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CN106745421A - A kind of multiple Intermediate Heat Exchanger rectification method treatment low concentration DMF waste water systems of band - Google Patents

A kind of multiple Intermediate Heat Exchanger rectification method treatment low concentration DMF waste water systems of band Download PDF

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Publication number
CN106745421A
CN106745421A CN201611167122.5A CN201611167122A CN106745421A CN 106745421 A CN106745421 A CN 106745421A CN 201611167122 A CN201611167122 A CN 201611167122A CN 106745421 A CN106745421 A CN 106745421A
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China
Prior art keywords
heat exchanger
dmf
waste water
intermediate heat
reboiler
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Pending
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CN201611167122.5A
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Chinese (zh)
Inventor
高晓新
朱碧云
黄泽恩
马江权
杨德明
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Changzhou University
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Changzhou University
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Priority to CN201611167122.5A priority Critical patent/CN106745421A/en
Publication of CN106745421A publication Critical patent/CN106745421A/en
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/043Details
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C231/00Preparation of carboxylic acid amides
    • C07C231/22Separation; Purification; Stabilisation; Use of additives
    • C07C231/24Separation; Purification
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The present invention relates to a kind of multiple Intermediate Heat Exchanger rectification method treatment low concentration DMF waste water systems of band, the system includes feed preheater, atmospheric distillation tower, multiple intermediate reboilers, overhead condenser and tower reactor reboiler.DMF waste water enters separation in rectifying column after preheater is preheating to bubble point.The present invention reduces the consumption of high-grade steam using multiple intermediate reboilers, and intermediate plate side take-off material is heated using the steam of lower level, so as to save tower bottom steam consumption, improves the thermodynamic efficiency of separation system;Thermodynamic efficiency can improve more than 39% compared with traditional rectificating method.

