CN104370768A - Method and equipment for distilling and purifying low-concentration DMAc in waste water containing small amount of low-boiling-point substances and high-boiling-point substances - Google Patents
Method and equipment for distilling and purifying low-concentration DMAc in waste water containing small amount of low-boiling-point substances and high-boiling-point substances Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 93
- 238000001704 evaporation Methods 0.000 claims abstract description 45
- 238000010992 reflux Methods 0.000 claims description 39
- 238000007599 discharging Methods 0.000 claims description 33
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- 239000012141 concentrate Substances 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 20
- 238000009835 boiling Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 18
- 239000000945 filler Substances 0.000 claims description 15
- 238000004821 distillation Methods 0.000 claims description 13
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- 238000007701 flash-distillation Methods 0.000 claims description 3
- 239000007792 gaseous phase Substances 0.000 claims description 3
- 238000003306 harvesting Methods 0.000 claims description 3
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- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 abstract description 102
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- 238000011084 recovery Methods 0.000 abstract description 7
- 238000004134 energy conservation Methods 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract 1
- 230000008016 vaporization Effects 0.000 abstract 1
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 21
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 17
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- 239000010865 sewage Substances 0.000 description 7
- 239000012528 membrane Substances 0.000 description 6
- 229920002492 poly(sulfone) Polymers 0.000 description 6
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- 238000004519 manufacturing process Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 3
- 239000010808 liquid waste Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
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- 241000707825 Argyrosomus regius Species 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 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 method and equipment for distilling and purifying low-concentration DMAc in waste water containing a small amount of low-boiling-point substances and high-boiling-point substances and relates to a method and equipment for distilling and purifying waste water containing a small amount of dimethylacetamide. The method for distilling and purifying low-concentration DMAc in the waste water containing the small amount of low-boiling-point substances and high-boiling-point substances comprises the steps of carrying out reduced pressure and low-temperature multistage concentration, evaporating and rectifying. The equipment for distilling and purifying low-concentration DMAc in the waste water containing a small amount of low-boiling-point substances and high-boiling-point substances comprises a primary concentrating tower, a secondary concentrating tower, a tertiary concentrating tower, a vaporizing tank, a quaternary concentrating tower, a rectifying tower and a deacidifying tower. The method and equipment for distilling and purifying low-concentration DMAc in the waste water containing a small amount of low-boiling-point substances and high-boiling-point substances can be used for overcoming the defects of the prior art and has the advantages that energy consumption is low, recovery rate is high, the small amount of DMAc is decomposed, the environment is not polluted, content of COD in water on the tower top is low, and energy conservation and environmental protection are realized.
Description
Technical field
The present invention relates to the method for a kind of distillation purifying containing less N,N-DIMETHYLACETAMIDE (DMAc) waste water; Say it is that a kind of capacity usage ratio is high in detail, save energy, DMAc decomposition of little, the distillation purifying method and apparatus containing lower concentration DMAc in the waste water of a small amount of low-boiling-point substance and high boiling material avoiding blowdown to pollute.
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 rapidly increases.In hollow-fibre membrane manufacturing processed, DMAc is mainly used as solvent, such as the solvent of polymkeric substance during synthon spinning, or as the solvent etc. of polymkeric substance during tubular fibre film preparation.In order to high-quality product can be obtained 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, specific conductivity < 0.6 μ S/cm.The DMAc meeting above-mentioned specification requirement is called pure DMAc hereinafter
It is reported, China has at present more than 500 hollow-fibre membrane manufacturing enterprises, and wherein the overwhelming majority is middle and small scale, and the waste water DMAc content of generation is all lower than 10%, and enterprise does not possess the ability of voluntary recall purifying containing DMAc waste liquid.If these waste water can not get effective process, will severe contamination soil, underground water and even whole ecotope.Purifying difficult point containing DMAc waste water is processing cost, wherein energy consumption cost is wherein most important part, and the purifying of unit mass DMAc, required processing cost (comprising energy consumption cost, human cost, equipment amortization cost etc.) is inversely proportional to DMAc concentration in initial waste liquid.Existing for DMAc concentration about 10% sewage treatment equipment and method, the pure DMAc reclaimed after separation and purification treatment is worth and can balances with processing cost, and for DMAc concentration lower than the wastewater treatment of 10%, is in lossing state, and concentration is lower, lose more serious.Under the situation that environmental requirement is increasingly strict, the DMAc Waste Water Centralized of generation is often delivered to professional separation and purification unit and is processed by Yangtze River Delta Area relevant enterprise.And the wastewater treatment expense of great number, make originally to make the matter worse with regard to the enterprise being in harmful competition profit meagre.DMAc purification process disclosed in the patent of invention of Chinese patent (publication number: 102030672 A), for reclaiming ultra-pure DMAc solvent in spandex production process, but its scope of application be only confined to DMAc concentration 20% to 70% waste water, for DMAc concentration lower than the waste water of 10%, be difficult to obtain high purity DMAc by the method.(publication number: 100341848) disclosed DMAc purification process, adopts normal pressure or a little more than condition of normal pressure to another Chinese patent, and rectifying tower tower top temperature is about 70 DEG C-115 DEG C, bottom temperature is about 150 DEG C-180 DEG C, obtains pure DMAc.But the method is higher due to service temperature, adds energy consumption, also easily make DMAc resolve into the small-molecule substance such as acetic acid, dimethylamine, add finished product depickling and overhead water takes off the burden of amine and easily causes secondary pollution.
