CN104829484A - Six-tower four-effect rectification system of DMAC or DMF waste liquid, and recovery method thereof - Google Patents
Six-tower four-effect rectification system of DMAC or DMF waste liquid, and recovery method thereof Download PDFInfo
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Abstract
The present invention discloses a six-tower four-effect rectification system of a DMAC and DMF waste liquid. The system comprises a first concentration tower, a second concentration tower, a third concentration tower, a fourth concentration tower, a rectification tower, and a deacidification tower. The invention further discloses a recovery method of the system, wherein the recovery method comprises DMAC and DMF waste liquid recovery treatment, high boiling point material and solid state material recovery treatment, water recycling, and steam recycling. According to the present invention, DMAC and DMF are concentrated within a temperature of 100 DEG C and are rectified and deacidified within a temperature of 105 DEG C, such that the whole process is completely performed at the low temperature, DMAC and DMF substantially are not decomposed, and the DMAC and DMF finished product recovery rate is more than 99%; and with the system and the recovery method, the problems of solid waste pollution and air pollution are solved.
Description
Technical field
The invention belongs to the separation and purification field of DMAC or DMF, be specifically related to a kind of six tower four-effect rectification system for synthesizing and recovery methods thereof of DMAC or DMF waste liquid.
Background technology
DMAC has another name called N,N-dimethylacetamide, DMF has another name called DMF, is excellent organic solvent, is applied in the industries such as medicine, agricultural chemicals, film industry, leather industry, textile industry widely, while use, create DMAC or DMF waste liquid.
Because DMAC or DMF is a kind of fungistat, also can kill the active sludge in treatment tank at low concentrations, therefore utilize the method process DMAC of biochemical treatment or DMF waste liquid to there is no good way at present.Economically consider in addition, the method process DMAC of rectifying or DMF waste liquid is adopted to be best selections, the domestic process for rectifying recovery having a lot of DMAC or DMF waste liquid at present, but ubiquity environmental issue: the product dimethylamine of DMAC or DMF pyrolytic decomposition, dimethylamine has toxicity breath malodor simultaneously.Take the pollution problem that various way all effectively can not solve dimethylamine in recent years, along with the establishment of environmental law, dimethylamine problem more and more causes the attention of Environmental Protection Agency and enterprise, is badly in need of the problem that a good way fundamentally solves dimethylamine.
The patent No. is that the Chinese patent of CN200910116460 discloses a kind of method reclaiming dimethyl formamide, this patent is four tower three-effect rectification recovery methods, technically rectifying tower is changed into rectification under vacuum by atmospheric distillation original, tower bottom of rectifying tower temperature is reduced to about 140 DEG C by about original 160 DEG C, the decomposition of DMF reduces greatly, and the content of degradation production dimethylamine in overhead water of DMF is reduced to about 800ppm by original about 1500ppm.But due to the dimethylamine still containing about 800ppm in overhead water, the smell of overhead water is still very large, could return production line recycling after needing process.In current overhead water, the terms of settlement of dimethylamine is the dimethylamine removed by steam stripped in overhead water, dimethylamine in overhead water can be removed to below 30ppm, but has regenerated two pollutents: the aqueous solution of dimethylamine content about 10% and dimethylamine gas.These two pollutents are all send to boiler house to burn at present, and its final product is nitrogen protoxide and nitrogen peroxide, again contaminate environment, brings new the difficult problem of environmental protection to enterprise.In addition, due to environmental protection, the coal burning boiler that a lot of enterprise has by oneself now requires that dimethylamine can not burn, and how to process the difficult problem of environmental protection that dimethylamine becomes urgently to be resolved hurrily in the recent period at the steam closely changing natural gas boiler in two years into or use instead in garden.
Summary of the invention
The object of the invention is the environmental issue solving existing topsoil and water pollutions, six tower four-effect rectification system for synthesizing and the recovery methods thereof that a kind of rate of recovery is high, reclaim DMAC or the DMF waste liquid of superior product quality are provided.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is:
Six tower four-effect rectification system for synthesizing of DMAC or DMF waste liquid, described six tower four-effect rectification system for synthesizing comprise the first upgrading tower, the second upgrading tower, the 3rd upgrading tower, the 4th upgrading tower, rectifying tower and extracting tower, it is characterized in that:
The material outlet of the waste liquid tank of tank field is connected with feed preheater material inlet through waste drains pump, feed preheater material outlet is connected with the first upgrading tower material inlet, the material outlet of the first upgrading tower is connected through the material inlet of T101 discharging pump with the second upgrading tower, the material outlet of the second upgrading tower is connected through the material inlet of T102 discharging pump with the 3rd upgrading tower, the material outlet of the 3rd upgrading tower is connected with the liquid phase material import of flash tank through T103 discharging pump, the liquid phase material outlet of flash tank is connected through the material inlet of forced circulation pump with charging vaporizer, the material outlet of charging vaporizer is connected with the gaseous phase materials import of flash tank, the gaseous phase materials outlet of flash tank is connected with the material inlet of the 4th upgrading tower, the material outlet of the 4th upgrading tower is connected with the material inlet of rectifying tower through T104 discharging pump, the material outlet of rectifying tower is connected with the material inlet of extracting tower through T105 discharging pump, the top gaseous phase material outlet of extracting tower is connected with the material inlet of DMAC or DMF condenser, the material outlet of DMAC or DMF condenser is connected with the material inlet of DMAC or DMF return tank, the material outlet of DMAC or DMF return tank is connected through the refluxing opening of DMAC or DMF reflux pump with extracting tower tower top, the liquid phase material outlet of extracting tower is connected with the material inlet of DMAC or DMF finished product water cooler, the material outlet of DMAC or DMF finished product water cooler is connected with the material inlet of DMAC or DMF finished pot, the material outlet of DMAC or DMF finished pot is connected through the material inlet of DMAC or DMF discharge pump with the finished pot of tank field.
