CN104671307A - DMF (dimethyl formamide) wastewater treatment device and method - Google Patents
DMF (dimethyl formamide) wastewater treatment device and method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000004065 wastewater treatment Methods 0.000 title claims abstract description 26
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 title abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 122
- 239000002351 wastewater Substances 0.000 claims abstract description 60
- 238000010992 reflux Methods 0.000 claims abstract description 41
- 238000004821 distillation Methods 0.000 claims description 76
- 239000012535 impurity Substances 0.000 claims description 22
- 239000000047 product Substances 0.000 claims description 22
- 238000000605 extraction Methods 0.000 claims description 19
- 239000000470 constituent Substances 0.000 claims description 18
- 239000006200 vaporizer Substances 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 13
- 239000012153 distilled water Substances 0.000 claims description 12
- 238000009833 condensation Methods 0.000 claims description 11
- 230000005494 condensation Effects 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 abstract description 6
- 239000002649 leather substitute Substances 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 7
- 239000007791 liquid phase Substances 0.000 description 6
- 238000005265 energy consumption Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 206010019663 Hepatic failure Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000003394 haemopoietic effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 208000007903 liver failure Diseases 0.000 description 1
- 231100000835 liver failure Toxicity 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000008234 soft water Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The invention provides a DMF (dimethyl formamide) wastewater treatment device and method. The device comprises a wastewater preheater, a reduced pressure rectifying column, a water vapor compressor, a reduced pressure rectifying column reboiler, a reduced pressure rectifying column reflux pump, an intermediate carburetor, a divided wall rectifying column, an intermediate vapor compressor, an intermediate reboiler, an intermediate condensate reflux pump, a DMF compressor, a divided wall rectifying column reboiler and a DMF conveying pump. According to the method, a rectifying system formed by the common reduced pressure rectifying column and the divided wall rectifying column is adopted to rectify DMF wastewater of synthetic leather to refine and recover DMF, meanwhile, effective energy-saving measures such as heat pump rectification and the like are used, a very good energy-saving effect is realized, and the product quality is high.
Description
Technical field
The invention belongs to field of waste water treatment, be specifically related to a kind of DMF wastewater treatment equipment and method.
Background technology
Urethane (PU) synthetic leather results from 20th century late nineteen seventies, develop the nineties in 20th century, be an important component part of plastics industry, be widely used in national economy every profession and trade, its Application Areas is throughout the every aspect of people's daily life.The production of synthetic leather generally adopts urethane as the basic raw material of basic unit and surface layer, pass through N, N-dimethylformamides (DMF) etc. obtain with solution polymerization process as primary solvent, the consumption of solvent accounts for greatly more than 60% of resin demand, and the consumption of wet process furnish DMF reaches more than 70%.DMF has bio-toxicity, and human body Long Term Contact or suction can hinder hematopoietic function and cause liver failure, and DMF is difficult to biological degradation simultaneously, can cause severe contamination to large G&W.In the production technique of synthetic leather, DMF is mainly used in batching dilution, all can produce a large amount of DMF waste gas, absorb DMF form waste water with water in dry, wet production.In addition, in wet production, urethane solidifies and DMF leaches in water, produces a large amount of DMF waste water.In order to eliminate the impact of waste water on environment, also in order to reduce production cost, must recycle to recycle or sell as byproduct to DMF waste water.The recovery of current DMF adopts rectificating method mostly, and the cost recovery of about 80% is used for heat energy consumption, there is the problem of high energy consumption.
Current domestic use is more is double tower DMF recovery technology, low-pressure steam or thermal oil is used to be heating agent, form with rectification under vacuum double tower by normal pressure is concentrated, DMF waste water first removes a part of water through atmospheric distillation, then obtain pure DMF through rectification under vacuum, this technique recovery technology is relatively backward, and energy consumption is high, DMF quality is unstable, and the rate of recovery is lower.Because double tower DMF recovery technology energy consumption is high, domestic from 2004, carry out three tower DMF recovery technology research and development and industrialization test.This technique is made up of two concentrating under reduced pressure towers and an atmospheric distillation tower.DMF waste water, respectively by a part of water of the concentrated removing of two-stage decompression, then obtains pure DMF by atmospheric distillation.Because under condition of normal pressure, DMF boiling point is higher, low-pressure steam cannot meet heating requirements, therefore uses thermal oil or middle pressure steam as heating agent.Document is had to propose a kind of energy-saving three tower DMF new recovering technology, employing one-level concentrating under reduced pressure, secondary atmospheric concentrate, three tower recovery process of rectification under vacuum, improve the processing power of two tower process, but energy-saving effect are poor, take up room large, equipment cost is higher.