Description

A kind of multiple Intermediate Heat Exchanger rectification method treatment low concentration DMF waste water systems of band
Technical field
The invention belongs to field of waste water treatment, it is related to a kind of separation method of low concentration DMF waste water, specifically, is related to A kind of multiple Intermediate Heat Exchanger rectification method treatment low concentration DMF waste water systems of band.
Background technology
DMF (DMF) is a kind of low toxicity, colourless, transparency liquid, in petrochemical industry, organic synthesis, agriculture As a kind of industrial chemicals of function admirable in the fields such as medicine, pharmacy, synthetic fibers, the fine artificial leather that reels off raw silk from cocoons of polypropylene, polarity compared with By force, can be miscible with water, ether, alcohol, ester, unsaturated hydrocarbons and aromatic hydrocarbons, there is the title of " alembroth ".DMF makes extensively in Chemical Manufacture With, the discharge of a large amount of DMF waste water is caused, human body Long Term Contact or suction can hinder hematopoietic function and cause liver failure, also Serious pollution can be caused to air and water.Therefore, the treatment to DMF waste water is particularly important.
DMF concentration is relatively low in the waste liquid discharged in production process, such as reclaims dress using simple DMF domestic at present Put, due to high energy consumption, treatment recovery cost is also higher so that factory economy decline in benefits.The direct discharge of DMF waste water is not only made Into environmental pollution, huge economic loss can be also caused.
The domestic and international processing method to DMF waste water mainly has physico-chemical process (rectifying, absorption, extraction), biochemical process, surpasses and face at present Boundary's water oxidation, chemical method (alkalization method).It is more long to there is process time in biochemical process, halfway shortcoming of degrading;Overcritical water oxygen Change method use condition is more harsh, and large-scale use difficulty is larger;Absorption method is related to adsorbent reactivation and back extraction to separate, not only Complex process, and processing cost is higher;It is to use more DMF recovery methods both at home and abroad at present that rectifying is reclaimed.
The centrifugal station of conventional DMF waste water uses rectifying column and is operated.DMF-H2O systems belong to typical big temperature Difference separation system, the temperature difference of tower top tower reactor is larger in conventional separation methods, and many conservation measures industrialization application technologies are immature. Directly by condensation water cooling, tower reactor has thereby resulted in substantial amounts of energy waste, thermodynamics effect to tower top by high-grade steam heating Rate is relatively low.
The content of the invention
The deficiency that the present invention exists for above-mentioned separation method, proposes that a kind of multiple Intermediate Heat Exchanger rectification method treatment of band are low Concentration DMF waste water systems, i.e., using the Finestill energy-saving method of multiple Intermediate Heat Exchangers, the present invention not only reclaims DMF steady qualities, The rate of recovery is high, while have energy consumption low, the simple advantage of equipment flowsheet.
The multiple Intermediate Heat Exchanger rectification method treatment low concentration DMF waste water systems of a kind of band that the present invention is provided, distillation system Boiled again including preheater 1, rectifying column 2, overhead condenser 3, tower reactor reboiler 7, intermediate reboiler 4, intermediate reboiler 5 and centre Device 6.
Preheater 1 connects rectifying column 2, and the tower top of rectifying column 2 connection overhead condenser 3 and water discharging opening, the bottom of towe of rectifying column 2 connect Intermediate reboiler 4 and DMF discharging openings are connect, the stripping section of rectifying column 2 is by connecting intermediate reboiler 4, intermediate reboiler 5 and centre again Boiling device 6 forms loop respectively.
Present invention also offers a kind of side with multiple Intermediate Heat Exchanger rectification method treatment low concentration DMF waste water system treatment Method, with following steps:
1. need to DMF waste water to be processed be preheating to bubble point temperature through waste water preheater 1 as raw material after be passed through rectifying column 2, rectifying obtains water vapour after separating in the tower top of rectifying column 2, and vapor is condensed through overhead condenser 3, and the condensate liquid for obtaining is through essence Evaporate the water discharging opening of tower 2 directly to produce, the bottom of towe of rectifying column 2 provides mass transfer force, isolated high temperature through the heat supply of tower reactor reboiler 7 DMF after concentration is directly produced;