A recovery method for six tower four-effect rectification system for synthesizing of DMAC or DMF waste liquid, comprises the recycling of the recycling of DMAC or DMF waste liquid, high boiling material and the recycling of solids, the recycling of water and steam.
Wherein, the recycling of above-mentioned DMAC or DMF waste liquid comprises the following steps:
Step 1: the waste liquid containing DMAC or DMF is sent into after feed preheater adopts the steam preheating of steam condensate flash distillation through waste drains pump and entered the first upgrading tower;
Step 2: entering the first upgrading tower (T101) after waste liquid preheating, to carry out first time dehydration concentrated, the first upgrading tower tower top temperature 40-45 DEG C (winter 40 DEG C, summer 45 DEG C), corresponding bottom temperature 43-48 DEG C;
Step 3: the tower bottoms after the first upgrading tower dehydration is concentrated is sent into the second upgrading tower (T102) by T101 discharging pump and carried out second time and dewater concentrated, the second upgrading tower tower top temperature 53 DEG C-58 DEG C, the bottom temperature 55 DEG C-60 DEG C of correspondence;
Step 4: the tower bottoms after the second upgrading tower dehydration is concentrated carries out third time by T102 discharging pump feeding the 3rd upgrading tower (T103) and dewaters concentrated, the 3rd upgrading tower tower top temperature 65 DEG C-70 DEG C, corresponding bottom temperature 67 DEG C-72 DEG C;
Step 5: the tower bottoms after the 3rd upgrading tower dehydration is concentrated sends into flash tank by T103 discharging pump, then charging vaporizer is pumped into by pump circulation, after carrying out heat exchange with primary steam, enter vacuum flashing in flash tank, gas, liquid are separated, and gas phase enters the 4th upgrading tower after wire mesh demister foam removal;
Step 6: it is concentrated that the gas that gas phase enters the 4th upgrading tower carries out the 4th dehydration in the 4th upgrading tower, the 4th upgrading tower tower top temperature 77 DEG C-82 DEG C, corresponding bottom temperature 79 DEG C-84 DEG C;
Step 7: (DMAC or DMF delivers to rectifying tower (T105) middle part charging by T104 discharging pump to the tower bottoms after the 4th upgrading tower dehydration is concentrated, in rectifying tower, in liquid phase, volatile component water shifts in gas phase, in gas phase, difficult volatiles DMAC or DMF shifts in liquid phase, gas, liquid two-phase counter current contact in tower, partial gasification repeatedly and partial condensation, mixed solution is separated, pure water is obtained containing DMAC or DMF<150ppm at tower top, the moisture <150ppm of pure DMAC or DMF is obtained in tower reactor, rectifying tower tower top 40-45 DEG C (winter 40 DEG C, summer 45 DEG C), corresponding bottom temperature 95-100 DEG C,
Step 8: as the moisture <150ppm of tower bottom of rectifying tower liquid, extracting tower (T106) is sent into by T105 discharging pump, in extracting tower, DMAC or DMF, dimethylamine and water easily gasify at extracting tower overhead extraction, DMAC or DMF return tank is entered after DMAC or DMF condenser condenses, extracting tower is sent back to again with DMAC or DMF reflux pump, the azeotrope of difficult volatiles DMAC or DMF and acetic acid (formic acid) is stayed extracting tower tower reactor disintegrate and is balanced, extracting tower tower top 90-95 DEG C, corresponding bottom temperature 100-105 DEG C;
Step 9: after DMAC or DMF sending extracting tower back to removes dimethylamine and water, liquid phase is from the extraction of extracting tower top, enters DMAC or DMF finished pot, then sends into the finished pot of tank field with DMAC or DMF discharge pump after the cooling of DMAC or DMF finished product water cooler.
Wherein, the recycling of above-mentioned high boiling material and solids comprises the following steps:
Step 1: utilize the discharging variable valve of flash tank to regulate discharging flow, the mixing liquid containing high boiling material, solids, DMAC or DMF and water in continuous micro extraction flash tank enters evaporating kettle, high boiling material then in flash tank and solids can maintain the lower concentration of a balance, to reduce the blocking of heat transfer tube in charging vaporizer;
Step 2: the mixing liquid containing high boiling material, solids, DMAC or DMF and water utilizes primary steam to heat at evaporating kettle, adopts high vacuum to be gasified at low temperatures by water simultaneously and enters the first upgrading tower;
Step 3: obtain one in water rear evaporating kettle containing the mixing liquid of high boiling material, solids, DMAC or DMF, deliver to production plant with evaporating kettle discharging pump and recycle.