Summary of the invention
One of the object of the invention is to provide a kind of DMF wastewater treatment equipment and method, the DMF steady quality that the present invention reclaims, and the rate of recovery is high, overcomes above-mentioned technical energy saving weak effect simultaneously, takes up room large, the problem that equipment cost is higher.
A kind of DMF wastewater treatment equipment provided by the invention, comprises waste water preheater, vacuum rectification tower, water vapor compressor, vacuum rectification tower reboiler, vacuum rectification tower reflux pump, middle vaporizer, divided-wall distillation column, intermediate steam compressor, intermediate reboiler, intermediate condensation liquid reflux pump, DMF compressor, divided-wall distillation column reboiler and DMF transferpump.
Waste water preheater connects vacuum rectification tower, rectification under vacuum column overhead connects water vapor compressor, water vapor compressor connects vacuum rectification tower by vacuum rectification tower reboiler, in vacuum rectification tower, hypomere forms loop by connecting vacuum rectification tower reboiler, vacuum rectification tower reboiler connects vacuum rectification tower and distilled water discharge port by vacuum rectification tower reflux pump, divided-wall distillation column is connected by middle vaporizer at the bottom of vacuum rectification tower tower, the opening for feed side tower top of divided-wall distillation column connects intermediate reboiler by intermediate steam compressor, opening for feed side, divided-wall distillation column middle and lower part forms loop by connecting intermediate reboiler, intermediate reboiler connects divided-wall distillation column opening for feed side and waste water preheater opening for feed by intermediate condensation liquid reflux pump, divided-wall distillation column connects divided-wall distillation column reboiler away from the side tower top of opening for feed by DMF compressor, divided-wall distillation column middle and lower part forms loop away from the side of opening for feed by connecting divided-wall distillation column reboiler, divided-wall distillation column reboiler connects divided-wall distillation column away from the side of opening for feed and DMF outlet for product by DMF transferpump, heavy constituent impurity discharge port is connected at the bottom of divided-wall distillation column tower.
Present invention also offers a kind of DMF wastewater treatment equipment, comprise waste water preheater, vacuum rectification tower, water vapor compressor, vacuum rectification tower reboiler, vacuum rectification tower reflux pump, middle vaporizer, except water tower, DMF rectifying tower, intermediate steam compressor, except water tower reboiler, except water tower condensate reflux pump, DMF compressor, DMF rectifying tower reboiler and DMF transferpump;
Waste water preheater connects vacuum rectification tower, rectification under vacuum column overhead connects water vapor compressor, water vapor compressor connects vacuum rectification tower by vacuum rectification tower reboiler, in vacuum rectification tower, hypomere forms loop by connecting vacuum rectification tower reboiler, vacuum rectification tower reboiler connects vacuum rectification tower and distilled water discharge port by vacuum rectification tower reflux pump, connect except water tower by middle vaporizer at the bottom of vacuum rectification tower tower, the column overhead that dewaters connects except water tower reboiler by intermediate steam compressor, except water tower middle and lower part is by connecting except water tower reboiler forms loop, except water tower reboiler is by connecting except water tower and waste water preheater opening for feed except water tower condensate reflux pump, except connecting DMF rectifying tower opening for feed at the bottom of water tower tower, DMF rectifying tower tower top connects DMF rectifying tower reboiler by DMF compressor, DMF rectifying tower middle and lower part forms loop by connecting DMF rectifying tower reboiler, DMF rectifying tower reboiler connects DMF rectifying tower and DMF outlet for product by DMF transferpump, heavy constituent impurity discharge port is connected at the bottom of DMF rectifying tower.