Summary of the invention
The object of the invention is to solve above-mentioned the deficiencies in the prior art, there is provided that a kind of energy consumption is low, the rate of recovery is high, DMAc decomposition of little, in free from environmental pollution, overhead water, COD content is few, the distillation purifying method and apparatus containing lower concentration DMAc in the waste water of a small amount of low-boiling-point substance and high boiling material of energy-conserving and environment-protective.
The present invention solves above-mentioned the deficiencies in the prior art, and the technical scheme adopted is:
Contain a distillation purifying method of lower concentration DMAc in the waste water of a small amount of low-boiling-point substance and high boiling material, it is characterized in that comprising the following steps:
Step 1: the waste water containing 1-10%DMAc, low-boiling-point substance and high boiling material is sent into primary concentrating tower through concentrate 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: send 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: deliver to three grades of upgrading towers by secondary discharging pump when DMAc concentration promotes 0.6%-1.5% in the tower bottoms of secondary concentrating tower and carry out three grades and concentrate, three grades of upgrading tower column bottom temperatures 68 DEG C-72 DEG C, tower top temperature 65 DEG C-69 DEG C;
Step 4: send into evaporating pot by three grades of discharging pumps when DMAc concentration promotes 2%-3% in the tower bottoms of three grades of upgrading towers, then feed heater is entered, heat exchange is carried out to after seething with excitement with steam, enter flash distillation in evaporating pot, gas, liquid are separated, gas phase enter level Four upgrading tower carry out level Four concentrate, level Four upgrading tower column bottom temperature 81 DEG C-85 DEG C, tower top temperature 78 DEG C-82 DEG C; Enter feed heater through feed cycle pump after unevaporated liquid phase and three grades of discharging pumps send into the liquid mixing of evaporating pot in evaporating pot to continue to evaporate;
Step 5: deliver in the middle part of rectifying tower by level Four discharging pump when DMAc concentration reaches 18%-25% in the tower bottoms of level Four upgrading tower, under the acting in conjunction of rectifying tower reboiler and trim the top of column, water is easily vaporized and step by step tray rises, and DMAc then step by step tray declines;
Step 6: in tower bottom of rectifying tower during the moisture <150ppm of DMAc, extracting tower is entered by the extraction of tower bottom of rectifying tower liquid phase, DMAc product, by extracting tower top side take-off, enters DMAc discharge tank, then delivers to DMAc finished pot with DMAc discharging pump after pure DMAc water cooler cooling;
In above-mentioned steps, the temperature of one to three grade of upgrading tower heating equipment controls to be controlled by the steam regulating valve steam regulation flow of each upgrading tower; The Energy harvesting method of upgrading tower at different levels, evaporating pot, rectifying tower and extracting tower is: the reboiler of level Four upgrading tower, feed heater, rectifying tower reboiler and the extracting tower reboiler energy are primary steam (producing through vapour source) heating; Level Four upgrading tower overhead vapours heats the reboiler of three grades of upgrading towers, and water of condensation enters four column overhead flow containers; The reboiler of three grades of upgrading tower overhead vapours heating secondary concentrating tower, water of condensation enters three column overhead flow containers; The reboiler of secondary concentrating tower overhead vapours heating primary concentrating tower, water of condensation enters two column overhead flow containers; Primary concentrating tower overhead vapours enters primary concentrating tower overhead condenser and becomes with recirculated water heat exchange after liquid overhead water to enter a column overhead flow container;
A primary concentrating tower overhead water part sends primary concentrating tower back to 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 sends secondary concentrating tower back to 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 upgrading tower overhead water parts send three grades of upgrading towers back to by three grades of upgrading tower reflux pumps, a part is pumped to four column overhead flow containers by three grades of upgrading tower water outlets, a level Four upgrading tower overhead water part sends level Four upgrading tower back to by level Four upgrading tower reflux pump, a part is pumped into tank field tower top water pot by four tower water outlets and returns and produce line and reuse or send into treatment tank and process,
Rectifying tower overhead vapours enters rectifying tower overhead condenser and becomes liquid overhead water with recirculated water heat exchange, and a part is by rectifier column reflux pumped back rectifying tower, and a part is pumped to four column overhead water pots by rectifying tower water outlet; Extracting tower overhead vapours enters DMAc condenser and becomes liquid DMAc with recirculated water heat exchange, all sends extracting tower back to by DMAc reflux pump; Four upgrading towers, rectifying tower and extracting towers are vacuum operating, and its vacuum tightness is respectively: primary concentrating tower-0.09MPa between-0.095MPa, secondary concentrating tower between-0.08MPa to-0.086MPa, three grades of upgrading towers between-0.06MPa to-0.07MPa, level Four upgrading tower between-0.04MPa to-0.052MPa, rectifying tower between-0.085MPa to-0.095MPa, extracting tower is between-0.08MPa to-0.09MPa.Vacuum tightness is undertaken aspirating, automatically regulating by vacuum pump.
