CN104370768B - The distillation purifying method and apparatus of low concentration DMAc in waste water containing a small amount of low-boiling-point substance and high-boiling components - Google Patents
The distillation purifying method and apparatus of low concentration DMAc in waste water containing a small amount of low-boiling-point substance and high-boiling components Download PDFInfo
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
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Abstract
The distillation purifying method and apparatus of low concentration DMAc in waste water containing a small amount of low-boiling-point substance and high-boiling components, relates to the distillation purifying method and apparatus containing less dimethyl acetylamide waste water; Including decompression, the step of low temperature multistage concentration and the step of evaporation, rectification. Equipment includes: primary concentrating tower, secondary concentrating tower, three grades of concentration towers, evaporator, level Four concentration tower, rectifying column, extracting towers. The advantages such as the present invention has and present invention aim to address above-mentioned the deficiencies in the prior art, it is provided that a kind of energy consumption is low, the response rate is high, DMAc decomposition of little, and in free from environmental pollution, overhead water, COD content is few, energy-conserving and environment-protective.
Description
Technical field
The present invention relates to a kind of distillation purifying method containing less dimethyl acetylamide (DMAc) waste water; Say it is that a kind of capacity usage ratio is high in detail, save the energy, DMAc decomposition of little, it is to avoid the distillation purifying method and apparatus of low concentration DMAc in the waste water containing a small amount of low-boiling-point substance and high-boiling components that blowdown is polluted.
Background technology
Along with shortage and the pollution of water resources in china, Membrane Separation for Water Treatment is applied to multiple water treatment field such as municipal water use, enterprise's sewage more and more widely. And hollow-fibre membrane is as the core of Membrane Separation for Water Treatment and easily-consumed products, demand is skyrocketed through. In hollow-fibre membrane manufacture process, DMAc is mainly used as solvent, for instance the solvent of polymer during synthetic fibers spinning, or solvent of polymer etc. during as doughnut film preparation. In order to obtain high-quality product in hollow-fibre membrane spinning, require that the DMAc used meets following specification: water content < 200ppm, acetic acid < 50ppm, dimethylamine < 30ppm, pH is 6.5-7.5, electrical conductivity < 0.6 �� S/cm. Meet the DMAc of above-mentioned specification requirement hereinafter referred to as pure DMAc
It is reported, China has more than 500 hollow-fibre membrane manufacturing enterprises at present, and is wherein mostly middle and small scale, and the waste water DMAc content of generation is below 10%, and enterprise does not possess the voluntary recall purification ability containing DMAc waste liquid. If these waste water can not get effective process, it will severe contamination soil, subsoil water or even whole ecological environment. Purification difficult point containing DMAc waste water is in that processing cost, wherein energy consumption cost is most important of which part, and the purification of unit mass DMAc, required processing cost (includes energy consumption cost, human cost, equipment depreciation cost etc.) and DMAc concentration in initial waste liquid is inversely proportional to. Existing for DMAc concentration about 10% sewage treatment equipment and method, the pure DMAc reclaimed after separation and purification treatment is worth and can balance with processing cost, and for the wastewater treatment lower than 10% of the DMAc concentration, is in lossing state, and concentration is more low, lose more serious.Under the situation that environmental requirement is increasingly strict, the DMAc Waste Water Centralized of generation is often delivered to specialty separation purification unit and is processed by Yangtze River Delta Area relevant enterprise. And the wastewater treatment expense of great number so that the enterprise being originally at harmful competition profit meagre makes the matter worse. DMAc purification process disclosed in the patent of invention of Chinese patent (publication number: 102030672A), for spandex production process reclaims ultra-pure DMAc solvent, but its scope of application is limited only to the waste water that DMAc concentration is 20% to 70%, for the DMAc concentration waste water lower than 10%, it is difficult to obtain high-purity DMAc by the method. DMAc purification process disclosed in another Chinese patent (publication number: 100341848), adopts normal pressure or slightly above condition of normal pressure, rectifying column tower top temperature be about 70 DEG C-115 DEG C, bottom temperature be about 150 DEG C-180 DEG C, obtain pure DMAc. But, the method is higher due to operation temperature, adds energy consumption, also easily makes DMAc resolve into the small-molecule substance such as acetic acid, dimethylamine, adds the burden of finished product deacidification and the de-amine of overhead water and easily causes secondary pollution.
Summary of the invention
Present invention aim to address above-mentioned the deficiencies in the prior art, energy consumption is low, the response rate is high to provide one, DMAc decomposition of little, in free from environmental pollution, overhead water, COD content is few, the distillation purifying method and apparatus of low concentration DMAc in the waste water containing a small amount of low-boiling-point substance and high-boiling components of energy-conserving and environment-protective.