Present invention also offers a kind of DMF method of wastewater treatment, comprise the steps:
Vacuum rectification tower need be passed into after waste water preheater preheats together with recycle stock by DMF waste water to be processed as raw material, water vapor is obtained at rectification under vacuum tower top after rectifying separation, it is the heat supply of vacuum rectification tower reboiler that water vapor improves after vapor temperature through water vapor compressor compresses, the phlegma obtained is back to vacuum rectification tower through a vacuum rectification tower reflux pump part, and a part is by the direct extraction of distilled water discharge port;
Obtain the DMF waste water after concentrating at the bottom of vacuum rectification tower tower, pass in the divided-wall distillation column of a shared stripping section after middle vaporizer is heat vaporized, carry out rectification process;
Obtain the water vapor containing a small amount of DMF with the side tower top of opening for feed homonymy in divided-wall distillation column, improving after vapor temperature through intermediate steam compressor compresses is intermediate reboiler heat supply, the phlegma obtained is by intermediate condensation liquid reflux pump, a part is back to divided-wall distillation column, a part, as recycle stock, again through waste water preheater enters vacuum rectification tower after mixing with DMF waste water raw material;
The DMF steam refined is obtained at the opposite side tower top of divided-wall distillation column, improving after vapor temperature through DMF compressor compresses is the heat supply of divided-wall distillation column reboiler, the phlegma obtained is by DMF transferpump, a part is back to divided-wall distillation column, a part as DMF product through the extraction of DMF outlet for product;
The heavy constituent impurity obtained at the bottom of divided-wall distillation column tower is through the extraction of heavy constituent impurity discharge port.
Present invention also offers a kind of DMF method of wastewater treatment, comprise the steps:
Vacuum rectification tower need be passed into after waste water preheater preheats together with recycle stock by DMF waste water to be processed as raw material, water vapor is obtained in rectification under vacuum column overhead after rectifying separation, it is the heat supply of vacuum rectification tower reboiler that water vapor improves after vapor temperature through water vapor compressor compresses, the phlegma obtained is back to vacuum rectification tower through a vacuum rectification tower reflux pump part, and a part is by the direct extraction of distilled water discharge port;
Obtain the DMF waste water after concentrating at the bottom of vacuum rectification tower tower, pass into after middle vaporizer is heat vaporized except water tower, carry out rectification process;
The water vapor containing a small amount of DMF is obtained in the column overhead that dewaters, improve after vapor temperature through intermediate steam compressor compresses, for removing the heat supply of water tower reboiler, the phlegma obtained is by removing water tower condensate reflux pump, a part is back to except water tower, a part, as recycle stock, again through waste water preheater enters vacuum rectification tower after mixing with DMF waste water raw material;
Except the material obtained at the bottom of water tower tower enters DMF rectifying tower, the DMF steam refined is obtained at DMF rectifying tower tower top, improve after vapor temperature through DMF compressor compresses, for the heat supply of DMF rectifying tower reboiler, the phlegma obtained is by DMF transferpump, a part is back to DMF rectifying tower, a part as DMF product through the extraction of DMF outlet for product;
The heavy constituent impurity obtained at the bottom of DMF rectifying tower is through the extraction of heavy constituent impurity discharge port.
Further, the service temperature of vacuum rectification tower is 70-110 DEG C, and working pressure is 0.05-0.1MPa, and trim the top of column ratio is 0.8 ~ 7.
Further, the service temperature of divided-wall distillation column is 80-120 DEG C, and working pressure is 0.01-0.1MPa, and the trim the top of column ratio of opening for feed side is 0.5 ~ 3, and the trim the top of column ratio away from opening for feed side is 0.2 ~ 2.
Further, service temperature except water tower is the service temperature of 80-120 DEG C, DMF rectifying tower is 90-130 DEG C, except the working pressure of water tower and DMF rectifying tower is 0.01-0.1MPa, the column overhead that dewaters reflux ratio is 0.5 ~ 4, DMF rectifying column top return ratio is 0.5 ~ 3.
Beneficial effect of the present invention is:
(1) have employed heat pump distillation, the low grade heat energy of rectifying tower tower top is converted into higher-grade heat energy, for reboiler heat supply, Appropriate application heat, instead of the use of low pressure or middle pressure steam, greatly reduce process energy consumption, reach energy-saving and cost-reducing object, compared with traditional three tower process, can save energy more than 50%, also reduce overhead condenser, the use both having decreased water coolant again reduces facility investment simultaneously;
(2) have employed vacuum rectification tower and divided-wall distillation column two tower process integration, compared with traditional three tower process, operation capacity is large, and energy-saving effect is remarkable, and reduces by a tower, thus decreases floor space, has saved facility investment;
(3) through the refining water that obtains and DMF product purity all very high, quality is good, and DMF product can be recycled, and also can directly sell as product, and water can be used as the use of technique soft water, decreases the discharge of waste water.