In evaporating pot described in the present invention, unevaporated liquid phase is at equipment work after 120 hours, often process 1 ~ 3 hour waste water, drying machine is entered predrying by the liquid phase of the slag-drip opening discharge evaporating pot volume 1% ~ 3% of evaporating pot, often process 6 days waste water, the fluid after drying machine inner drying is pumped into screw extrusion press by PVP concentrate pump and extrudes PVP.
A kind of
containing the distillation purifying of lower concentration DMAc in the waste water of a small amount of low-boiling-point substance and high boiling materialequipment, is characterized in that comprising: primary concentrating tower, secondary concentrating tower, three grades of upgrading towers, evaporating pot, level Four upgrading tower, rectifying tower, extracting towers, the outlet of primary concentrating tower overhead vapours is connected with the import of primary concentrating tower tower top flow container through overhead condenser, the outlet of primary concentrating tower tower top flow container is connected with secondary concentrating tower tower top flow container entrance with primary concentrating tower filler with primary effluent pump through one-level reflux pump respectively, primary concentrating tower discharging pump is connected with secondary concentrating tower opening for feed, 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 three grades of upgrading tower tower top flow container entrances with secondary concentrating tower filler with secondary effluent pump through secondary reflux pump respectively, secondary concentrating tower discharging pump is connected with three grades of upgrading tower opening for feeds, and three grades of upgrading tower overhead vapours outlets are connected with the reboiler thermal source inlet of secondary concentrating tower, and the reboiler thermal source outlet of secondary concentrating tower is connected with the tower top flow container entrance of three grades of upgrading towers, the outlet of three grades of upgrading tower tower top flow containers goes out water pump through three grades of reflux pumps be connected with level Four upgrading tower tower top flow container with three grades of upgrading tower filler with three grade respectively, three grades of upgrading tower discharging pumps are connected with pan feeding a bite of evaporating pot, the discharge port of evaporating pot is connected with feed heater entrance through feed cycle pump, feed heater outlet is connected with the pan feeding two mouthfuls of evaporating pot, the gaseous phase outlet of evaporating pot is connected with level Four upgrading tower opening for feed, the outlet of level Four upgrading tower overhead vapours is connected with the reboiler thermal source inlet of three grades of upgrading towers, the reboiler thermal source outlet of three grades of upgrading towers is connected with the tower top flow container entrance of level Four upgrading tower, the tower top flow container outlet of level Four upgrading tower goes out water pump through level Four reflux pump and level Four respectively and is connected with waste water tank with level Four upgrading tower filler, level Four upgrading tower discharging pump is connected with rectifying tower opening for feed, rectifying tower tower top vapour outlet is connected with rectifying tower tower top flow container entrance through rectifying tower condenser, the outlet of rectifying tower tower top flow container goes out water pump through rectifier column reflux pump and rectifying tower respectively and is connected with level Four upgrading tower tower top flow container entrance with rectifying tower filler, rectifying tower discharging pump is connected with extracting tower opening for feed, 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 water cooler, the vacuum port of primary concentrating tower, secondary concentrating tower, three grades of upgrading towers, level Four upgrading tower, rectifying tower, extracting tower is connected to vacuum pump.
Evaporating pot blowing slag-drip opening described in the present invention is connected with drying machine, and the discharge port of drying machine is connected with PVP forcing machine through PVP concentrate pump.
Primary concentrating tower side described in the present invention is provided with feed preheater, and the outlet of feed preheater is connected with concentrate pump import.