2. the stripping section of rectifying column 2 forms loop by intermediate reboiler 4, intermediate reboiler 5, intermediate reboiler 6;
3. 10%DMF is contained in feedstock, first Intermediate Heat Exchanger 4 is located at the 37th block of plate, and the amount of liquid of extraction is 7705.1kg/h, it is 102.4 DEG C to extract temperature out;Second Intermediate Heat Exchanger 5 is located at the 38th block of plate, extracts amount of liquid out and is 543.1kg/h, it is 104.5 DEG C to extract temperature out;3rd Intermediate Heat Exchanger 6 is located at the 39th block of plate, extracts amount of liquid out and is 391.5kg/h, it is 111.7 DEG C to extract temperature out;
4. 20%DMF is contained in feedstock, first Intermediate Heat Exchanger 4 is located at the 21st block of plate, and the amount of liquid of extraction is 3692.6kg/h, it is 101.7 DEG C to extract temperature out;Second Intermediate Heat Exchanger 5 is located at the 25th block of plate, extracts amount of liquid out and is 4835.8kg/h, it is 113.3 DEG C to extract temperature out.
Further, rectifying column is packed tower, is made up of rectifying section and stripping section;Operating pressure is normal pressure, overhead reflux Than being 0.44-0.54;The perforated plate corrugated structured packing of filling tape in tower;Side take-off amount is 391-9671kg/h;Tower reactor is produced DMF of the mass fraction more than or equal to 99.8%, water of the overhead extraction mass fraction more than or equal to 99.8%.
The beneficial effects of the present invention are:
1. improve bottom of towe in traditional rectifying column and be mainly and give material heat supply by high-grade steam, so as to the energy that causes A large amount of consumption problems, compared with traditional single column, as shown in Figure 1, for 10%DMF chargings, energy consumption increases with intermediate reboiler Number present decreases in non-linear trend, increase by three intermediate reboilers after trend become gentle, consider heat exchange area etc. because Element, it is determined that three Intermediate Heat Exchangers of increase are optimal, can save energy 77.43%, and for 20%DMF chargings, energy consumption is with intermediate reboiler Number is successively decreased, and increasing by two intermediate reboiler trend becomes gentle, considers the factors such as heat exchange area, it is determined that increasing in two Between heat exchanger it is optimal, can save energy 71.31%;
2. using the extraction of stripping section material, material heat supply is given by low-grade steam by intermediate reboiler, is entered back into Separated in tower, reduce the consumption of tower reactor high-grade steam, and do not increase equipment investment;
3. intermediate heat transfer technology can increase substantially thermodynamic efficiency, as shown in Figure 2, right compared with traditional single column In 10%DMF chargings, first three intermediate reboiler and the linear decline trend of energy consumption, the 4th intermediate reboiler trend base of increase This is steady, and comprehensive energy consumption determines that three Intermediate Heat Exchangers of increase are optimal, and thermodynamic efficiency improves 65.69%, enters for 20%DMF Material, available energy loss reduces as intermediate reboiler number increases, and comprehensive energy consumption determines that two intermediate reboilers of increase are optimal, heat Mechanical efficiency improves 47.10%,;
4. the water and DMF product purities by being refining to obtain are all very high, and high-purity DMF products can be recycled, and also may be used Sold as product, water can be used as technique soft water, reduce the discharge of waste water.
Brief description of the drawings
Fig. 1 is Intermediate Heat Exchanger number and energy consumption graph of a relation
Fig. 2 is Intermediate Heat Exchanger number and available energy loss graph of a relation
Fig. 3 is flow chart of the invention
Label is as follows in Fig. 3:1- preheaters;2-DMF-H2O separating rectification towers;3- overhead condensers;4- intermediate reboilers 1;5- intermediate reboilers 2;6- intermediate reboilers 3;7- tower reactor reboilers.101- raw materials DMF-H2O mixtures preheat feed pipe, DMF-H after 102- raw material preheatings2O mixture feed pipes, 301- overhead product water discharge nozzles, 401- side take-off pipe Isosorbide-5-Nitraes 02- Side take-off return duct 2,501- side take-offs pipe 3,502- side take-offs return duct 4,601- side take-offs pipe 5,602- side lines Extraction return duct 6,701- bottom of towe liquid-phase product DMF discharge nozzles.
Specific embodiment
The present invention is given a detailed account with reference to accompanying drawing:
The DMF-H of low concentration in the present invention2O systems belong to big temperature difference separation system, and the system, tower top are separated at ambient pressure The tower reactor temperature difference is larger, and many conservation measures cannot be utilized directly.