Accompanying drawing explanation
Figure 1 shows that DMF wastewater treatment equipment structural representation in the embodiment of the present invention 1.
Figure 2 shows that DMF wastewater treatment equipment structural representation in the embodiment of the present invention 2.
Embodiment
Hereafter will describe the present invention in detail in conjunction with specific embodiments.It should be noted that the combination of technical characteristic or the technical characteristic described in following embodiment should not be considered to isolated, they can mutually be combined thus be reached better technique effect.
Embodiment 1
Divided-wall distillation column (Dividing Wall Column, be called for short DWC) be that a vertical wall is set in rectifying tower, also vertical wall can be extended at the bottom of tower top or tower, DWC tower can be had common rectifying section or stripping section by two portions that partition wall separates, or has common rectifying section and stripping section simultaneously.DWC tower is comparatively ideal system architecture on thermodynamics, when separation 3 component mixture, with identical number of theoretical plate, completes same separation task, adopts DWC tower to need less boiling hot again amount and condensation number than traditional two-tower process.For the material that some is given, divided-wall distillation column compares reflux ratio that need be less with conventional rectification tower, therefore operation capacity increases, and energy-conservationly can reach more than 60%, may save facility investment 30%.DWC tower can be widely used in refining of petroleum, petrochemical complex, chemical and gas delivery.
The invention provides a kind of DMF method of wastewater treatment, the distillation system that the method uses common vacuum rectification tower and divided-wall distillation column to form carries out rectified purifiedly reclaiming DMF to DMF waste water, employ the effective conservation measuress such as heat pump distillation simultaneously, have good energy-saving effect, the quality product obtained is high.
Figure 1 shows that DMF wastewater treatment equipment structural representation in the embodiment of the present invention 1.
As shown in Figure 1, a kind of DMF wastewater treatment equipment provided by the invention, comprises waste water preheater 1, vacuum rectification tower 2, water vapor compressor 3, vacuum rectification tower reboiler 4, vacuum rectification tower reflux pump 5, middle vaporizer 6, divided-wall distillation column 7, intermediate steam compressor 8, intermediate reboiler 9, intermediate condensation liquid reflux pump 10, DMF compressor 11, divided-wall distillation column reboiler 12 and DMF transferpump 13;
Waste water preheater 1 connects vacuum rectification tower 2, vacuum rectification tower 2 tower top connects water vapor compressor 3, water vapor compressor 3 connects vacuum rectification tower 2 by vacuum rectification tower reboiler 4, in vacuum rectification tower 2, hypomere forms loop by connecting vacuum rectification tower reboiler 4, vacuum rectification tower reboiler 4 connects vacuum rectification tower 2 and distilled water discharge port 14 by vacuum rectification tower reflux pump 5, divided-wall distillation column 7 is connected by middle vaporizer 6 at the bottom of vacuum rectification tower 2 tower, the opening for feed side tower top of divided-wall distillation column 7 connects intermediate reboiler 9 by intermediate steam compressor 8, opening for feed side, divided-wall distillation column 7 middle and lower part forms loop by connecting intermediate reboiler 9, intermediate reboiler 9 connects divided-wall distillation column 7 opening for feed side and waste water preheater 1 opening for feed by intermediate condensation liquid reflux pump 10, divided-wall distillation column 7 connects divided-wall distillation column reboiler 12 away from the side tower top of opening for feed by DMF compressor 11, divided-wall distillation column 7 middle and lower part forms loop away from the side of opening for feed by connecting divided-wall distillation column reboiler 12, divided-wall distillation column reboiler 12 connects divided-wall distillation column 7 away from the side of opening for feed and DMF outlet for product 15 by DMF transferpump 13, heavy constituent impurity discharge port 16 is connected at the bottom of divided-wall distillation column 7 tower.