Wherein, the recycling of above-mentioned water comprises the following steps:
Step 1: the first upgrading tower overhead vapor stream enters overhead condenser and becomes with recirculated water heat exchange liquid overhead water to enter the first upgrading tower tower top flow container, a part sends the first upgrading tower back to by T101 reflux pump, a part is pumped to the second upgrading tower tower top flow container by T101 water outlet;
Step 2: the second upgrading tower overhead vapor stream enters after the first upgrading tower reboiler becomes liquid overhead water with the first upgrading tower tower bottoms heat exchange and enters the second upgrading tower tower top flow container, a part sends the second upgrading tower back to by T102 reflux pump, a part is pumped to the 3rd upgrading tower tower top flow container by T102 water outlet;
Step 3: the 3rd upgrading tower overhead vapor stream enters after the second upgrading tower reboiler becomes liquid overhead water with the second upgrading tower tower bottoms heat exchange and enters the 3rd upgrading tower tower top flow container, a part sends the 3rd upgrading tower back to by T103 reflux pump, a part is pumped to the 4th upgrading tower tower top flow container by T103 water outlet;
Step 4: the 4th upgrading tower overhead vapor stream enters after the 3rd upgrading tower reboiler becomes liquid overhead water with the 3rd upgrading tower tower bottoms heat exchange and enters the 4th upgrading tower tower top flow container, the tower top water pot that a part sends the 4th upgrading tower back to by T104 reflux pump, a part is pumped to tank field by T104 water outlet returns to be produced line and reuses;
Step 5: rectifying tower overhead vapor stream enters rectifying tower overhead condenser and becomes with recirculated water heat exchange liquid overhead water to enter rectifying tower tower top flow container, a part sends rectifying tower back to by T105 reflux pump, a part sends into the 4th upgrading tower tower top flow container after being pumped to gas water separation tank by T105 water outlet again.
Wherein, the recycling of above-mentioned steam comprises the following steps:
Step 1: the 4th upgrading tower reboiler, charging vaporizer, rectifying tower reboiler and the extracting tower reboiler energy are primary steam heating, are controlled the respective temperature of these four equipment by respective steam regulating valve steam regulation flow;
Step 2: the 4th upgrading tower reboiler adopts primary steam heating tower bottoms, the overhead vapor stream of water heat exchange gasification rising formation the 4th upgrading tower in tower bottoms;
Step 3: charging vaporizer adopts the liquid in primary steam heating flash evaporation tank, makes DMAC or DMF and waterly enters the 4th upgrading tower, the overhead vapor stream of water vapor rising formation the 4th upgrading tower;
Step 4: overhead vapor stream heating the 3rd upgrading tower reboiler of the 4th upgrading tower, the overhead vapor stream of water heat exchange gasification rising formation the 3rd upgrading tower in tower bottoms;
Step 5: the overhead vapor stream of the 3rd upgrading tower heats the second upgrading tower reboiler, the overhead vapor stream of water heat exchange gasification rising formation second upgrading tower in tower bottoms;
Step 6: the overhead vapor stream of the second upgrading tower heats the first upgrading tower reboiler, the overhead vapor stream of water heat exchange gasification rising formation first upgrading tower in tower bottoms;
Step 7: the overhead vapor stream of the first upgrading tower becomes liquid overhead water to enter the first upgrading tower tower top flow container with recirculated water heat exchange;
Step 8: rectifying tower reboiler adopts primary steam heating tower bottoms, makes the water heat exchange gasification in tower rise by transmission ofenergy and forms the overhead vapor stream of rectifying tower;
Step 9: the overhead vapor stream of rectifying tower becomes liquid overhead water to enter rectifying tower tower top flow container with recirculated water heat exchange;
Step 10: extracting tower reboiler adopts primary steam heating tower bottoms, makes DMAC or the DMF heat exchange gasification rising in tower form tower top DMAC or the DMF steam of extracting tower by transmission ofenergy;
Step 11: the tower top DMAC of extracting tower or DMF steam become liquid DMAC or DMF to enter DMAC or DMF return tank with recirculated water heat exchange.
Above-mentioned first upgrading tower, the second upgrading tower, the 3rd upgrading tower, the 4th upgrading tower, rectifying tower and extracting tower are vacuum operating, are controlled the respective vacuum tightness of these six towers by respective vacuum conditions valve regulation charge flow rate.First upgrading tower adopts water ring vacuum pump suction, its top vacuum degree is :-0.09MPa-0.0925Mpa, second upgrading tower adopts water ring vacuum pump suction, its top vacuum degree is :-0.0815MPa-0.0855Mpa, 3rd upgrading tower adopts water ring vacuum pump suction, its top vacuum degree is :-0.066MPa-0.072Mpa, 4th upgrading tower adopts water ring vacuum pump suction, its top vacuum degree is :-0.048MPa-0.057Mpa, rectifying tower adopts water ring vacuum pump suction, its top vacuum degree is :-0.09MPa-0.0925Mpa, extracting tower adopts the vacuum pump suction of rectifying tower, its top vacuum degree is :-0.086MPa-0.09Mpa.
Compared with prior art, tool of the present invention has the following advantages:
The present invention solves topsoil and water pollution problems preferably: the decomposition reaction of DMAC or DMF is self-catalyzed reaction, deposit in case in acid or alkali, catalysis can accelerate its decomposition, below 120 DEG C, denier decomposes, and more than the 120 DEG C rising decomposition amounts along with temperature are the increase of geometry multiple.Therefore only have and adopt cryoconcentration and low temperature fractionation, low temperature depickling, fundamentally could suppress the decomposition of DMAC or DMF.DMAC or DMF of the present invention concentrates within 100 DEG C, rectifying and depickling is carried out within 105 DEG C, whole technological process is all carried out at low temperatures, DMAC or DMF does not decompose substantially, the product dimethylamine content <10mg/m in an atmosphere that final DMAC or DMF decomposes
3, can qualified discharge;
The present invention also solves solid waste pollution problem simultaneously, achieves high boiling material and solids recycle, becomes and pollutes into precious.High boiling material in DMAC or DMF waste liquid and solids are the starting material in production process, after adopting high vacuum low temperature to be removed by water, form the mixing liquid containing high boiling material, solids, DMAC or DMF, can return production line and reuse in evaporating kettle.