During work, the reboiler of level Four upgrading tower, the feed heater of vaporizer, rectifying tower reboiler are connected with vapour source with the thermal source inlet of extracting tower reboiler, and thermal source outlet is connected with collection water tank.Primary concentrating tower, secondary concentrating tower, three grades of upgrading towers, level Four upgrading tower, rectifying tower, extracting towers are vacuum operating, and its vacuum tightness is respectively: primary concentrating tower-0.09MPa between-0.095MPa, secondary concentrating tower between-0.08MPa to-0.086MPa, three grades of upgrading towers between-0.06MPa to-0.07MPa, level Four upgrading tower between-0.04MPa to-0.052MPa, rectifying tower between-0.085MPa to-0.095MPa, extracting tower is between-0.08MPa to-0.09MPa.Vacuum tightness is undertaken aspirating, automatically regulating by vacuum pump.
The present invention has environmental protection, ultrahigh-recovery-rate and the advantage such as energy-conservation, make concentration lower than 10% the energy consumption of DMAc waste-water purification significantly reduce, and the DMAc finished product indices after purifying all reaches the standard of pure DMAc, can reuse, make enterprise reduce cost in liquid waste disposal and the purchasing of raw materials two.Avoid DMAc in treating processes and at high temperature resolve into acetic acid and dimethylamine, reduce that impurity increases, the change of pH value and specific conductivity, avoid contaminate environment.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Embodiment
Contain a distillation purifying method of lower concentration DMAc in the waste water of a small amount of low-boiling-point substance and high boiling material, it is characterized in that comprising the following steps:
Step 1: the waste water containing 2%DMAc, low-boiling-point substance and high boiling material is sent into primary concentrating tower through concentrate pump 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: when DMAc concentration promotes 0.4% in the tower bottoms of primary concentrating tower, (reaching 2.4%) is sent into secondary concentrating tower by one-level (T101) discharging pump and carried 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: when DMAc concentration promotes 0.9% in the tower bottoms of secondary concentrating tower, (reaching 3.3%) is delivered to three grades of upgrading towers by secondary discharging pump and carried out three grades and concentrate, and three grades of upgrading 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 upgrading towers) time send into evaporating pots by three grades of discharging pumps, then feed heater is entered, heat exchange is carried out to after seething with excitement with steam, enter flash distillation in evaporating pot, gas, liquid are separated, gas phase enter level Four upgrading tower carry out level Four concentrate, level Four upgrading tower column bottom temperature controls at 81 DEG C-85 DEG C, and tower top temperature controls at 78 DEG C-82 DEG C; Enter feed heater through feed cycle pump after unevaporated liquid phase and three grades of discharging pumps send into the liquid mixing of evaporating pot in evaporating pot to continue to evaporate;
Step 5: deliver in the middle part of rectifying tower by level Four discharging pump when DMAc concentration reaches 20% in the tower bottoms of level Four upgrading tower, under the acting in conjunction of rectifying tower reboiler and trim the top of column, water is easily vaporized and step by step tray rises, and DMAc then step by step tray declines;
Step 6: in tower bottom of rectifying tower during the moisture <150ppm of DMAc, extracting tower is entered by the extraction of tower bottom of rectifying tower liquid phase, DMAc product, by extracting tower top side take-off, enters DMAc discharge tank, then delivers to DMAc finished pot with DMAc discharging pump after pure DMAc water cooler cooling;
In above-mentioned steps, the temperature of one to three grade of upgrading tower heating equipment controls to be controlled by steam regulating valve steam regulation flow; The Energy harvesting method of upgrading tower at different levels, evaporating pot, rectifying tower and extracting tower is: the reboiler of level Four upgrading tower, feed heater, rectifying tower reboiler and the extracting tower reboiler energy are the primary steam that vapour source produces; Level Four upgrading tower overhead vapours heats the reboiler of three grades of upgrading towers, and water of condensation enters four column overhead flow containers; The reboiler of three grades of upgrading tower overhead vapours heating secondary concentrating tower, water of condensation enters three column overhead flow containers; The reboiler of secondary concentrating tower overhead vapours heating primary concentrating tower, water of condensation enters two column overhead flow containers; Primary concentrating tower overhead vapours enters primary concentrating tower overhead condenser and becomes with recirculated water heat exchange after liquid overhead water to enter a column overhead flow container;
A primary concentrating tower overhead water part is sent primary concentrating tower back to by primary concentrating tower reflux pump and is reused, 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 secondary concentrating tower back to by secondary concentrating tower reflux pump and is reused, a part is pumped to three column overhead flow containers by secondary concentrating tower water outlet, three grades of upgrading tower overhead water parts are sent three grades of upgrading towers back to by three grades of upgrading tower reflux pumps and are reused, a part is pumped to four column overhead flow containers by three grades of upgrading tower water outlets, a level Four upgrading tower overhead water part is sent level Four upgrading tower back to by level Four upgrading tower reflux pump and is reused, a part is pumped into tank field tower top water pot by the water outlet of level Four upgrading tower and returns and produce line and reuse or send into treatment tank and process,
Rectifying tower overhead vapours enters rectifying tower overhead condenser and becomes liquid overhead water with recirculated water heat exchange, and a part is by rectifier column reflux pumped back rectifying tower, and a part is pumped to four column overhead water pots by rectifying tower water outlet; Extracting tower overhead vapours enters DMAc condenser and becomes liquid DMAc with recirculated water heat exchange, all sends extracting tower back to by DMAc reflux pump; Four upgrading towers, rectifying tower and extracting towers are vacuum operating, and its vacuum tightness is respectively: primary concentrating tower-0.093MPa, secondary concentrating tower-0.082MPa, three grades of upgrading towers-0.063, level Four upgrading tower-0.048MPa, rectifying tower-0.09MPa, extracting tower-0.082MPa.Vacuum tightness is undertaken aspirating, automatically regulating by vacuum pump.