Vacuum rectification tower reboiler 4 in this device, intermediate reboiler 9 and divided-wall distillation column reboiler 12 are the equipment of the vaporizing liquid making to be distillated, and general being combined with rectifying tower forms loop.The liquid phase stream gone out from rectifying tower underflow enters into reboiler, in reboiler, usually have the liquid of 25-30% to be vaporized.The gaseous component be vaporized is sent back in rectifying tower, and flows upwards through tower tray, and liquid phase component turns back at the bottom of tower.Vacuum rectification tower 2 and divided-wall distillation column 7 form loop by corresponding reboiler, thus provide upflowing vapor for rectifying tower inside, carry out vapour-liquid mass, ensure the carrying out of rectifying with the liquid phase stream in tower.
A kind of DMF method of wastewater treatment provided by the invention, comprises the steps:
Vacuum rectification tower 2 need be passed into after waste water preheater 1 preheating together with recycle stock by DMF waste water to be processed as raw material, water vapor is obtained at vacuum rectification tower 2 tower top after rectifying separation, it is vacuum rectification tower reboiler 4 heat supply that water vapor compresses after raising vapor temperature through water vapor compressor 3, the phlegma obtained is through vacuum rectification tower reflux pump 5, a part is back to vacuum rectification tower 2, and a part is by distilled water discharge port 14 directly extraction;
At the bottom of vacuum rectification tower 2 tower, obtain the DMF waste water after concentrating, pass into from opening for feed the divided-wall distillation column 7 of a shared stripping section after middle vaporizer 6 is heat vaporized, carry out rectification process;
Obtain the water vapor containing a small amount of DMF with the side tower top of opening for feed homonymy in divided-wall distillation column 7, compressing after raising vapor temperature through intermediate steam compressor 8 is intermediate reboiler 9 heat supply, the phlegma obtained is by intermediate condensation liquid reflux pump 10, a part is back to divided-wall distillation column 7, a part, as recycle stock, again through waste water preheater 1 enters vacuum rectification tower 2 after mixing with DMF waste water raw material;
The DMF steam refined is obtained at the opposite side tower top of divided-wall distillation column 7, compressing after raising vapor temperature through DMF compressor 11 is divided-wall distillation column reboiler 12 heat supply, the phlegma obtained is by DMF transferpump 13, a part is back to divided-wall distillation column 7, a part as DMF product through DMF outlet for product 15 extraction;
The heavy constituent impurity obtained at the bottom of divided-wall distillation column 7 tower is through the extraction of heavy constituent impurity discharge port 16.
In DMF waste water, main component is DMF and water, and wherein the weight percent content of DMF is 10 ~ 80%, in addition also containing one or more in the components such as saline and alkaline, ketone, ester class or other organism on a small quantity, and the composition impurity and these impurity are attached most importance to.
Vacuum rectification tower 2 service temperature is 70-110 DEG C, and working pressure is 0.05-0.1MPa, and trim the top of column ratio is 0.8 ~ 7.
Divided-wall distillation column 7 service temperature is 80-120 DEG C, and working pressure is 0.01-0.1MPa, and the trim the top of column ratio of opening for feed side is 0.5 ~ 3, and the trim the top of column ratio away from opening for feed side is 0.2 ~ 2.
Embodiment 2
Figure 2 shows that DMF wastewater treatment equipment structural representation in the embodiment of the present invention 2.
As shown in Figure 2, a kind of DMF wastewater treatment equipment provided by the invention, comprise waste water preheater 1, vacuum rectification tower 2, water vapor compressor 3, vacuum rectification tower reboiler 4, vacuum rectification tower reflux pump 5, middle vaporizer 6, except water tower 17, DMF rectifying tower 20, intermediate steam compressor 8, except water tower reboiler 18, except water tower condensate reflux pump 19, DMF compressor 11, DMF rectifying tower reboiler 21 and DMF transferpump 13;
Waste water preheater 1 connects vacuum rectification tower 2, vacuum rectification tower 2 tower top connects water vapor compressor 3, water vapor compressor 3 connects vacuum rectification tower 2 by vacuum rectification tower reboiler 4, in vacuum rectification tower 2, hypomere forms loop by connecting vacuum rectification tower reboiler 4, vacuum rectification tower reboiler 4 connects vacuum rectification tower 2 and distilled water discharge port 14 by vacuum rectification tower reflux pump 5, connect by middle vaporizer 6 17 towers that dewater at the bottom of vacuum rectification tower 2 tower, except water tower 17 tower top connects except water tower reboiler 18 by intermediate steam compressor 8, except water tower 17 middle and lower part is by connecting except water tower reboiler 18 forms loop, except water tower reboiler 18 is by connecting except water tower 17 and waste water preheater 1 opening for feed except water tower condensate reflux pump 19, except connecting DMF rectifying tower 20 opening for feed at the bottom of water tower 17 tower, DMF rectifying tower 20 tower top connects DMF rectifying tower reboiler 21 by DMF compressor 11, DMF rectifying tower 20 middle and lower part forms loop by connecting DMF rectifying tower reboiler 21, DMF rectifying tower reboiler 21 connects DMF rectifying tower 20 and DMF outlet for product 15 by DMF transferpump 13, heavy constituent impurity discharge port 16 is connected at the bottom of DMF rectifying tower 20 tower.