This invention address that above-mentioned the deficiencies in the prior art, be the technical scheme is that
A kind of distillation purifying method of low concentration DMAc in waste water containing a small amount of low-boiling-point substance and high-boiling components, it is characterised in that comprise the following steps:
Step 1: the waste water containing 1-10%DMAc, low-boiling-point substance and high-boiling components is sent into primary concentrating tower through raw liquor pump and carries out primary concentration, primary concentrating tower column bottom temperature 42-46 DEG C, tower top temperature 39-43 DEG C;
Step 2: sent into secondary concentrating tower by one-level discharging pump when DMAc concentration promotes 0.2%-0.5% in the tower bottoms of primary concentrating tower and carry out secondary concentration, secondary concentrating tower column bottom temperature 55 DEG C-59 DEG C, tower top temperature 52 DEG C-56 DEG C;
Step 3: DMAc concentration is delivered to three grades of concentration towers by two grades of discharging pumps and carried out three grades of concentrations when promoting 0.6%-1.5% in the tower bottoms of secondary concentrating tower, three grades of concentration tower column bottom temperatures 68 DEG C-72 DEG C, tower top temperature 65 DEG C-69 DEG C;
Step 4: DMAc concentration is sent into evaporator by three grades of discharging pumps when promoting 2%-3% in the tower bottoms of three grades of concentration towers, subsequently into feed heater, after carrying out heat exchange extremely boiling with steam, enter flash distillation in evaporator, air-liquid is made to separate, gas phase enters level Four concentration tower and carries out level Four concentration, level Four concentration tower column bottom temperature 81 DEG C-85 DEG C, tower top temperature 78 DEG C-82 DEG C; Feed heater continuation evaporation is entered through feed cycle pump after unevaporated liquid phase and the liquid mixing of three grades of discharging pumps feeding evaporators in evaporator;
Step 5: DMAc concentration is delivered in the middle part of rectifying column by level Four discharging pump when reaching 18%-25% in the tower bottoms of level Four concentration tower, under the combined effect with overhead reflux of the rectifying column reboiler, water is easily vaporized and step by step tray rising, and DMAc then step by step tray declines;
Step 6: DMAc is moisture < during 150ppm in tower bottom of rectifying tower, extracting tower is entered by tower bottom of rectifying tower liquid phase extraction, DMAc product, by extracting tower top side take-off, enters DMAc discharge tank after pure DMAc cooler cools down, then delivers to DMAc finished pot with DMAc discharging pump;
In above-mentioned steps, the temperature of one to three grade of concentration tower heating equipment controls to be regulated steam flow control by the steam control valve of each concentration tower; The Energy harvesting method of concentration towers at different levels, evaporator, rectifying column and extracting tower is: the reboiler of level Four concentration tower, feed heater, rectifying column reboiler and the extracting tower reboiler energy are primary steam (producing through vapour source) heating; The reboiler of level Four concentration tower overhead vapours three grades of concentration towers of heating, condensed water enters four column overhead flow containers; The reboiler of three grades of concentration tower overhead vapours heating secondary concentrating tower, condensed water enters three column overhead flow containers; The reboiler of secondary concentrating tower overhead vapours heating primary concentrating tower, condensed water enters two column overhead flow containers; Primary concentrating tower overhead vapours enters primary concentrating tower overhead condenser and becomes with recirculated water heat exchange to enter a column overhead flow container after liquid overhead water;
A primary concentrating tower overhead water part is sent back to primary concentrating tower by primary concentrating tower reflux pump, a part is pumped to two column overhead flow containers by primary concentrating tower water outlet, a secondary concentrating tower overhead water part is sent back to secondary concentrating tower by secondary concentrating tower reflux pump, a part is pumped to three column overhead flow containers by secondary concentrating tower water outlet, three grades of concentration tower overhead water parts are sent back to three grades of concentration towers by three grades of concentration tower reflux pumps, a part is pumped to four column overhead flow containers by three grades of concentration tower water outlets, a level Four concentration tower overhead water part is sent back to level Four concentration tower by level Four concentration tower reflux pump, a part is pumped into tank field tower top water pot by four tower water outlets and returns production line and reuse or send into treatment tank and process,
Rectifying column overhead vapours enters rectifying column overhead condenser and becomes liquid overhead water with recirculated water heat exchange, and a part is by rectifier column reflux pumped back rectifying column, and a part is pumped to four column overhead water pots by rectifying column water outlet; Extracting tower overhead vapours enters DMAc condenser and becomes liquid DMAc with recirculated water heat exchange, is all sent back to extracting tower by DMAc reflux pump; Four concentration towers, rectifying column and extracting tower are vacuumizing, its vacuum be respectively as follows: primary concentrating tower between-0.09MPa to-0.095MPa, secondary concentrating tower between-0.08MPa to-0.086MPa, three grades of concentration towers between-0.06MPa to-0.07MPa, level Four concentration tower between-0.04MPa to-0.052MPa, rectifying column between-0.085MPa to-0.095MPa, extracting tower is between-0.08MPa to-0.09MPa. Vacuum is undertaken aspirating, being automatically adjusted by vacuum pump.
In heretofore described evaporator, unevaporated liquid phase is after equipment works 120 hours, often process 1 ~ 3 hour waste water, the liquid phase entrance drying machine being discharged evaporator volume 1% ~ 3% by the slag-drip opening of evaporator is predrying, often processing 6 days waste water, the fluid after drying machine inner drying is pumped into screw extruder extrusion PVP by PVP heavy liquor pump.