In evaporating pot described in the present invention, unevaporated liquid phase is after sewage disposal device work 120 hours (to sewage disposal 120 hours), often process 2 hours waste water, drying machine is entered predrying by the liquid phase of the slag-drip opening discharge evaporating pot volume 2% of evaporating pot, often process 6 days waste water, the fluid after drying machine inner drying is sent into screw extrusion press by PVP concentrate pump and is extruded PVP.
The distillation purifying equipment containing lower concentration DMAc in the waste water of a small amount of low-boiling-point substance and high boiling material for realizing aforesaid method as shown in Figure 1, comprising: primary concentrating tower 5, secondary concentrating tower 6, three grades of upgrading towers 7, evaporating pot 11, level Four upgrading tower 13, rectifying tower 15, extracting towers 25, the outlet of primary concentrating tower 5 overhead vapours is connected with the import of primary concentrating tower tower top flow container 1 through overhead condenser 2, primary concentrating tower tower top flow container 1 exports and is connected with secondary concentrating tower tower top flow container 44 entrance with primary concentrating tower 5 filler 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 opening for feed, 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 three grades of upgrading tower tower top flow container 39 entrances with secondary concentrating tower 6 filler respectively with secondary effluent pump 42 through secondary reflux pump 43, secondary concentrating tower discharging pump 36 is connected with three grades of upgrading tower 7 opening for feeds, three grades of upgrading 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 is connected with three grades of upgrading tower tower top flow container 39 entrances, three grades of upgrading tower tower top flow containers 39 export and go out water pump 37 through three grades of reflux pumps 38 be connected with level Four upgrading tower tower top flow container 35 with three grades of upgrading tower 7 filler respectively with three grades, three grades of upgrading tower discharging pumps 33 are connected with pan feeding a bite of evaporating pot 11, the discharge port of evaporating pot 11 is connected with feed heater 12 entrance through feed cycle pump 31, feed heater 12 exports and is connected with the pan feeding two mouthfuls of evaporating pot 11, the gaseous phase outlet of evaporating pot is connected with level Four upgrading tower 13 opening for feed, the outlet of level Four upgrading tower 13 overhead vapours is connected with reboiler 8 thermal source inlet of three grades of upgrading towers, reboiler 8 thermal source outlet of three grades of upgrading towers is connected with level Four upgrading tower tower top flow container 35 entrance, the outlet of level Four upgrading tower tower top flow container through level Four reflux pump 9 and level Four go out water pump 34 respectively with level Four upgrading tower filler with reclaim water pot or apparatus for treating sewage is connected, level Four upgrading tower discharging pump 29 is connected with rectifying tower 15 opening for feed, the outlet of rectifying tower 15 overhead vapours is connected with rectifying tower tower top flow container 17 entrance through rectifying tower condenser 18, rectifying tower tower top flow container 17 exports and goes out water pump through rectifier column reflux pump 16 and rectifying tower respectively and be connected with level Four upgrading tower tower top flow container entrance with rectifying tower filler, rectifying tower discharging pump 27 is connected with extracting tower 25 opening for feed, 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 water cooler 19, DMAc discharge tank 24 outlet is provided with discharging pump 23, the vacuum port of primary concentrating tower, secondary concentrating tower, three grades of upgrading towers, level Four upgrading tower, rectifying tower, extracting tower is connected to vacuum pump.Evaporating pot blowing slag-drip opening is connected with drying machine 10, the discharge port of drying machine 10 is connected with PVP forcing machine 30 through PVP concentrate pump 32, when the equipment liquid solute run in certain hour, evaporating pot reaches normality, drying machine is entered predrying from the solution of evaporating pot slag-drip opening discharge certain volume, fluid after drying machine inner drying is sent into screw extrusion press by PVP concentrate pump and is extruded PVP(polyvinylpyrrolidone), present treatment device contamination-free is discharged, energy-conserving and environment-protective, and create byproduct, 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 opening for feed through concentrate pump, to the laggard row relax of waste water preheating, and enhancement process effect.When the present invention works, the reboiler 14 of level Four upgrading tower, the feed heater 12 of vaporizer, rectifying tower reboiler 28 are connected with vapour source with the thermal source inlet of extracting tower reboiler 26, thermal source outlet is connected with collection water tank or is connected with the thermal source inlet of feed preheater, makes full use of energy.Primary concentrating tower, secondary concentrating tower, three grades of upgrading towers, level Four upgrading tower, rectifying tower, extracting towers are vacuum operating, and its vacuum tightness is respectively: primary concentrating tower-0.095MPa, secondary concentrating tower-0.085MPa, three grades of upgrading tower-0.068MPa, level Four upgrading tower-0.05MPa, rectifying tower-0.09MPa, extracting tower-0.088MPa.Its vacuum tightness is undertaken aspirating automatic adjustment by vacuum pump.