The middle vacuum rectification tower reboiler 4 of this device, be the equipment of the vaporizing liquid making to be distillated except water tower reboiler 18 and DMF rectifying tower reboiler 21, general being combined with rectifying tower forms loop.The liquid phase stream gone out from rectifying tower underflow enters into reboiler, in reboiler, usually have the liquid of 25-30% to be vaporized.The gaseous component be vaporized is sent back in rectifying tower, and flows upwards through tower tray, and liquid phase component turns back at the bottom of tower.Vacuum rectification tower 2, form loop by corresponding reboiler except water tower 17 and DMF rectifying tower 20, thus provide upflowing vapor for rectifying tower inside, carry out vapour-liquid mass with the liquid phase stream in tower, ensure the carrying out of rectifying.
A kind of DMF method of wastewater treatment, comprises the steps:
Vacuum rectification tower 2 need be passed into after waste water preheater 1 preheating together with recycle stock by DMF waste water to be processed as raw material, water vapor is obtained at vacuum rectification tower 2 tower top after rectifying separation, it is vacuum rectification tower reboiler 4 heat supply that water vapor compresses after raising vapor temperature through water vapor compressor 3, the phlegma obtained is back to vacuum rectification tower 2 through vacuum rectification tower reflux pump 5 part, and a part is by distilled water discharge port 14 directly extraction;
Obtain the DMF waste water after concentrating at the bottom of vacuum rectification tower 2 tower, pass into except water tower 17 carries out rectification process after middle vaporizer 6 is heat vaporized;
The water vapor containing a small amount of DMF is being obtained except water tower 17 tower top, compress after raising vapor temperature for removing water tower reboiler 18 heat supply through intermediate steam compressor 8, the phlegma obtained is by removing water tower condensate reflux pump 19, a part is back to except water tower 17, again enters vacuum rectification tower 2 through waste water preheater 1 after a part mixes with DMF waste water raw material as recycle stock;
Except the material obtained at the bottom of water tower 17 tower enters DMF rectifying tower 20, the DMF steam refined is obtained at DMF rectifying tower 20 tower top, compressing after raising vapor temperature through DMF compressor 11 is the heat supply of DMF rectifying tower reboiler 21, the phlegma obtained is by DMF transferpump 13, a part is back to DMF rectifying tower 20, a part as DMF product through DMF outlet for product 15 extraction;
The heavy constituent impurity obtained at the bottom of DMF rectifying tower 20 tower is through the extraction of heavy constituent impurity discharge port 16.
In DMF waste water, main component is DMF and water, and wherein the weight percent content of DMF is 10 ~ 80%, in addition also containing one or more in the components such as saline and alkaline, ketone, ester class or other organism on a small quantity, and the composition impurity and these impurity are attached most importance to;
Vacuum rectification tower 2 service temperature is 70-110 DEG C, and working pressure is 0.05-0.1MPa, and trim the top of column ratio is 0.8 ~ 7.
Service temperature except water tower 17 is 80-120 DEG C, the service temperature of DMF rectifying tower 20 is 90-130 DEG C, except the working pressure of water tower 17 and DMF rectifying tower 20 is 0.01-0.1MPa, be 0.5 ~ 3 except water tower 17 trim the top of column ratio is 0.5 ~ 4, DMF rectifying tower 20 trim the top of column ratio.
The present invention adopts tower top direct type heat pump distillation: rectifying tower ejects material steam and enters after vacuum pump is elevated to higher pressure and temperature, enter corresponding reboiler, it is reboiler heat supply that vapor condensation releases heat, and the backflow of a phlegma part, a part is as discharging extraction.