Originally beam back that yield is high, superior product quality: because DMAC or DMF concentrates within 100 DEG C, rectifying and depickling is carried out within 105 DEG C, DMAC or DMF does not decompose substantially, the rate of recovery >99% of DMAC or DMF finished product, the simultaneously moisture <200ppm of DMAC or DMF finished product, acetic acid <20ppm, dimethylamine <10ppm.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention;
Wherein in order to ensure the Chinese word articulation of figure and can identification, therefore numbering is made to corresponding explanatory note indicate as follows: 1-first upgrading tower tower top flow container; 2-overhead condenser; 3-first upgrading tower vacuum pump; 4-T101 reflux pump; 5-T101 goes out water pump; 6-degass water separation tank; 7-feed preheater; 8-DMAC or DMF waste liquid; 9-steam condensate; 10-hot water tank; 11-first upgrading tower; 12-first upgrading tower reboiler; 13-second upgrading tower tower top flow container; 14-T102 goes out water pump; 15-T102 reflux pump; 16-T101 discharging pump; 17-second upgrading tower; 18-second upgrading tower reboiler; 19-the 3rd upgrading tower tower top flow container; 20-T103 goes out water pump; 21-T103 reflux pump; 22-T102 discharging pump; 23-the 3rd upgrading tower; 24-the 3rd upgrading tower reboiler; 25-the 4th upgrading tower liquid of top of the tower is filled with; 26-T104 goes out water pump; 27-T104 reflux pump; 28-T103 discharging pump; 29-evaporating kettle; 30-evaporating kettle discharging pump; 31-forced circulation pump; 32-flash tank; 33-charging vaporizer; 34-the 4th upgrading tower; 35-the 4th upgrading tower reboiler; 36-T104 discharging pump; 37-rectifying tower reboiler; 38-rectifying tower; 39-T105 discharging pump; 40-extracting tower; 41-extracting tower reboiler; 42-DMAC or DMF finished pot; 43-DMAC or DMF discharge pump; 44-second upgrading tower vacuum pump; 45-the 3rd upgrading tower vacuum pump; 46-the 4th upgrading tower vacuum pump; 47-removes the tower top water pot of tank field; 48-mixed solution removes production plant; 49-steam; 50-DMAC or DMF finished product water cooler; 51-DMAC or DMF return tank; 52-DMAC or DMF reflux pump; 53-T105 reflux pump; 54-T105 goes out water pump; 55-rectifying tower vacuum pump; 56-rectifying tower overhead condenser; 57-rectifying tower tower top flow container; 58-gas water separation tank; 59-gas water separation tank goes out water pump; 60-is from each vacuum pump; 61-DMAC or DMF finished product removes the finished pot of tank field.
Embodiment
A kind of six tower four-effect rectification system for synthesizing of DMAC or DMF waste liquid, comprise the first upgrading tower, second upgrading tower, 3rd upgrading tower, 4th upgrading tower, rectifying tower and extracting tower, the material outlet of the waste liquid tank of tank field is connected with feed preheater material inlet through waste drains pump, feed preheater material outlet is connected with the first upgrading tower material inlet, the material outlet of the first upgrading tower is connected through the material inlet of T101 discharging pump with the second upgrading tower, the material outlet of the second upgrading tower is connected through the material inlet of T102 discharging pump with the 3rd upgrading tower, the material outlet of the 3rd upgrading tower is connected with the liquid phase material import of flash tank through T103 discharging pump, the liquid phase material outlet of flash tank is connected through the material inlet of forced circulation pump with charging vaporizer, the material outlet of charging vaporizer is connected with the gaseous phase materials import of flash tank, the gaseous phase materials outlet of flash tank is connected with the material inlet of the 4th upgrading tower, the material outlet of the 4th upgrading tower is connected with the material inlet of rectifying tower through T104 discharging pump, the material outlet of rectifying tower is connected with the material inlet of extracting tower through T105 discharging pump, the top gaseous phase material outlet of extracting tower is connected with the material inlet of DMAC or DMF condenser, the material outlet of DMAC or DMF condenser is connected with the material inlet of DMAC or DMF return tank, the material outlet of DMAC or DMF return tank is connected through the refluxing opening of DMAC or DMF reflux pump with extracting tower tower top, the liquid phase material outlet of extracting tower is connected with the material inlet of DMAC or DMF finished product water cooler, the material outlet of DMAC or DMF finished product water cooler is connected with the material inlet of DMAC or DMF finished pot, the material outlet of DMAC or DMF finished pot is connected through the material inlet of DMAC or DMF discharge pump with the finished pot of tank field.
A recovery method for six tower four-effect rectification system for synthesizing of DMAC or DMF waste liquid, comprises the recycling of the recycling of DMAC or DMF waste liquid, high boiling material and the recycling of solids, the recycling of water and steam.