Raw mixture A enters preheater 1 through raw material preheating feed pipe 101, and preheating reaches bubble point through 102 material feeding tubes Into DMF-H2O separating rectification towers 2, the H of high concentration2O is produced through overhead product discharge nozzle 301, and the DMF of high concentration is through tower bottoms Phase product discharge pipe 701 is produced as product, and stripping section lower section side line production material comes back to after being exchanged heat through intermediate reboiler Separated in tower.
Embodiment 1:
Using the technological process shown in accompanying drawing 3, DMF 10% (mass fraction), H are contained in raw mixture A2O90% (mass fraction), inlet amount is 5000kg/h, is preheated into preheater 1 at normal temperatures and pressures, is entered by 102 after reaching bubble point temperature Enter in rectifying column 2 and separate.DMF waste water separating rectification tower needs 42 pieces of theoretical plates, and operating pressure is 0.1MPa, and the filler for being used is Mellapak packing with holes, tower diameter is 1.15 meters, and reflux ratio is 0.44.The concentration of overhead water reaches 99.8%, and tower reactor obtains purity It is 99.8% DMF products.The 90% i.e. mixture of 7705.1kg/h of column plate material total amount is extracted out by 401 pipes from 37 blocks of plates Road is produced, and temperature of charge is 102.4 DEG C, (is heated with 0.17MPa steam) through Intermediate Heat Exchanger 4, consumes the work(of 3038.07kW Consumption, obtains the material that temperature is 108.6 DEG C and returns to separation in rectifying column by 402 pipelines;It is total from 38 blocks of plate extraction column plate materials The 10% of the amount i.e. mixture of 543.1kg/h is produced by 501 pipelines, and temperature of charge is 104.5 DEG C, (is used through Intermediate Heat Exchanger 5 0.17MPa steam is heated), the power consumption of 178.6kW is consumed, obtain the material that temperature is 115.4 DEG C and return to rectifying by 502 pipelines Separated in tower;The 10% i.e. mixture of 391.5kg/h for extracting column plate material total amount out from 39 blocks of plates is produced by 601 pipelines, thing Material temperature degree is 111.7 DEG C, (is heated with 0.2MPa steam) through Intermediate Heat Exchanger 6, consumes the power consumption of 91.1kW, and obtaining temperature is 130.6 DEG C of material is returned in rectifying column by 602 pipelines and separated;Tower top is with 33 DEG C of cooling water condensation;Tower reactor 0.62MPa Steam give tower reactor heat supply.
Through analytical calculation, three intermediate reboilers can reduce the consumption of tower reactor GOOD TASTE steam, make full use of low energy The steam of level is used for the material heating of middle extraction stream stock, and energy-conservation energy consumption so, is obtaining the same of the product of same concentrations When, thermodynamic efficiency improves 39.3% compared with conventional rectification, and energy consumption reduces 79.1%.
Embodiment 2:
Using the technological process shown in accompanying drawing 3, DMF 20% (mass fraction), H are contained in raw mixture A2O 80% (mass fraction), inlet amount is 5000kg/h, is preheated into preheater 1 at normal temperatures and pressures, is reached after bubble point temperature by S102 Separated in into rectifying column 2.DMF waste water separating rectification tower needs 28 pieces of theoretical plates, and operating pressure is 101.3kPa, and what is used fills out Expect to be mellapak packing with holes, tower diameter is 1.1 meters, and reflux ratio is 0.51.The concentration of overhead water reaches 99.8%, and tower reactor obtains pure Spend the DMF products for 99.8%.The 30% i.e. mixture of 3692.6kg/h for extracting column plate material total amount out from 21 blocks of plates passes through 401 Pipeline is produced, and temperature of charge is 101.7 DEG C, (is heated with 0.17MPa steam) through Intermediate Heat Exchanger 4, consumes the work(of 1638.2kW Consumption, obtains the material that temperature is 105.2 DEG C and returns to separation in rectifying column by 402 pipelines;It is total from 25 blocks of plate extraction column plate materials The 50% of the amount i.e. mixture of 4835.8kg/h is produced by 501 pipelines, and temperature of charge is 113.3 DEG C, through Intermediate Heat Exchanger 5 (being heated with 0.23MPa steam), consumes the power consumption of 1081.8kW, obtains the material that temperature is 132.7 DEG C and is returned to by 502 pipelines Separated in rectifying column;Tower top is with 33 DEG C of cooling water condensation;Tower reactor gives tower reactor heat supply with the steam of 0.62MPa.
Through analytical calculation, two intermediate reboilers can reduce the consumption of tower reactor GOOD TASTE steam, by the steaming of low-lying level Vapour is used for the material heating of middle extraction stream stock, energy-conservation energy consumption, so, and normal while the product of same concentrations is obtained Rule rectifying improves 47.1% compared to thermodynamic efficiency, and energy consumption reduces 71.3%.