A kind ofThe distillation purifying of low concentration DMAc in waste water containing a small amount of low-boiling-point substance and high-boiling componentsEquipment, it is characterised in that including: primary concentrating tower, secondary concentrating tower, three grades of concentration towers, evaporator, level Four concentration tower, rectifying column, extracting towers, the outlet of primary concentrating tower overhead vapours is connected with primary concentrating tower tower top flow container import through overhead condenser, the outlet of primary concentrating tower tower top flow container is connected with primary concentrating tower filler and secondary concentrating tower tower top flow container entrance with primary effluent pump through one-level reflux pump respectively, primary concentrating tower discharging pump is connected with secondary concentrating tower charging aperture, the outlet of secondary concentrating tower overhead vapours is connected with the reboiler thermal source inlet of primary concentrating tower, the reboiler thermal source outlet of primary concentrating tower is connected with the tower top flow container entrance of secondary concentrating tower, the outlet of secondary concentrating tower tower top flow container is connected with secondary concentrating tower filler and three grades of concentration tower tower top flow container entrances with secondary effluent pump through two grades of reflux pumps respectively, secondary concentrating tower discharging pump and three grades of concentration tower charging apertures are connected, and three grades of concentration tower overhead vapours outlets are connected with the reboiler thermal source inlet of secondary concentrating tower, and the tower top flow container entrance of the reboiler thermal source outlet of secondary concentrating tower and three grades of concentration towers is connected, the outlet of three grades of concentration tower tower top flow containers goes out water pump and three grades of concentration tower filler and level Four concentration tower tower top flow container is connected through three grades of reflux pumps and three grades respectively, three grades of concentration tower discharging pumps are connected with pan feeding a bite of evaporator, the discharging opening of evaporator is connected with feed heater entrance through feed cycle pump, feed heater outlet is connected with the pan feeding two mouthfuls of evaporator, the gaseous phase outlet of evaporator is connected with level Four concentration tower charging aperture, the outlet of level Four concentration tower overhead vapours is connected with the reboiler thermal source inlet of three grades of concentration towers, the reboiler thermal source outlet of three grades of concentration towers is connected with the tower top flow container entrance of level Four concentration tower, the tower top flow container outlet of level Four concentration tower goes out water pump through level Four reflux pump with level Four respectively and is connected with level Four concentration tower filler and waste water tank, level Four concentration tower discharging pump is connected with rectifying column charging aperture, rectifying column tower top steam (vapor) outlet is connected with rectifying column tower top flow container entrance through rectifying column condenser, the outlet of rectifying column tower top flow container goes out water pump through rectifier column reflux pump with rectifying column respectively and is connected with rectifying column filler and level Four concentration tower tower top flow container entrance, rectifying column discharging pump is connected with extracting tower charging aperture, the outlet of extracting tower overhead vapours is connected with DMAc condensate drum entrance through DMAc condenser, the outlet of DMAc condensate drum is connected with extracting tower refluxing opening through DMAc reflux pump, extracting tower side line discharge is connected with DMAc discharge tank entrance through pure DMAc cooler,Primary concentrating tower, secondary concentrating tower, three grades of concentration towers, level Four concentration tower, rectifying column, extracting tower vacuum port be connected to vacuum pump.
Heretofore described evaporator blowing slag-drip opening is connected to drying machine, and the discharging opening of drying machine is connected with PVP extruder through PVP heavy liquor pump.
Heretofore described primary concentrating tower side is provided with feed preheater, and the outlet of feed preheater is connected with raw liquor pump import.
During work, the reboiler of level Four concentration tower, the feed heater of vaporizer, rectifying column reboiler are connected with vapour source with the thermal source inlet of extracting tower reboiler, and thermal source outlet is connected with collecting water tank. Primary concentrating tower, secondary concentrating tower, three grades of concentration towers, level Four concentration tower, rectifying column, extracting towers are vacuumizing, its vacuum be respectively as follows: primary concentrating tower-0.09MPa between-0.095MPa, secondary concentrating tower between-0.08MPa to-0.086MPa, three grades of concentration towers between-0.06MPa to-0.07MPa, level Four concentration tower between-0.04MPa to-0.052MPa, rectifying column between-0.085MPa to-0.095MPa, extracting tower is between-0.08MPa to-0.09MPa. Vacuum is undertaken aspirating, being automatically adjusted by vacuum pump.
The present invention has environmental protection, ultrahigh-recovery-rate and the advantage such as energy-conservation, the concentration DMAc waste-water purification energy resource consumption lower than 10% is made to significantly reduce, and the DMAc finished product indices after purification all reaches the standard of pure DMAc, can reuse, make enterprise reduce cost in liquid waste processing and the purchasing of raw materials two. Processing procedure avoids DMAc and at high temperature resolves into acetic acid and dimethylamine, reduce the change of impurity increase, pH value and electrical conductivity, it is to avoid contaminated environment.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention.