The present invention has environmental protection, ultrahigh-recovery-rate and the advantage such as energy-conservation, make concentration lower than 10% the energy consumption of DMAc waste-water purification significantly reduce, and the DMAc finished product indices after purifying all reaches the standard of pure DMAc, can reuse, make enterprise reduce cost in liquid waste disposal and the purchasing of raw materials two.Due to the working temperature that the employing of each tower is lower in treating processes, avoid DMAc and at high temperature resolve into acetic acid and dimethylamine, reduce that impurity increases, the change of pH value and specific conductivity, avoid contaminate environment.Four upgrading tower energy supplies that the present invention uses primary energy source to coordinate each upgrading tower to reduce step by step temperature requirement, while energy is made full use of, coordinate the specific temperature of each upgrading tower, vacuum tightness achieves consumption and lacked energy purifying and contain lower concentration (lower than 10%) DMAc waste water, make enterprise reduce cost in liquid waste disposal and the purchasing of raw materials two.
Table 1 multi-effect rectifying process process CIMS
Remarks: steam is by 200 yuan/ton, and electricity is by 1 yuan/degree, and water is by 3 yuan/ton of calculating, and DMAC is by 10000 yuan/ton of calculating.Labour cost does not calculate.
Table 1 is existing three tower triple effects, the some processes index of four tower quadruple effect treatment unit and treatment unit of the present invention and method compares.In table, the listed rate of recovery of the present invention is the real data that equipment runs, and the rate of recovery of three tower triple effects and four tower quadruple effects is most high-recoveries of estimation.Can be seen by upper table, three tower triple effects and four tower quadruple effect two schemes reclaim MDAc value and are less than running cost, only have MDAc of the present invention to be worth and are greater than running cost.
The invention has the advantages that the high and environmental protection of the finished product rate of recovery.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.Service temperature is higher, and the decomposition amount of DMAc is larger, and in overhead water, the content of dimethylamine is higher, corresponding higher of COD value.The overhead water of existing three tower triple effects and four tower quadruple effect treatment facilities just can enter garden sewage network after having to pass through the treatment tank process that plant area carries, and adopts treatment facility of the present invention and treatment process (COD < 200) then can directly access garden sewage network.
Due to the decomposition of DMAc, dimethylamine in the gas phase can enter in air along with vacuum pump, contaminate environment, the current treatment process of the dimethylamine in the gas phase of existing three tower triple effects and four tower quadruple effects is that boiler house burns, but can cause NO and NO in the flue gas of boiler
2exceed standard, cause a large amount of NO and NO
2discharge.And the present invention is because the service temperature of whole system is all lower than 105 DEG C, decomposition amount is extremely low, directly can discharge air.
Therefore, no matter from environmental angle or economic angle, the present invention is best for the treatment effect of the waste liquid of lower concentration.
The described waste water containing a small amount of low-boiling-point substance and high boiling material, refer to that low-boiling-point substance and high boiling material concentration are lower than 5%, a small amount of DMAc refers to that in waste water, DMAc concentration is lower than 10%.Wherein low-boiling-point substance comprises the small molecules such as water, acetic acid, dimethylamine, and high boiling material comprises the polymer such as polyvinylpyrrolidone, polysulfones.DMAc at high temperature easily resolves into acetic acid and dimethylamine, and their generation can make system impurity increase, and pH value and specific conductivity also can change.
Have employed the technical process that drying machine pre-treatment adds the polymer substances such as extruser spiral squeezing polyvinylpyrrolidone, polysulfones, the polymer substance recoverable such as polyvinylpyrrolidone, polysulfones of discharge or go to burn station and burn.