Wherein, the recycling of above-mentioned DMAC or DMF waste liquid comprises the following steps:
Step 1: the waste liquid containing DMAC or DMF is sent into after feed preheater adopts the steam preheating of steam condensate flash distillation through waste drains pump and entered the first upgrading tower;
Step 2: entering the first upgrading tower (T101) after waste liquid preheating, to carry out first time dehydration concentrated, the first upgrading tower tower top temperature 40-45 DEG C (winter 40 DEG C, summer 45 DEG C), corresponding bottom temperature 43-48 DEG C;
Step 3: the tower bottoms after the first upgrading tower dehydration is concentrated is sent into the second upgrading tower (T102) by T101 discharging pump and carried out second time and dewater concentrated, the second upgrading tower tower top temperature 53 DEG C-58 DEG C, the bottom temperature 55 DEG C-60 DEG C of correspondence;
Step 4: the tower bottoms after the second upgrading tower dehydration is concentrated carries out third time by T102 discharging pump feeding the 3rd upgrading tower (T103) and dewaters concentrated, the 3rd upgrading tower tower top temperature 65 DEG C-70 DEG C, corresponding bottom temperature 67 DEG C-72 DEG C;
Step 5: the tower bottoms after the 3rd upgrading tower dehydration is concentrated sends into flash tank by T103 discharging pump, then charging vaporizer is pumped into by pump circulation, after carrying out heat exchange with primary steam, enter vacuum flashing in flash tank, gas, liquid are separated, and gas phase enters the 4th upgrading tower after wire mesh demister foam removal;
Step 6: it is concentrated that the gas that gas phase enters the 4th upgrading tower carries out the 4th dehydration in the 4th upgrading tower, the 4th upgrading tower tower top temperature 77 DEG C-82 DEG C, corresponding bottom temperature 79 DEG C-84 DEG C;
Step 7: (DMAC or DMF delivers to rectifying tower (T105) middle part charging by T104 discharging pump to the tower bottoms after the 4th upgrading tower dehydration is concentrated, in rectifying tower, in liquid phase, volatile component water shifts in gas phase, in gas phase, difficult volatiles DMAC or DMF shifts in liquid phase, gas, liquid two-phase counter current contact in tower, partial gasification repeatedly and partial condensation, mixed solution is separated, pure water is obtained containing DMAC or DMF<150ppm at tower top, the moisture <150ppm of pure DMAC or DMF is obtained in tower reactor, rectifying tower tower top 40-45 DEG C (winter 40 DEG C, summer 45 DEG C), corresponding bottom temperature 95-100 DEG C,
Step 8: as the moisture <150ppm of tower bottom of rectifying tower liquid, extracting tower (T106) is sent into by T105 discharging pump, in extracting tower, DMAC or DMF, dimethylamine and water easily gasify at extracting tower overhead extraction, DMAC or DMF return tank is entered after DMAC or DMF condenser condenses, extracting tower is sent back to again with DMAC or DMF reflux pump, the azeotrope of difficult volatiles DMAC or DMF and acetic acid (formic acid) is stayed extracting tower tower reactor disintegrate and is balanced, extracting tower tower top 90-95 DEG C, corresponding bottom temperature 100-105 DEG C;
Step 9: after DMAC or DMF sending extracting tower back to removes dimethylamine and water, liquid phase is from the extraction of extracting tower top, enters DMAC or DMF finished pot, then sends into the finished pot of tank field with DMAC or DMF discharge pump after the cooling of DMAC or DMF finished product water cooler.
The recycling of above-mentioned high boiling material and solids comprises the following steps:
Step 1: utilize the discharging variable valve of flash tank to regulate discharging flow, the mixing liquid containing high boiling material, solids, DMAC or DMF and water in continuous micro extraction flash tank enters evaporating kettle, high boiling material then in flash tank and solids can maintain the lower concentration of a balance, to reduce the blocking of heat transfer tube in charging vaporizer;
Step 2: the mixing liquid containing high boiling material, solids, DMAC or DMF and water utilizes primary steam to heat at evaporating kettle, adopts high vacuum to be gasified at low temperatures by water simultaneously and enters the first upgrading tower;
Step 3: obtain one in water rear evaporating kettle containing the mixing liquid of high boiling material, solids, DMAC or DMF, deliver to production plant with evaporating kettle discharging pump and recycle.
The recycling of above-mentioned water comprises the following steps:
Step 1: the first upgrading tower overhead vapor stream enters overhead condenser and becomes with recirculated water heat exchange liquid overhead water to enter the first upgrading tower tower top flow container, a part sends the first upgrading tower back to by T101 reflux pump, a part is pumped to the second upgrading tower tower top flow container by T101 water outlet;
Step 2: the second upgrading tower overhead vapor stream enters after the first upgrading tower reboiler becomes liquid overhead water with the first upgrading tower tower bottoms heat exchange and enters the second upgrading tower tower top flow container, a part sends the second upgrading tower back to by T102 reflux pump, a part is pumped to the 3rd upgrading tower tower top flow container by T102 water outlet;
Step 3: the 3rd upgrading tower overhead vapor stream enters after the second upgrading tower reboiler becomes liquid overhead water with the second upgrading tower tower bottoms heat exchange and enters the 3rd upgrading tower tower top flow container, a part sends the 3rd upgrading tower back to by T103 reflux pump, a part is pumped to the 4th upgrading tower tower top flow container by T103 water outlet;
Step 4: the 4th upgrading tower overhead vapor stream enters after the 3rd upgrading tower reboiler becomes liquid overhead water with the 3rd upgrading tower tower bottoms heat exchange and enters the 4th upgrading tower tower top flow container, the tower top water pot that a part sends the 4th upgrading tower back to by T104 reflux pump, a part is pumped to tank field by T104 water outlet returns to be produced line and reuses;
Step 5: rectifying tower overhead vapor stream enters rectifying tower overhead condenser and becomes with recirculated water heat exchange liquid overhead water to enter rectifying tower tower top flow container, a part sends rectifying tower back to by T105 reflux pump, a part sends into the 4th upgrading tower tower top flow container after being pumped to gas water separation tank by T105 water outlet again.