Detailed description of the invention
A kind of distillation purifying method of low concentration DMAc in waste water containing a small amount of low-boiling-point substance and high-boiling components, it is characterised in that comprise the following steps:
Step 1: through raw liquor pump, the waste water containing 2%DMAc, low-boiling-point substance and high-boiling components being sent into primary concentrating tower and carries out primary concentration, primary concentrating tower column bottom temperature controls at 42 DEG C-46 DEG C, and tower top temperature controls at 39 DEG C-43 DEG C;
Step 2: (reach 2.4%) when DMAc concentration promotes 0.4% in the tower bottoms of primary concentrating tower by one-level (T101) discharging pump feeding secondary concentrating tower and carry out secondary concentration, secondary concentrating tower column bottom temperature controls at 55 DEG C-59 DEG C, and tower top temperature controls at 52 DEG C-56 DEG C;
Step 3: (reaching 3.3%) when DMAc concentration promotes 0.9% in the tower bottoms of secondary concentrating tower and delivered to three grades of concentration towers by two grades of discharging pumps to carry out three grades of concentrations, three grades of concentration tower column bottom temperatures control at 68 DEG C-72 DEG C, and tower top temperature controls at 65 DEG C-69 DEG C;
Step 4: DMAc concentration promotes 2.4%(and namely reaches 5.7% in the tower bottoms of three grades of concentration towers) time sent into evaporators by three grades of discharging pumps, subsequently into feed heater, after carrying out heat exchange extremely boiling with steam, enter flash distillation in evaporator, air-liquid is made to separate, gas phase enters level Four concentration tower and carries out level Four concentration, and level Four concentration tower column bottom temperature controls at 81 DEG C-85 DEG C, and tower top temperature controls at 78 DEG C-82 DEG C; Feed heater continuation evaporation is entered through feed cycle pump after unevaporated liquid phase and the liquid mixing of three grades of discharging pumps feeding evaporators in evaporator;
Step 5: DMAc concentration is delivered in the middle part of rectifying column by level Four discharging pump when reaching 20% in the tower bottoms of level Four concentration tower, under the combined effect with overhead reflux of the rectifying column reboiler, water is easily vaporized and step by step tray rising, and DMAc then step by step tray declines;
Step 6: DMAc is moisture < during 150ppm in tower bottom of rectifying tower, extracting tower is entered by tower bottom of rectifying tower liquid phase extraction, DMAc product, by extracting tower top side take-off, enters DMAc discharge tank after pure DMAc cooler cools down, then delivers to DMAc finished pot with DMAc discharging pump;
In above-mentioned steps, the temperature of one to three grade of concentration tower heating equipment controls to be regulated steam flow control by steam control valve; The Energy harvesting method of concentration towers at different levels, evaporator, rectifying column and extracting tower is: the reboiler of level Four concentration tower, feed heater, rectifying column reboiler and the extracting tower reboiler energy are the primary steam that vapour source produces; The reboiler of level Four concentration tower overhead vapours three grades of concentration towers of heating, condensed water enters four column overhead flow containers; The reboiler of three grades of concentration tower overhead vapours heating secondary concentrating tower, condensed water enters three column overhead flow containers; The reboiler of secondary concentrating tower overhead vapours heating primary concentrating tower, condensed water enters two column overhead flow containers; Primary concentrating tower overhead vapours enters primary concentrating tower overhead condenser and becomes with recirculated water heat exchange to enter a column overhead flow container after liquid overhead water;
A primary concentrating tower overhead water part is sent back to primary concentrating tower recycling by primary concentrating tower reflux pump, a part is pumped to two column overhead flow containers by primary concentrating tower water outlet, a secondary concentrating tower overhead water part is sent back to secondary concentrating tower recycling by secondary concentrating tower reflux pump, a part is pumped to three column overhead flow containers by secondary concentrating tower water outlet, three grades of concentration tower overhead water parts are sent back to three grades of concentration tower recyclings by three grades of concentration tower reflux pumps, a part is pumped to four column overhead flow containers by three grades of concentration tower water outlets, a level Four concentration tower overhead water part is sent back to the recycling of level Four concentration tower by level Four concentration tower reflux pump, a part is pumped into tank field tower top water pot by level Four concentration tower water outlet and returns production line and reuse or send into treatment tank and process,
Rectifying column overhead vapours enters rectifying column overhead condenser and becomes liquid overhead water with recirculated water heat exchange, and a part is by rectifier column reflux pumped back rectifying column, and a part is pumped to four column overhead water pots by rectifying column water outlet; Extracting tower overhead vapours enters DMAc condenser and becomes liquid DMAc with recirculated water heat exchange, is all sent back to extracting tower by DMAc reflux pump; Four concentration towers, rectifying column and extracting tower are vacuumizing, and its vacuum is respectively as follows: primary concentrating tower-0.093MPa, secondary concentrating tower-0.082MPa, three grades of concentration towers-0.063, level Four concentration tower-0.048MPa, rectifying column-0.09MPa, extracting tower-0.082MPa. Vacuum is undertaken aspirating, being automatically adjusted by vacuum pump.
In heretofore described evaporator, unevaporated liquid phase is after sewage disposal device works 120 hours (to sewage disposal 120 hours), often process 2 hours waste water, the liquid phase entrance drying machine being discharged evaporator volume 2% by the slag-drip opening of evaporator is predrying, often processing 6 days waste water, the fluid after drying machine inner drying is sent into screw extruder extrusion PVP by PVP heavy liquor pump.