Method and apparatus of the present invention, has following features:
The rate of recovery is high: the technical process adopting level Four concentrating under reduced pressure, the concentrate process of whole DMAc waste liquid is carried out all at low temperatures, and the decomposition amount of DMAc is down to minimum.Simultaneously due to the technical process that have employed crude product DMAc rectification under vacuum, finished product DMAc decompression depickling is refined, whole DMAc finished product treating process is all carried out under very low 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 is less than 200ppm and can returns production line and reuse, and without the need to discharge, has saved water resources.2. because the polymer substance such as polyvinylpyrrolidone, polysulfones concentration in waste liquid is 0.1%, this device have employed the technical process that drying machine pre-treatment adds the polymer substances such as extruser spiral squeezing polyvinylpyrrolidone, polysulfones, and the polymer substance such as polyvinylpyrrolidone, polysulfones of discharge is recycled or gone to burn station and burns.3. dimethylamine content <10mg/ m in air
3, can qualified discharge.
Claims (5)
1. contain a distillation purifying method of lower concentration DMAc in the waste water of a small amount of low-boiling-point substance and high boiling material, it is characterized in that comprising the following steps:
Step 1: the waste water containing 1-10%DMAc, low-boiling-point substance and high boiling material is sent into primary concentrating tower through concentrate 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: send 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: deliver to three grades of upgrading towers by secondary discharging pump when DMAc concentration promotes 0.6%-1.5% in the tower bottoms of secondary concentrating tower and carry out three grades and concentrate, three grades of upgrading tower column bottom temperatures 68 DEG C-72 DEG C, tower top temperature 65 DEG C-69 DEG C;
Step 4: send into evaporating pot by three grades of discharging pumps when DMAc concentration promotes 2%-3% in the tower bottoms of three grades of upgrading towers, then feed heater is entered, heat exchange is carried out to after seething with excitement with steam, enter flash distillation in evaporating pot, gas, liquid are separated, gas phase enter level Four upgrading tower carry out level Four concentrate, level Four upgrading tower column bottom temperature 81 DEG C-85 DEG C, tower top temperature 78 DEG C-82 DEG C; Enter feed heater through feed cycle pump after unevaporated liquid phase and three grades of discharging pumps send into the liquid mixing of evaporating pot in evaporating pot to continue to evaporate;
Step 5: deliver in the middle part of rectifying tower by level Four discharging pump when DMAc concentration reaches 18%-25% in the tower bottoms of level Four upgrading tower, under the acting in conjunction of rectifying tower reboiler and trim the top of column, water is easily vaporized and step by step tray rises, and DMAc then step by step tray declines;
Step 6: in tower bottom of rectifying tower during the moisture <150ppm of DMAc, enter extracting tower by the extraction of tower bottom of rectifying tower liquid phase, DMAc product, by extracting tower top side take-off, enters DMAc discharge tank after pure DMAc water cooler cooling;
In above-mentioned steps, the temperature of one to three grade of upgrading tower heating equipment controls to be controlled by steam regulating valve steam regulation flow; The Energy harvesting method of upgrading tower at different levels, evaporating pot, rectifying tower and extracting tower is: the reboiler of level Four upgrading tower, feed heater, rectifying tower reboiler and the extracting tower reboiler energy are primary steam heating; Level Four upgrading tower overhead vapours heats the reboiler of three grades of upgrading towers, and water of condensation enters four column overhead flow containers; The reboiler of three grades of upgrading tower overhead vapours heating secondary concentrating tower, water of condensation enters three column overhead flow containers; The reboiler of secondary concentrating tower overhead vapours heating primary concentrating tower, water of condensation enters two column overhead flow containers; Primary concentrating tower overhead vapours enters primary concentrating tower overhead condenser and becomes with recirculated water heat exchange after liquid overhead water to enter a column overhead flow container;
A primary concentrating tower overhead water part sends primary concentrating tower back to 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 sends secondary concentrating tower back to 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 upgrading tower overhead water parts send three grades of upgrading towers back to by three grades of upgrading tower reflux pumps, a part is pumped to four column overhead flow containers by three grades of upgrading tower water outlets, a level Four upgrading tower overhead water part sends level Four upgrading tower back to by level Four upgrading tower reflux pump, a part is pumped into tank field tower top water pot by four tower water outlets and returns and produce line and reuse or send into treatment tank and process,
Rectifying tower overhead vapours enters rectifying tower overhead condenser and becomes liquid overhead water with recirculated water heat exchange, and a part is reused by rectifier column reflux pumped back rectifying tower, and a part is pumped to four column overhead water pots by rectifying tower water outlet; Extracting tower overhead vapours enters DMAc condenser and becomes liquid DMAc with recirculated water heat exchange, all sends extracting tower back to by DMAc reflux pump; Four upgrading towers, rectifying tower and extracting towers are vacuum operating, and its vacuum tightness is respectively: primary concentrating tower-0.09MPa between-0.095MPa, secondary concentrating tower between-0.08MPa to-0.086MPa, three grades of upgrading towers between-0.06MPa to-0.07MPa, level Four upgrading tower between-0.04MPa to-0.052MPa, rectifying tower between-0.085MPa to-0.095MPa, extracting tower is between-0.08MPa to-0.09MPa.
