀溶液被加热蒸发，换热后的蒸汽凝液进入到三级凝液缓冲罐(39)中，蒸发产生的蒸汽进入到冷凝器(22)中，并在循环冷却水的作用下冷凝，冷凝器产生的工质凝液通过工质循环泵分别进入到制热蒸发器(23)和制冷蒸发器(25)中，在制热蒸发器(23)中，工质凝液被来自另一部分的一级闪蒸蒸汽加热蒸发，冷凝后的一级闪蒸蒸汽凝液进入到三级凝液缓冲罐(39)中，被加热蒸发的工质蒸汽进入到制热吸收器(24)中，溴化锂浓溶液在制热吸收器(24)中处于不饱和状态，从而将工质蒸汽进行吸 收，在吸收过程中放出大量的热量，来自四级凝液输送泵(35)的凝液进入到制热吸收器(24)中，并被加热，加热后的凝液进入到二级凝液缓冲罐(34)中，并在此发生闪蒸，产生中、低压蒸汽，并进入到后续系统利用。
  4. 根据权利要求2所述的PTA精制单元母液的回收利用方法，其特征在于：
    所述制冷单元具体发生如下步骤：
    进入到所述制冷蒸发器(25)中的工质凝液，在低温水加热的作用下进行蒸发，蒸发产生的工质蒸汽进入到制冷吸收器(26)中，溴化锂浓溶液在制冷吸收器(26)中处于不饱和状态，从而将工质蒸汽进行吸收，在吸收过程中放出的大量热量由冷却循环水进行冷却，在制冷蒸发器(25)中换热后的低温水降温，从而获得温度更低的冷冻水；
    由制冷蒸发器(25)产生的冷冻水，一部分进入到空气换热器(36)中，将空气压缩机进口的空气进行冷却，换热后的冷冻水进入到冷冻水缓冲罐(37)中，并通过冷冻水输送泵(38)输送至制冷蒸发器(25)中循环使用，另一部分冷冻水进入到高效多级闪蒸塔(1)中，并对闪蒸蒸汽进行冷却。
  5. 根据权利要求2所述的PTA精制单元母液的回收利用方法，其特征在于：
    所述发电单元具体发生如下步骤：
    第二级闪蒸段至第M级闪蒸段均分别各自连接有换热器，且各个换热器之间同时进行串联连接，以使得高效多级闪蒸塔(1)产生的蒸汽能够将换热器中的溶剂气化；
    来自第M级闪蒸段的闪蒸蒸汽与来自溶剂输送泵(8)的溶剂在与其相连接的一级换热器中进行间接换热，经换热后的蒸汽凝液排入到一级凝液缓冲罐(9)中；
    经上一步骤加热后的溶剂进入到与一级换热器串联的下一级换热器中，经换热后的蒸汽凝液排入到一级凝液缓冲罐(9)中；
    重复上述溶剂与闪蒸段的闪蒸蒸汽的换热步骤；
    经气化后的溶剂蒸汽进入到汽轮机(5)中，并推动汽轮机做功发电，做功后的溶剂蒸汽随后进入到溶剂冷凝器(6)中，冷凝产生的溶剂凝液进 入到溶剂缓冲罐(7)中，再通过溶剂输送泵(8)的作用下输送至一级换热器中，从而完成PTA母液中部分的余热转化成电能的循环过程；
    一级凝液缓冲罐(9)中的凝液在一级凝液输送泵(10)的作用下输送至后续系统使用。
  6. 根据权利要求1～5任一项所述的PTA精制单元母液的回收利用方法，其特征在于：
    所述低温结晶单元具体发生如下步骤：
    所述高效多级闪蒸塔(1)中的第N-2级闪蒸段连接有文丘里引射器(12)；所述高效多级闪蒸塔(1)中的第N级闪蒸段为闪蒸冷却段，且连接有二级凝液输送泵(13)；
    第N-1级闪蒸段产生的母液进入结晶罐(15)中，PT酸在结晶罐(15)中大量结晶析出，结晶后剩余的含有少量固体杂质的液体在一级母液输送泵(16)加压的作用下依次进入多个串联的过滤器中，固体颗粒被截留下来，并通过过滤器底部排出，过滤后的母液进入到母液缓冲罐(19)中，并在二级母液输送泵(20)的作用下进入到文丘里引射器(12)中，将来自第N-2级闪蒸段的闪蒸蒸汽进行冷凝，冷凝后的凝液在二级凝液输送泵(13)的作用下输送至后续的膜处理系统。
  7. 根据权利要求1～5任一项所述的PTA精制单元母液的回收利用方法，其特征在于：N为8，M为4。
  8. 根据权利要求6所述的PTA精制单元母液的回收利用方法，其特征在于：N为8，M为4。
  9. 根据权利要求7所述的PTA精制单元母液的回收利用方法，其特征在于：所述PTA精制单元母液的温度为140～150℃。
  10. 根据权利要求5所述的PTA精制单元母液的回收利用方法，其特征在于：所述溶剂输送泵(8)的溶剂采用R245fa溶剂。
  11. 根据权利要求3或4所述的PTA精制单元母液的回收利用方法，其特征在于：所述溴化锂稀溶液的质量浓度为56％～60％，所述溴化锂浓溶液的质量浓度为60％～64％。
  12. 根据权利要求6所述的PTA精制单元母液的回收利用方法，其特征在于：所述多个串联的过滤器为一级过滤器(17)、二级过滤器(18)串 联，且所述多个串联的过滤器中设置有滤布。
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