As shown in Figure 1 for realizing the distillation purifying equipment of low concentration DMAc in the waste water containing a small amount of low-boiling-point substance and high-boiling components of said method, including primary concentrating tower 5, secondary concentrating tower 6, three grades of concentration towers 7, evaporator 11, level Four concentration tower 13, rectifying column 15, extracting towers 25, the outlet of primary concentrating tower 5 overhead vapours is connected with primary concentrating tower tower top flow container 1 import through overhead condenser 2, primary concentrating tower tower top flow container 1 exports and is connected with primary concentrating tower 5 filler and secondary concentrating tower tower top flow container 44 entrance respectively with primary effluent pump 4 through one-level reflux pump 3, primary concentrating tower discharging pump 41 is connected with secondary concentrating tower 6 charging aperture, the outlet of secondary concentrating tower 6 overhead vapours is connected with reboiler 45 thermal source inlet of primary concentrating tower, reboiler 45 thermal source outlet of primary concentrating tower is connected with secondary concentrating tower tower top flow container 44 entrance, secondary concentrating tower tower top flow container 44 exports and is connected with secondary concentrating tower 6 filler and three grades of concentration tower tower top flow container 39 entrances respectively with secondary effluent pump 42 through two grades of reflux pumps 43,Secondary concentrating tower discharging pump 36 is connected with three grades of concentration tower 7 charging apertures, three grades of concentration tower 7 overhead vapours outlets are connected with reboiler 40 thermal source inlet of secondary concentrating tower, and reboiler 40 thermal source outlet of secondary concentrating tower and three grades of concentration tower tower top flow container 39 entrances are connected, three grades of concentration tower tower top flow containers 39 export and go out water pump 37 through three grades of reflux pumps 38 with three grades and be connected with three grades of concentration tower 7 filler and level Four concentration tower tower top flow container 35 respectively, three grades of concentration tower discharging pumps 33 are connected with pan feeding a bite of evaporator 11, the discharging opening of evaporator 11 is connected with feed heater 12 entrance through feed cycle pump 31, the pan feeding two mouthfuls that feed heater 12 exports with evaporator 11 is connected, the gaseous phase outlet of evaporator is connected with level Four concentration tower 13 charging aperture, the outlet of level Four concentration tower 13 overhead vapours is connected with reboiler 8 thermal source inlet of three grades of concentration towers, reboiler 8 thermal source outlet of three grades of concentration towers is connected with level Four concentration tower tower top flow container 35 entrance, the outlet of level Four concentration tower tower top flow container goes out water pump 34 through level Four reflux pump 9 and is connected with level Four concentration tower filler and recovery water pot or apparatus for treating sewage respectively with level Four, level Four concentration tower discharging pump 29 is connected with rectifying column 15 charging aperture, the outlet of rectifying column 15 overhead vapours is connected with rectifying column tower top flow container 17 entrance through rectifying column condenser 18, rectifying column tower top flow container 17 exports and goes out water pump through rectifier column reflux pump 16 with rectifying column respectively and be connected with rectifying column filler and level Four concentration tower tower top flow container entrance, rectifying column discharging pump 27 is connected with extracting tower 25 charging aperture, the outlet of extracting tower 25 overhead vapours is connected with DMAc condensate drum 22 entrance through DMAc condenser 20, DMAc condensate drum 22 exports and is connected with extracting tower 25 refluxing opening through DMAc reflux pump 21, extracting tower 25 side line discharge is connected with DMAc discharge tank 24 entrance through pure DMAc cooler 19, DMAc discharge tank 24 outlet is provided with discharging pump 23, primary concentrating tower, secondary concentrating tower, three grades of concentration towers, level Four concentration tower, rectifying column, extracting tower vacuum port be connected to vacuum pump. evaporator blowing slag-drip opening is connected to drying machine 10, the discharging opening of drying machine 10 is connected with PVP extruder 30 through PVP heavy liquor pump 32, when the liquid solute in equipment operation certain time, evaporator reaches normal concentration, the solution entrance drying machine discharging certain volume from evaporator slag-drip opening is predrying, fluid after drying machine inner drying is sent into screw extruder extrusion PVP(polyvinylpyrrolidone by PVP heavy liquor pump), present treatment device contamination-free is discharged, energy-conserving and environment-protective, and create side-product, reduce cost for wastewater treatment.
The present invention can be provided with feed preheater in primary concentrating tower side, and the outlet of feed preheater is connected with primary concentrating tower charging aperture through raw liquor pump, processes, enhancement process effect after waste water is preheated. When the present invention works, the reboiler 14 of level Four concentration tower, the feed heater 12 of vaporizer, rectifying column reboiler 28 are connected with vapour source with the thermal source inlet of extracting tower reboiler 26, thermal source outlet is connected with collecting water tank or is connected with the thermal source inlet of feed preheater, and energy is made full use of. Primary concentrating tower, secondary concentrating tower, three grades of concentration towers, level Four concentration tower, rectifying column, extracting towers are vacuumizing, and its vacuum is respectively as follows: primary concentrating tower-0.095MPa, secondary concentrating tower-0.085MPa, three grades of concentration tower-0.068MPa, level Four concentration tower-0.05MPa, rectifying column-0.09MPa, extracting tower-0.088MPa.Its vacuum is undertaken aspirating automatic adjustment by vacuum pump.