The application of heat pump distillation technology, Appropriate application heat, makes low-grade thermal energy to be high-grade heat energy, replace the use of raw steam, substantially reduce the consumption of raw steam, decrease the consumption of recirculated cooling water simultaneously, reach energy-saving and cost-reducing object; Decrease overhead condenser in addition, reduce facility investment, also reduce floor space.
Although give some embodiments of the present invention, it will be understood by those of skill in the art that without departing from the spirit of the invention herein, can change embodiment herein.Above-described embodiment is exemplary, should using embodiment herein as the restriction of interest field of the present invention.
Claims (7)
1. a DMF wastewater treatment equipment, it is characterized in that, comprise waste water preheater, vacuum rectification tower, water vapor compressor, vacuum rectification tower reboiler, vacuum rectification tower reflux pump, middle vaporizer, divided-wall distillation column, intermediate steam compressor, intermediate reboiler, intermediate condensation liquid reflux pump, DMF compressor, divided-wall distillation column reboiler and DMF transferpump;
Described waste water preheater connects described vacuum rectification tower, described rectification under vacuum column overhead connects described water vapor compressor, described water vapor compressor connects described vacuum rectification tower by described vacuum rectification tower reboiler, in described vacuum rectification tower, hypomere forms loop by connecting described vacuum rectification tower reboiler, described vacuum rectification tower reboiler connects described vacuum rectification tower and distilled water discharge port by described vacuum rectification tower reflux pump, described divided-wall distillation column is connected by described middle vaporizer at the bottom of described vacuum rectification tower tower, the opening for feed side tower top of described divided-wall distillation column connects described intermediate reboiler by described intermediate steam compressor, opening for feed side, described divided-wall distillation column middle and lower part forms loop by connecting described intermediate reboiler, described intermediate reboiler connects described divided-wall distillation column opening for feed side and waste water preheater opening for feed by described intermediate condensation liquid reflux pump, described divided-wall distillation column connects described divided-wall distillation column reboiler away from the side tower top of opening for feed by described DMF compressor, described divided-wall distillation column middle and lower part forms loop away from the side of opening for feed by connecting described divided-wall distillation column reboiler, described divided-wall distillation column reboiler connects described divided-wall distillation column away from the side of opening for feed and DMF outlet for product by described DMF transferpump, heavy constituent impurity discharge port is connected at the bottom of described divided-wall distillation column tower.
2. a DMF wastewater treatment equipment, it is characterized in that, comprise waste water preheater, vacuum rectification tower, water vapor compressor, vacuum rectification tower reboiler, vacuum rectification tower reflux pump, middle vaporizer, except water tower, DMF rectifying tower, intermediate steam compressor, except water tower reboiler, except water tower condensate reflux pump, DMF compressor, DMF rectifying tower reboiler and DMF transferpump;
Described waste water preheater connects described vacuum rectification tower, described rectification under vacuum column overhead connects described water vapor compressor, described water vapor compressor connects described vacuum rectification tower by described vacuum rectification tower reboiler, in described vacuum rectification tower, hypomere forms loop by connecting described vacuum rectification tower reboiler, described vacuum rectification tower reboiler connects described vacuum rectification tower and distilled water discharge port by described vacuum rectification tower reflux pump, connected described except water tower at the bottom of described vacuum rectification tower tower by described middle vaporizer, the described column overhead that dewaters connects described except water tower reboiler by described intermediate steam compressor, described except passing through described in connection except water tower reboiler forms loop water tower middle and lower part, the described water tower reboiler that removes removes water tower and waste water preheater opening for feed by described except the connection of water tower condensate reflux pump is described, described except connecting DMF rectifying tower opening for feed at the bottom of water tower tower, described DMF rectifying tower tower top connects described DMF rectifying tower reboiler by described DMF compressor, described DMF rectifying tower middle and lower part forms loop by connecting described DMF rectifying tower reboiler, described DMF rectifying tower reboiler connects described DMF rectifying tower and DMF outlet for product by described DMF transferpump, heavy constituent impurity discharge port is connected at the bottom of described DMF rectifying tower.