The recycling of above-mentioned steam comprises the following steps:
Step 1: the 4th upgrading tower reboiler, charging vaporizer, rectifying tower reboiler and the extracting tower reboiler energy are primary steam heating, are controlled the respective temperature of these four equipment by respective steam regulating valve steam regulation flow;
Step 2: the 4th upgrading tower reboiler adopts primary steam heating tower bottoms, the overhead vapor stream of water heat exchange gasification rising formation the 4th upgrading tower in tower bottoms;
Step 3: charging vaporizer adopts the liquid in primary steam heating flash evaporation tank, makes DMAC or DMF and waterly enters the 4th upgrading tower, the overhead vapor stream of water vapor rising formation the 4th upgrading tower;
Step 4: overhead vapor stream heating the 3rd upgrading tower reboiler of the 4th upgrading tower, the overhead vapor stream of water heat exchange gasification rising formation the 3rd upgrading tower in tower bottoms;
Step 5: the overhead vapor stream of the 3rd upgrading tower heats the second upgrading tower reboiler, the overhead vapor stream of water heat exchange gasification rising formation second upgrading tower in tower bottoms;
Step 6: the overhead vapor stream of the second upgrading tower heats the first upgrading tower reboiler, the overhead vapor stream of water heat exchange gasification rising formation first upgrading tower in tower bottoms;
Step 7: the overhead vapor stream of the first upgrading tower becomes liquid overhead water to enter the first upgrading tower tower top flow container with recirculated water heat exchange;
Step 8: rectifying tower reboiler adopts primary steam heating tower bottoms, makes the water heat exchange gasification in tower rise by transmission ofenergy and forms the overhead vapor stream of rectifying tower;
Step 9: the overhead vapor stream of rectifying tower becomes liquid overhead water to enter rectifying tower tower top flow container with recirculated water heat exchange;
Step 10: extracting tower reboiler adopts primary steam heating tower bottoms, makes DMAC or the DMF heat exchange gasification rising in tower form tower top DMAC or the DMF steam of extracting tower by transmission ofenergy;
Step 11: the tower top DMAC of extracting tower or DMF steam become liquid DMAC or DMF to enter DMAC or DMF return tank with recirculated water heat exchange.
Following table is four-effect rectification system for synthesizing and the present invention's comparing in running condition:
As can be known from the above table, DMAC or DMF of the present invention concentrates within 100 DEG C, within 105 DEG C, carry out rectifying and depickling, and whole technological process is all carried out at low temperatures.Because DMAC or DMF concentrates within 100 DEG C, within 105 DEG C, carry out rectifying and depickling, DMAC or DMF does not decompose substantially, DMAC or DMF finished product rate of recovery >99%, dimethylamine content <30ppm in overhead water, solves water pollution problems simultaneously.
Claims (5)
1. six tower four-effect rectification system for synthesizing of DMAC or DMF waste liquid, described six tower four-effect rectification system for synthesizing comprise the first upgrading tower, the second upgrading tower, the 3rd upgrading tower, the 4th upgrading tower, rectifying tower and extracting tower, it is characterized in that:
The material outlet of the waste liquid tank of tank field is connected with feed preheater material inlet through waste drains pump, feed preheater material outlet is connected with the first upgrading tower material inlet, the material outlet of the first upgrading tower is connected through the material inlet of T101 discharging pump with the second upgrading tower, the material outlet of the second upgrading tower is connected through the material inlet of T102 discharging pump with the 3rd upgrading tower, the material outlet of the 3rd upgrading tower is connected with the liquid phase material import of flash tank through T103 discharging pump, the liquid phase material outlet of flash tank is connected through the material inlet of forced circulation pump with charging vaporizer, the material outlet of charging vaporizer is connected with the gaseous phase materials import of flash tank, the gaseous phase materials outlet of flash tank is connected with the material inlet of the 4th upgrading tower, the material outlet of the 4th upgrading tower is connected with the material inlet of rectifying tower through T104 discharging pump, the material outlet of rectifying tower is connected with the material inlet of extracting tower through T105 discharging pump, the top gaseous phase material outlet of extracting tower is connected with the material inlet of DMAC or DMF condenser, the material outlet of DMAC or DMF condenser is connected with the material inlet of DMAC or DMF return tank, the material outlet of DMAC or DMF return tank is connected through the refluxing opening of DMAC or DMF reflux pump with extracting tower tower top, the liquid phase material outlet of extracting tower is connected with the material inlet of DMAC or DMF finished product water cooler, the material outlet of DMAC or DMF finished product water cooler is connected with the material inlet of DMAC or DMF finished pot, the material outlet of DMAC or DMF finished pot is connected through the material inlet of DMAC or DMF discharge pump with the finished pot of tank field.