The present invention has environmental protection, ultrahigh-recovery-rate and the advantage such as energy-conservation, the concentration DMAc waste-water purification energy resource consumption lower than 10% is made to significantly reduce, and the DMAc finished product indices after purification all reaches the standard of pure DMAc, can reuse, make enterprise reduce cost in liquid waste processing and the purchasing of raw materials two. Processing procedure adopts relatively low operating temperature due to each tower, it is to avoid DMAc at high temperature resolves into acetic acid and dimethylamine, reduce impurity increase, the change of pH value and electrical conductivity, it is to avoid contaminated environment. The present invention uses primary energy to coordinate four concentration tower energy supplies that temperature requirement is reduced by each concentration tower step by step, while energy is made full use of, coordinate the specific temperature of each concentration tower, vacuum to achieve consumption to have lacked energy purification and contain low concentration (lower than 10%) DMAc waste water, make enterprise reduce cost in liquid waste processing and the purchasing of raw materials two.
Table 1 multi-effect rectifying process process CIMS
Remarks: steam presses 200 yuan/ton, electricity is by 1 yuan/degree, and water presses 3 yuan/ton of calculating, and DMAC presses 10000 yuan/ton of calculating. Labour cost does not calculate.
The some processes index processing device and method that table 1 is existing three tower triple effects, four tower quadruple effects process devices and the present invention compares. In table, the response rate of the listed present invention is the real data that equipment runs, and the response rate of three tower triple effects and four tower quadruple effects is the most high-recovery of estimation. By upper table it will be seen that three tower triple effects and four tower quadruple effect two schemes reclaim MDAc value less than operating cost, MDAc only of the present invention is worth more than operating cost.
It is an advantage of the current invention that finished product response rate height and environmental protection. The tower bottom of rectifying tower temperature of existing three tower triple effects is 145 DEG C; The tower bottom of rectifying tower temperature of four tower quadruple effects is 165 DEG C; And tower bottom of rectifying tower temperature of the present invention is 105 DEG C. Operation temperature is more high, and the decomposition amount of DMAc is more big, and in overhead water, the content of dimethylamine is more high, corresponding more high of COD value. The overhead water of existing three tower triple effects and four tower quadruple effects process equipment just can enter garden sewage network after having to pass through the treatment tank process that plant area carries, and adopts the process equipment of the present invention and processing method (COD < 200) then can be directly accessed garden sewage network.
Decomposition due to DMAc, dimethylamine in the gas phase can enter in air along with vacuum pump, contaminated environment, the current processing method of dimethylamine in the gas phase of existing three tower triple effects and four tower quadruple effects is that boiler room burns, but can cause NO and the NO in the flue gas of boiler2Exceed standard, cause a large amount of NO and NO2Discharge. And due to the fact that the operation temperature of whole system is below 105 DEG C, decomposition amount is extremely low, it is possible to air is directly discharged.
Therefore, no matter from environmental angle or economic angle, the present invention is best for the treatment effect of the waste liquid of low concentration.
The described waste water containing a small amount of low-boiling-point substance and high-boiling components, refers to that low-boiling-point substance and high-boiling components concentration are lower than 5%, and a small amount of DMAc refers to that in waste water, DMAc concentration is lower than 10%. Wherein low-boiling-point substance includes the little molecules such as water, acetic acid, dimethylamine, and high-boiling components includes the macromolecule such as polyvinylpyrrolidone, polysulfones. DMAc is at high temperature readily decomposed to acetic acid and dimethylamine, and their generation can make system impurity increase, and pH value and electrical conductivity also can change.
Have employed drying machine pre-treatment and add the technological process of the polymer substances such as extruser spiral squeezing polyvinylpyrrolidone, polysulfones, the polymer substance recoverable such as the polyvinylpyrrolidone of discharge, polysulfones or go to burn station and burn.
The method and apparatus of the present invention, has a characteristic that
The response rate is high: adopt the technological process of level Four concentrating under reduced pressure so that the concentration process of whole DMAc waste liquid carries out all at low temperatures, and the decomposition amount of DMAc is down to minimum. Simultaneously because have employed crude product DMAc rectification under vacuum, finished product DMAc reduces pressure the refining technological process of deacidification so that whole DMAc finished product subtractive process all carries out under ultralow temperature, and the decomposition amount of DMAc is down to minimum. Final finished DMAc concentration > 99.9%, water content < 200ppm, acetic acid < 50ppm, dimethylamine < 30ppm.
Environmental protection: 1. in overhead water, COD content can return production line less than 200ppm and be repeated use, it is not necessary to discharge, has saved water resource. 2. due in waste liquid the polymer substance such as polyvinylpyrrolidone, polysulfones concentration be 0.1%, this device have employed drying machine pre-treatment and adds the technological process of the polymer substances such as extruser spiral squeezing polyvinylpyrrolidone, polysulfones, and the polymer substance such as the polyvinylpyrrolidone of discharge, polysulfones is recycled or gone to burn station and burns. 3. dimethylamine content < 10mg/m in air3, it is possible to qualified discharge.