2. the distillation purifying method containing lower concentration DMAc in the waste water of a small amount of low-boiling-point substance and high boiling material according to claim 1, to it is characterized in that in described evaporating pot unevaporated liquid phase in work after 120 hours, often process 1 ~ 3 hour waste water, drying machine is entered predrying by the liquid phase of the slag-drip opening discharge evaporating pot volume 1% ~ 3% of evaporating pot, often process 6 days waste water, the fluid after drying machine inner drying is pumped into screw extrusion press by PVP concentrate pump and extrudes PVP.
3., for realizing a kind of distillation purifying equipment containing lower concentration DMAc in the waste water of a small amount of low-boiling-point substance and high boiling material of aforesaid method, it is characterized in that comprising: primary concentrating tower, secondary concentrating tower, three grades of upgrading towers, evaporating pot, level Four upgrading tower, rectifying tower, extracting towers, the outlet of primary concentrating tower overhead vapours is connected with the import of primary concentrating tower tower top flow container through overhead condenser, the outlet of primary concentrating tower tower top flow container is connected with secondary concentrating tower tower top flow container entrance with primary concentrating tower filler with primary effluent pump through one-level reflux pump respectively, primary concentrating tower discharging pump is connected with secondary concentrating tower opening for feed, 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 three grades of upgrading tower tower top flow container entrances with secondary concentrating tower filler with secondary effluent pump through secondary reflux pump respectively, secondary concentrating tower discharging pump is connected with three grades of upgrading tower opening for feeds, and three grades of upgrading tower overhead vapours outlets are connected with the reboiler thermal source inlet of secondary concentrating tower, and the reboiler thermal source outlet of secondary concentrating tower is connected with the tower top flow container entrance of three grades of upgrading towers, the outlet of three grades of upgrading tower tower top flow containers goes out water pump through three grades of reflux pumps be connected with level Four upgrading tower tower top flow container with three grades of upgrading tower filler with three grade respectively, three grades of upgrading tower discharging pumps are connected with pan feeding a bite of evaporating pot, the discharge port of evaporating pot is connected with feed heater entrance through feed cycle pump, feed heater outlet is connected with the pan feeding two mouthfuls of evaporating pot, the gaseous phase outlet of evaporating pot is connected with level Four upgrading tower opening for feed, the outlet of level Four upgrading tower overhead vapours is connected with the reboiler thermal source inlet of three grades of upgrading towers, the reboiler thermal source outlet of three grades of upgrading towers is connected with the tower top flow container entrance of level Four upgrading tower, the tower top flow container outlet of level Four upgrading tower goes out water pump through level Four reflux pump and level Four respectively and is connected with waste water tank with level Four upgrading tower filler, level Four upgrading tower discharging pump is connected with rectifying tower opening for feed, rectifying tower tower top vapour outlet is connected with rectifying tower tower top flow container entrance through rectifying tower condenser, the outlet of rectifying tower tower top flow container goes out water pump through rectifier column reflux pump and rectifying tower respectively and is connected with level Four upgrading tower tower top flow container entrance with rectifying tower filler, rectifying tower discharging pump is connected with extracting tower opening for feed, 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 water cooler, the vacuum port of primary concentrating tower, secondary concentrating tower, three grades of upgrading towers, level Four upgrading tower, rectifying tower, extracting tower is connected to vacuum pump.
4. the distillation purifying equipment containing lower concentration DMAc in the waste water of a small amount of low-boiling-point substance and high boiling material according to claim 3, it is characterized in that described evaporating pot blowing slag-drip opening is connected with drying machine, the discharge port of drying machine is connected with PVP forcing machine through PVP concentrate pump.
5. the distillation purifying equipment containing lower concentration DMAc in the waste water of a small amount of low-boiling-point substance and high boiling material according to claim 3, it is characterized in that described primary concentrating tower side is provided with feed preheater, the outlet of feed preheater is connected with concentrate pump import.
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| CN108774149A (en) * | 2018-07-02 | 2018-11-09 | 南京久盈膜科技有限公司 | A kind of solvent reclaiming method and device in PVDF seperation films production |
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Address after: No.20, Xingshan Road, torch hi tech Industrial Development Zone, Huancui District, Weihai City, Shandong Province 264200 Patentee after: Shandong Weigao blood purification products Co.,Ltd. Patentee after: CHANGZHOU JIDE ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. Address before: No.20, Xingshan Road, torch hi tech Industrial Development Zone, Weihai City, Shandong Province 264200 Patentee before: WEIHAI WEIGAO BLOOD PURIFICATION PRODUCTS Co.,Ltd. Patentee before: CHANGZHOU JIDE ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. |