Claims (3)

1. a kind of multiple Intermediate Heat Exchanger rectification methods of band process low concentration DMF waste water systems, it is characterized by the multiple intermediate heat transfers of band The distillation system of device:Including preheater, rectifying column, overhead condenser, tower reactor reboiler, intermediate reboiler;
The preheater connects the rectifying column, and the rectifying column tower top connects the overhead condenser and H2O discharging openings, it is described Rectifying tower bottom connects the intermediate reboiler and DMF discharging openings, and the rectifying column stripping section is boiled again by connecting the centre Device forms loop.
2. the multiple Intermediate Heat Exchanger rectification methods of a kind of band as claimed in claim 1 process low concentration DMF waste water systems, its feature It is:Intermediate Heat Exchanger includes intermediate reboiler 4, intermediate reboiler 5, intermediate reboiler 6;
The intermediate reboiler includes side line material extraction pipe and feed back pipe.
3. the method that a kind of use low concentration DMF waste water systems as claimed in claim 1 are processed, with following steps:
1. need to DMF waste water to be processed be preheating to bubble point temperature through the waste water preheater as raw material after be passed through the rectifying Tower, rectifying obtains water vapour after separating in the rectifying column tower top, and vapor is condensed through the overhead condenser, the condensation for obtaining Liquid is directly produced through the rectifying column tower top water discharging opening, and the rectifying tower bottom provides mass transfer and pushes away through tower reactor reboiler heat supply Power, the DMF after isolated high temperature concentration is directly produced;
2. the stripping section of the rectifying column 2 passes through the intermediate reboiler (4), the intermediate reboiler (5), the intermediate reboiler (6) loop is formed;
3. 10%DMF is contained in the feedstock, first Intermediate Heat Exchanger (4) is positioned at the 37th block of plate, the liquid of extraction It is 7705.1kg/h to measure, and it is 102.4 DEG C to extract temperature out;Second Intermediate Heat Exchanger (5) extracts liquid out positioned at the 38th block of plate It is 543.1kg/h to measure, and it is 104.5 DEG C to extract temperature out;3rd Intermediate Heat Exchanger 6 is located at the 39th block of plate, extracts amount of liquid out It is 391.5kg/h, it is 111.7 DEG C to extract temperature out;
4. 20%DMF is contained in the feedstock, first Intermediate Heat Exchanger (4) is positioned at the 21st block of plate, the liquid of extraction It is 3692.6kg/h to measure, and it is 101.7 DEG C to extract temperature out;Second Intermediate Heat Exchanger (5) extracts liquid out positioned at the 25th block of plate It is 4835.8kg/h to measure, and it is 113.3 DEG C to extract temperature out.
CN201611167122.5A 2016-12-16 2016-12-16 A kind of multiple Intermediate Heat Exchanger rectification method treatment low concentration DMF waste water systems of band Pending CN106745421A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108079611A (en) * 2018-02-08 2018-05-29 燕山大学 A kind of intermediate reboiler step heating system based on absorption heat pump
CN108329227A (en) * 2018-03-13 2018-07-27 索闻特环保科技(上海)有限公司 Method of purification containing Dimethylformamide Residue
CN108529804A (en) * 2018-04-24 2018-09-14 浙江荣凯科技发展有限公司 A kind of dichloro-nicotinic acid production sewage treatment device
CN111004144A (en) * 2019-12-31 2020-04-14 山东三和维信生物科技有限公司 Low-concentration DMF concentration recovery process
CN113398618A (en) * 2020-03-17 2021-09-17 北京诺维新材科技有限公司 Method for improving distillation separation effect and distillation system

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US4419188A (en) * 1980-06-02 1983-12-06 Mccall Thomas F Thermally coupled extractive distillation process
CN104671307A (en) * 2015-03-03 2015-06-03 吴嘉 DMF (dimethyl formamide) wastewater treatment device and method
CN105814029A (en) * 2013-12-06 2016-07-27 国际壳牌研究有限公司 Improvements relating to propylene oxide purification

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
US4419188A (en) * 1980-06-02 1983-12-06 Mccall Thomas F Thermally coupled extractive distillation process
CN105814029A (en) * 2013-12-06 2016-07-27 国际壳牌研究有限公司 Improvements relating to propylene oxide purification
CN104671307A (en) * 2015-03-03 2015-06-03 吴嘉 DMF (dimethyl formamide) wastewater treatment device and method

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108079611A (en) * 2018-02-08 2018-05-29 燕山大学 A kind of intermediate reboiler step heating system based on absorption heat pump
CN108329227A (en) * 2018-03-13 2018-07-27 索闻特环保科技(上海)有限公司 Method of purification containing Dimethylformamide Residue
CN108329227B (en) * 2018-03-13 2021-03-09 索闻特环保科技(上海)有限公司 Method for purifying waste liquid containing dimethyl formamide
CN108529804A (en) * 2018-04-24 2018-09-14 浙江荣凯科技发展有限公司 A kind of dichloro-nicotinic acid production sewage treatment device
CN111004144A (en) * 2019-12-31 2020-04-14 山东三和维信生物科技有限公司 Low-concentration DMF concentration recovery process
CN113398618A (en) * 2020-03-17 2021-09-17 北京诺维新材科技有限公司 Method for improving distillation separation effect and distillation system

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