3. a DMF method of wastewater treatment, is characterized in that, comprises the steps:
Described vacuum rectification tower need be passed into after described waste water preheater preheats together with recycle stock by DMF waste water to be processed as raw material, water vapor is obtained in described rectification under vacuum column overhead after rectifying separation, water vapor improves after vapor temperature through described water vapor compressor compresses, for the heat supply of described vacuum rectification tower reboiler, the phlegma obtained is through described vacuum rectification tower reflux pump, a part is back to described vacuum rectification tower, and a part is by the direct extraction of described distilled water discharge port;
Obtain the DMF waste water after concentrating at the bottom of described vacuum rectification tower tower, pass into after described middle vaporizer is heat vaporized in the described divided-wall distillation column of a shared stripping section, carry out rectification process;
Obtain the water vapor containing a small amount of DMF with the side tower top of opening for feed homonymy in described divided-wall distillation column, improve after vapor temperature through described intermediate steam compressor compresses, for described intermediate reboiler heat supply, the phlegma obtained is by described intermediate condensation liquid reflux pump, a part is back to described divided-wall distillation column, a part, as recycle stock, again through described waste water preheater enters vacuum rectification tower after mixing with DMF waste water raw material;
The DMF steam refined is obtained at the opposite side tower top of described divided-wall distillation column, improve after vapor temperature through described DMF compressor compresses, for the heat supply of described divided-wall distillation column reboiler, the phlegma obtained is by described DMF transferpump, a part is back to a point described next door rectifying tower, a part as DMF product through the extraction of described DMF outlet for product;
The heavy constituent impurity obtained at the bottom of described divided-wall distillation column tower is through the extraction of described heavy constituent impurity discharge port.
4. a DMF method of wastewater treatment, is characterized in that, comprises the steps:
Described vacuum rectification tower need be passed into after described waste water preheater preheats together with recycle stock by DMF waste water to be processed as raw material, water vapor is obtained in described rectification under vacuum column overhead after rectifying separation, water vapor improves after vapor temperature through described water vapor compressor compresses, for the heat supply of described vacuum rectification tower reboiler, the phlegma obtained is through described vacuum rectification tower reflux pump, a part is back to described vacuum rectification tower, and a part is by the direct extraction of described distilled water discharge port;
Obtain the DMF waste water after concentrating at the bottom of described vacuum rectification tower tower, pass into except water tower after described middle vaporizer is heat vaporized, carry out rectification process;
The water vapor containing a small amount of DMF is obtained in the described column overhead that dewaters, improve after vapor temperature through described intermediate steam compressor compresses, for described except the heat supply of water tower reboiler, the phlegma obtained removes water tower condensate reflux pump by described, a part is back to described except water tower, a part, as recycle stock, again through described waste water preheater enters vacuum rectification tower after mixing with DMF waste water raw material;
The described material except obtaining at the bottom of water tower tower enters described DMF rectifying tower, the DMF steam refined is obtained at described DMF rectifying tower tower top, improve after vapor temperature through described DMF compressor compresses, for the heat supply of described DMF rectifying tower reboiler, the phlegma obtained is by described DMF transferpump, a part is back to described DMF rectifying tower, a part as DMF product through the extraction of described DMF outlet for product;
The heavy constituent impurity obtained at the bottom of described DMF rectifying tower is through the extraction of described heavy constituent impurity discharge port.
5. a kind of DMF method of wastewater treatment as described in any one of claim 3 or 4, is characterized in that, the service temperature of described vacuum rectification tower is 70-110 DEG C, and working pressure is 0.05-0.1MPa, and trim the top of column ratio is 0.8 ~ 7.
6. a kind of DMF method of wastewater treatment as claimed in claim 3, it is characterized in that, the service temperature of described divided-wall distillation column is 80-120 DEG C, and working pressure is 0.01-0.1MPa, the trim the top of column ratio of opening for feed side is 0.5 ~ 3, and the trim the top of column ratio away from opening for feed side is 0.2 ~ 2.
7. a kind of DMF method of wastewater treatment as claimed in claim 4, it is characterized in that, the described service temperature except water tower is 80-120 DEG C, the service temperature of described DMF rectifying tower is 90-130 DEG C, the described working pressure except water tower and DMF rectifying tower is 0.01-0.1MPa, the described column overhead reflux ratio that dewaters is 0.5 ~ 4, and described DMF rectifying column top return ratio is 0.5 ~ 3.
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