2. the recovery method of six tower four-effect rectification system for synthesizing of DMAC or DMF waste liquid described in a claim 1, comprise the recycling of the recycling of DMAC or DMF waste liquid, high boiling material and the recycling of solids, the recycling of water and steam, it is characterized in that, the recycling of described DMAC or DMF waste liquid comprises the following steps:
Step 1: the waste liquid containing DMAC or DMF is sent into after feed preheater adopts the steam preheating of steam condensate flash distillation through waste drains pump and entered the first upgrading tower;
Step 2: entering the first upgrading tower (T101) after waste liquid preheating, to carry out first time dehydration concentrated, the first upgrading tower tower top temperature 40-45 DEG C (winter 40 DEG C, summer 45 DEG C), corresponding bottom temperature 43-48 DEG C;
Step 3: the tower bottoms after the first upgrading tower dehydration is concentrated is sent into the second upgrading tower (T102) by T101 discharging pump and carried out second time and dewater concentrated, the second upgrading tower tower top temperature 53 DEG C-58 DEG C, the bottom temperature 55 DEG C-60 DEG C of correspondence;
Step 4: the tower bottoms after the second upgrading tower dehydration is concentrated carries out third time by T102 discharging pump feeding the 3rd upgrading tower (T103) and dewaters concentrated, the 3rd upgrading tower tower top temperature 65 DEG C-70 DEG C, corresponding bottom temperature 67 DEG C-72 DEG C;
Step 5: the tower bottoms after the 3rd upgrading tower dehydration is concentrated sends into flash tank by T103 discharging pump, then charging vaporizer is pumped into by pump circulation, after carrying out heat exchange with primary steam, enter vacuum flashing in flash tank, gas, liquid are separated, and gas phase enters the 4th upgrading tower after wire mesh demister foam removal;
Step 6: it is concentrated that the gas that gas phase enters the 4th upgrading tower carries out the 4th dehydration in the 4th upgrading tower, the 4th upgrading tower tower top temperature 77 DEG C-82 DEG C, corresponding bottom temperature 79 DEG C-84 DEG C;
Step 7: (DMAC or DMF delivers to rectifying tower (T105) middle part charging by T104 discharging pump to the tower bottoms after the 4th upgrading tower dehydration is concentrated, in rectifying tower, in liquid phase, volatile component water shifts in gas phase, in gas phase, difficult volatiles DMAC or DMF shifts in liquid phase, gas, liquid two-phase counter current contact in tower, partial gasification repeatedly and partial condensation, mixed solution is separated, pure water is obtained containing DMAC or DMF<150ppm at tower top, the moisture <150ppm of pure DMAC or DMF is obtained in tower reactor, rectifying tower tower top 40-45 DEG C (winter 40 DEG C, summer 45 DEG C), corresponding bottom temperature 95-100 DEG C,
Step 8: as the moisture <150ppm of tower bottom of rectifying tower liquid, extracting tower (T106) is sent into by T105 discharging pump, in extracting tower, DMAC or DMF, dimethylamine and water easily gasify at extracting tower overhead extraction, DMAC or DMF return tank is entered after DMAC or DMF condenser condenses, extracting tower is sent back to again with DMAC or DMF reflux pump, the azeotrope of difficult volatiles DMAC or DMF and acetic acid (formic acid) is stayed extracting tower tower reactor disintegrate and is balanced, extracting tower tower top 90-95 DEG C, corresponding bottom temperature 100-105 DEG C;
Step 9: after DMAC or DMF sending extracting tower back to removes dimethylamine and water, liquid phase is from the extraction of extracting tower top, enters DMAC or DMF finished pot, then sends into the finished pot of tank field with DMAC or DMF discharge pump after the cooling of DMAC or DMF finished product water cooler.
3. the recovery method of six tower four-effect rectification system for synthesizing of DMAC or DMF waste liquid as claimed in claim 2, it is characterized in that, the recycling of described high boiling material and solids comprises the following steps:
Step 1: utilize the discharging variable valve of flash tank to regulate discharging flow, the mixing liquid containing high boiling material, solids, DMAC or DMF and water in continuous micro extraction flash tank enters evaporating kettle, high boiling material then in flash tank and solids can maintain the lower concentration of a balance, to reduce the blocking of heat transfer tube in charging vaporizer;
Step 2: the mixing liquid containing high boiling material, solids, DMAC or DMF and water utilizes primary steam to heat at evaporating kettle, adopts high vacuum to be gasified at low temperatures by water simultaneously and enters the first upgrading tower;
Step 3: obtain one in water rear evaporating kettle containing the mixing liquid of high boiling material, solids, DMAC or DMF, deliver to production plant with evaporating kettle discharging pump and recycle.