Claims (5)
1. the distillation purifying method of low concentration DMAc in the waste water containing a small amount of low-boiling-point substance and high-boiling components, it is characterised in that comprise the following steps:
Step 1: the waste water containing 1-10%DMAc, low-boiling-point substance and high-boiling components is sent into primary concentrating tower through raw liquor pump and carries out primary concentration, primary concentrating tower column bottom temperature 42-46 DEG C, tower top temperature 39-43 DEG C;
Step 2: sent into secondary concentrating tower by one-level discharging pump when DMAc concentration promotes 0.2%-0.5% in the tower bottoms of primary concentrating tower and carry out secondary concentration, secondary concentrating tower column bottom temperature 55 DEG C-59 DEG C, tower top temperature 52 DEG C-56 DEG C;
Step 3: DMAc concentration is delivered to three grades of concentration towers by two grades of discharging pumps and carried out three grades of concentrations when promoting 0.6%-1.5% in the tower bottoms of secondary concentrating tower, three grades of concentration tower column bottom temperatures 68 DEG C-72 DEG C, tower top temperature 65 DEG C-69 DEG C;
Step 4: DMAc concentration is sent into evaporator by three grades of discharging pumps when promoting 2%-3% in the tower bottoms of three grades of concentration towers, subsequently into feed heater, after carrying out heat exchange extremely boiling with steam, enter flash distillation in evaporator, air-liquid is made to separate, gas phase enters level Four concentration tower and carries out level Four concentration, level Four concentration tower column bottom temperature 81 DEG C-85 DEG C, tower top temperature 78 DEG C-82 DEG C; Feed heater continuation evaporation is entered through feed cycle pump after unevaporated liquid phase and the liquid mixing of three grades of discharging pumps feeding evaporators in evaporator;
Step 5: DMAc concentration is delivered in the middle part of rectifying column by level Four discharging pump when reaching 18%-25% in the tower bottoms of level Four concentration tower, under the combined effect with overhead reflux of the rectifying column reboiler, water is easily vaporized and step by step tray rising, and DMAc then step by step tray declines;
Step 6: in tower bottom of rectifying tower DMAc moisture < during 150ppm, by tower bottom of rectifying tower liquid phase extraction enter extracting tower, DMAc product by extracting tower top side take-off, through pure DMAc cooler cool down after enter DMAc discharge tank;
In above-mentioned steps, the temperature of one to three grade of concentration tower heating equipment controls to be regulated steam flow control by steam control valve; The Energy harvesting method of concentration towers at different levels, evaporator, rectifying column and extracting tower is: the reboiler of level Four concentration tower, feed heater, rectifying column reboiler and the extracting tower reboiler energy are primary steam heating; The reboiler of level Four concentration tower overhead vapours three grades of concentration towers of heating, condensed water enters four column overhead flow containers;The reboiler of three grades of concentration tower overhead vapours heating secondary concentrating tower, condensed water enters three column overhead flow containers; The reboiler of secondary concentrating tower overhead vapours heating primary concentrating tower, condensed water enters two column overhead flow containers; Primary concentrating tower overhead vapours enters primary concentrating tower overhead condenser and becomes with recirculated water heat exchange to enter a column overhead flow container after liquid overhead water;
A primary concentrating tower overhead water part is sent back to primary concentrating tower by primary concentrating tower reflux pump, a part is pumped to two column overhead flow containers by primary concentrating tower water outlet, a secondary concentrating tower overhead water part is sent back to secondary concentrating tower by secondary concentrating tower reflux pump, a part is pumped to three column overhead flow containers by secondary concentrating tower water outlet, three grades of concentration tower overhead water parts are sent back to three grades of concentration towers by three grades of concentration tower reflux pumps, a part is pumped to four column overhead flow containers by three grades of concentration tower water outlets, a level Four concentration tower overhead water part is sent back to level Four concentration tower by level Four concentration tower reflux pump, a part is pumped into tank field tower top water pot by four tower water outlets and returns production line and reuse or send into treatment tank and process,
Rectifying column overhead vapours enters rectifying column overhead condenser and becomes liquid overhead water with recirculated water heat exchange, and a part is reused by rectifier column reflux pumped back rectifying column, and a part is pumped to four column overhead water pots by rectifying column water outlet; Extracting tower overhead vapours enters DMAc condenser and becomes liquid DMAc with recirculated water heat exchange, is all sent back to extracting tower by DMAc reflux pump; Four concentration towers, rectifying column and extracting tower are vacuumizing, its vacuum be respectively as follows: primary concentrating tower between-0.09MPa to-0.095MPa, secondary concentrating tower between-0.08MPa to-0.086MPa, three grades of concentration towers between-0.06MPa to-0.07MPa, level Four concentration tower between-0.04MPa to-0.052MPa, rectifying column between-0.085MPa to-0.095MPa, extracting tower is between-0.08MPa to-0.09MPa.
2. the distillation purifying method of low concentration DMAc in the waste water containing a small amount of low-boiling-point substance and high-boiling components according to claim 1, it is characterized in that in described evaporator, unevaporated liquid phase is after work 120 hours, often process 1 ~ 3 hour waste water, the liquid phase entrance drying machine being discharged evaporator volume 1% ~ 3% by the slag-drip opening of evaporator is predrying, often processing 6 days waste water, the fluid after drying machine inner drying is pumped into screw extruder extrusion PVP by PVP heavy liquor pump.