4. the recovery method of six tower four-effect rectification system for synthesizing of DMAC or DMF waste liquid as claimed in claim 2, it is characterized in that, the recycling of described water comprises the following steps:
Step 1: the first upgrading tower overhead vapor stream enters overhead condenser and becomes with recirculated water heat exchange liquid overhead water to enter the first upgrading tower tower top flow container, a part sends the first upgrading tower back to by T101 reflux pump, a part is pumped to the second upgrading tower tower top flow container by T101 water outlet;
Step 2: the second upgrading tower overhead vapor stream enters after the first upgrading tower reboiler becomes liquid overhead water with the first upgrading tower tower bottoms heat exchange and enters the second upgrading tower tower top flow container, a part sends the second upgrading tower back to by T102 reflux pump, a part is pumped to the 3rd upgrading tower tower top flow container by T102 water outlet;
Step 3: the 3rd upgrading tower overhead vapor stream enters after the second upgrading tower reboiler becomes liquid overhead water with the second upgrading tower tower bottoms heat exchange and enters the 3rd upgrading tower tower top flow container, a part sends the 3rd upgrading tower back to by T103 reflux pump, a part is pumped to the 4th upgrading tower tower top flow container by T103 water outlet;
Step 4: the 4th upgrading tower overhead vapor stream enters after the 3rd upgrading tower reboiler becomes liquid overhead water with the 3rd upgrading tower tower bottoms heat exchange and enters the 4th upgrading tower tower top flow container, the tower top water pot that a part sends the 4th upgrading tower back to by T104 reflux pump, a part is pumped to tank field by T104 water outlet returns to be produced line and reuses;
Step 5: rectifying tower overhead vapor stream enters rectifying tower overhead condenser and becomes with recirculated water heat exchange liquid overhead water to enter rectifying tower tower top flow container, a part sends rectifying tower back to by T105 reflux pump, a part sends into the 4th upgrading tower tower top flow container after being pumped to gas water separation tank by T105 water outlet again.
5. the recovery method of six tower four-effect rectification system for synthesizing of DMAC or DMF waste liquid as claimed in claim 2, it is characterized in that, the recycling of described steam comprises the following steps:
Step 1: the 4th upgrading tower reboiler, charging vaporizer, rectifying tower reboiler and the extracting tower reboiler energy are primary steam heating, are controlled the respective temperature of these four equipment by respective steam regulating valve steam regulation flow;
Step 2: the 4th upgrading tower reboiler adopts primary steam heating tower bottoms, the overhead vapor stream of water heat exchange gasification rising formation the 4th upgrading tower in tower bottoms;
Step 3: charging vaporizer adopts the liquid in primary steam heating flash evaporation tank, makes DMAC or DMF and waterly enters the 4th upgrading tower, the overhead vapor stream of water vapor rising formation the 4th upgrading tower;
Step 4: overhead vapor stream heating the 3rd upgrading tower reboiler of the 4th upgrading tower, the overhead vapor stream of water heat exchange gasification rising formation the 3rd upgrading tower in tower bottoms;
Step 5: the overhead vapor stream of the 3rd upgrading tower heats the second upgrading tower reboiler, the overhead vapor stream of water heat exchange gasification rising formation second upgrading tower in tower bottoms;
Step 6: the overhead vapor stream of the second upgrading tower heats the first upgrading tower reboiler, the overhead vapor stream of water heat exchange gasification rising formation first upgrading tower in tower bottoms;
Step 7: the overhead vapor stream of the first upgrading tower becomes liquid overhead water to enter the first upgrading tower tower top flow container with recirculated water heat exchange;
Step 8: rectifying tower reboiler adopts primary steam heating tower bottoms, makes the water heat exchange gasification in tower rise by transmission ofenergy and forms the overhead vapor stream of rectifying tower;
Step 9: the overhead vapor stream of rectifying tower becomes liquid overhead water to enter rectifying tower tower top flow container with recirculated water heat exchange;
Step 10: extracting tower reboiler adopts primary steam heating tower bottoms, makes DMAC or the DMF heat exchange gasification rising in tower form tower top DMAC or the DMF steam of extracting tower by transmission ofenergy;
Step 11: the tower top DMAC of extracting tower or DMF steam become liquid DMAC or DMF to enter DMAC or DMF return tank with recirculated water heat exchange.
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| CN201510175184.XA CN104829484A (en) | 2015-04-14 | 2015-04-14 | Six-tower four-effect rectification system of DMAC or DMF waste liquid, and recovery method thereof |
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| CN201510175184.XA CN104829484A (en) | 2015-04-14 | 2015-04-14 | Six-tower four-effect rectification system of DMAC or DMF waste liquid, and recovery method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107098826A (en) * | 2017-05-18 | 2017-08-29 | 常州冀德环保科技有限公司 | The ten towers six effect distillation system and recovery method of a kind of DMAC or DMF waste liquids |
| 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 |
| CN112807732A (en) * | 2021-02-02 | 2021-05-18 | 常州冀德环保科技有限公司 | Three-tower two-effect rectification system and recovery method for NMP waste liquid |
| CN112933631A (en) * | 2021-02-02 | 2021-06-11 | 常州冀德环保科技有限公司 | Five-tower four-effect rectification system and recovery method for NMP waste liquid |
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2015
- 2015-04-14 CN CN201510175184.XA patent/CN104829484A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107098826A (en) * | 2017-05-18 | 2017-08-29 | 常州冀德环保科技有限公司 | The ten towers six effect distillation system and recovery method of a kind of DMAC or DMF waste liquids |
| 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 |
| CN112807732A (en) * | 2021-02-02 | 2021-05-18 | 常州冀德环保科技有限公司 | Three-tower two-effect rectification system and recovery method for NMP waste liquid |
| CN112933631A (en) * | 2021-02-02 | 2021-06-11 | 常州冀德环保科技有限公司 | Five-tower four-effect rectification system and recovery method for NMP waste liquid |
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Application publication date: 20150812 |