3. for realizing the distillation purifying equipment of low concentration DMAc in a kind of waste water containing a small amount of low-boiling-point substance and high-boiling components of the method described in claim 1, it is characterised in that including: primary concentrating tower, secondary concentrating tower, three grades of concentration towers, evaporator, level Four concentration tower, rectifying column, extracting towers, the outlet of primary concentrating tower overhead vapours is connected with primary concentrating tower tower top flow container import through overhead condenser, the outlet of primary concentrating tower tower top flow container is connected with primary concentrating tower filler and secondary concentrating tower tower top flow container entrance with primary effluent pump through one-level reflux pump respectively, primary concentrating tower discharging pump is connected with secondary concentrating tower charging aperture, the outlet of secondary concentrating tower overhead vapours is connected with the reboiler thermal source inlet of primary concentrating tower, the reboiler thermal source outlet of primary concentrating tower is connected with the tower top flow container entrance of secondary concentrating tower, the outlet of secondary concentrating tower tower top flow container is connected with secondary concentrating tower filler and three grades of concentration tower tower top flow container entrances with secondary effluent pump through two grades of reflux pumps respectively, secondary concentrating tower discharging pump and three grades of concentration tower charging apertures are connected, and three grades of concentration tower overhead vapours outlets are connected with the reboiler thermal source inlet of secondary concentrating tower, and the tower top flow container entrance of the reboiler thermal source outlet of secondary concentrating tower and three grades of concentration towers is connected, the outlet of three grades of concentration tower tower top flow containers goes out water pump and three grades of concentration tower filler and level Four concentration tower tower top flow container is connected through three grades of reflux pumps and three grades respectively, three grades of concentration tower discharging pumps are connected with pan feeding a bite of evaporator, the discharging opening of evaporator is connected with feed heater entrance through feed cycle pump, feed heater outlet is connected with the pan feeding two mouthfuls of evaporator, the gaseous phase outlet of evaporator is connected with level Four concentration tower charging aperture, the outlet of level Four concentration tower overhead vapours is connected with the reboiler thermal source inlet of three grades of concentration towers, the reboiler thermal source outlet of three grades of concentration towers is connected with the tower top flow container entrance of level Four concentration tower, the tower top flow container outlet of level Four concentration tower goes out water pump through level Four reflux pump with level Four respectively and is connected with level Four concentration tower filler and waste water tank, level Four concentration tower discharging pump is connected with rectifying column charging aperture, rectifying column tower top steam (vapor) outlet is connected with rectifying column tower top flow container entrance through rectifying column condenser, the outlet of rectifying column tower top flow container goes out water pump through rectifier column reflux pump with rectifying column respectively and is connected with rectifying column filler and level Four concentration tower tower top flow container entrance, rectifying column discharging pump is connected with extracting tower charging aperture, the outlet of extracting tower overhead vapours is connected with DMAc condensate drum entrance through DMAc condenser, the outlet of DMAc condensate drum is connected with extracting tower refluxing opening through DMAc reflux pump, extracting tower side line discharge is connected with DMAc discharge tank entrance through pure DMAc cooler,Primary concentrating tower, secondary concentrating tower, three grades of concentration towers, level Four concentration tower, rectifying column, extracting tower vacuum port be connected to vacuum pump.
4. the distillation purifying equipment of low concentration DMAc in the waste water containing a small amount of low-boiling-point substance and high-boiling components according to claim 3, it is characterized in that described evaporator blowing slag-drip opening is connected to drying machine, the discharging opening of drying machine is connected with PVP extruder through PVP heavy liquor pump.
5. the distillation purifying equipment of low concentration DMAc in the waste water containing a small amount of low-boiling-point substance and high-boiling components according to claim 3, it is characterised in that described primary concentrating tower side is provided with feed preheater, and the outlet of feed preheater is connected with raw liquor pump import.
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| CN104944661B (en) * | 2015-04-14 | 2017-07-07 | 常州冀德环保科技有限公司 | Seven tower five effect distillation system and its recovery method of a kind of DMAC or DMF waste liquids |
| RU2606118C1 (en) * | 2015-12-22 | 2017-01-10 | Акционерное общество "Каменскволокно" | Method of removing water from process circuit in chemical production |
| CN105732411A (en) * | 2016-03-04 | 2016-07-06 | 广东立国制药有限公司 | System and process for recovering dimethylacetamide from cefuroxime axetil production waste liquor |
| WO2017190299A1 (en) * | 2016-05-05 | 2017-11-09 | 章旭元 | Seven-tower five-effect rectification system for dmac or dmf waste liquid and method for recovering same |
| CN106220537A (en) * | 2016-08-31 | 2016-12-14 | 烟台国邦化工机械科技有限公司 | A kind of by separate to rectifying section and stripping section rectification process |
| CN109665972A (en) * | 2017-10-16 | 2019-04-23 | 中国石油化工股份有限公司 | A kind of ultrafiltration membrane produces the recovery system and method for dimethyl acetamide in waste water |
| CN108774149B (en) * | 2018-07-02 | 2024-04-02 | 南京久盈膜科技有限公司 | Solvent recycling method and device in PVDF separation membrane production |
| CN109320432A (en) * | 2018-10-31 | 2019-02-12 | 浙江本优机械有限公司 | A kind of evaporation equipment for the recycling purification of low concentration dimethyl acetamide |
| CN111847751B (en) * | 2020-08-29 | 2022-10-11 | 江苏美能膜材料科技有限公司 | Zero-emission recovery process for waste liquid generated by preparing polyvinylidene fluoride porous membrane |
| CN114956234A (en) * | 2022-06-16 | 2022-08-30 | 浙江泓泰德建新纤维有限公司 | Recovery process for purifying PVA from waste liquid |
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