CN208166891U - A kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system - Google Patents
A kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system Download PDFInfo
- Publication number
- CN208166891U CN208166891U CN201820456311.2U CN201820456311U CN208166891U CN 208166891 U CN208166891 U CN 208166891U CN 201820456311 U CN201820456311 U CN 201820456311U CN 208166891 U CN208166891 U CN 208166891U
- Authority
- CN
- China
- Prior art keywords
- tower
- effect
- unit
- crude product
- reboiler
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn - After Issue
Links
- 239000007788 liquid Substances 0.000 title claims abstract description 143
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 title claims abstract description 142
- 230000018044 dehydration Effects 0.000 title claims abstract description 100
- 238000006297 dehydration reaction Methods 0.000 title claims abstract description 100
- 239000002699 waste material Substances 0.000 title claims abstract description 66
- 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 title claims abstract description 49
- GSNUFIFRDBKVIE-UHFFFAOYSA-N DMF Natural products CC1=CC=C(C)O1 GSNUFIFRDBKVIE-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000011084 recovery Methods 0.000 title claims abstract description 39
- 238000000746 purification Methods 0.000 title claims abstract description 38
- 239000012043 crude product Substances 0.000 claims abstract description 102
- 238000010438 heat treatment Methods 0.000 claims abstract description 46
- 239000011552 falling film Substances 0.000 claims abstract description 45
- 238000001704 evaporation Methods 0.000 claims abstract description 36
- 230000008020 evaporation Effects 0.000 claims abstract description 32
- 238000000926 separation method Methods 0.000 claims abstract description 24
- 239000002351 wastewater Substances 0.000 claims abstract description 10
- 230000000694 effects Effects 0.000 claims description 276
- 239000000047 product Substances 0.000 claims description 153
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 238000010992 reflux Methods 0.000 claims description 31
- 239000006096 absorbing agent Substances 0.000 claims description 22
- 230000004087 circulation Effects 0.000 claims description 18
- 239000002253 acid Substances 0.000 claims description 17
- 238000009835 boiling Methods 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 10
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims description 7
- 238000001179 sorption measurement Methods 0.000 claims description 7
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims 1
- 235000011941 Tilia x europaea Nutrition 0.000 claims 1
- 239000004571 lime Substances 0.000 claims 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 abstract description 87
- 238000000605 extraction Methods 0.000 abstract description 33
- 239000002904 solvent Substances 0.000 abstract description 14
- 229910021655 trace metal ion Inorganic materials 0.000 abstract description 4
- 230000000630 rising effect Effects 0.000 abstract description 3
- 208000005156 Dehydration Diseases 0.000 description 80
- 239000012071 phase Substances 0.000 description 15
- 238000000034 method Methods 0.000 description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 238000007670 refining Methods 0.000 description 7
- 230000008878 coupling Effects 0.000 description 6
- 238000010168 coupling process Methods 0.000 description 6
- 238000005859 coupling reaction Methods 0.000 description 6
- 238000004064 recycling Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 230000002411 adverse Effects 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 3
- 229940113088 dimethylacetamide Drugs 0.000 description 3
- 239000012492 regenerant Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 241000237502 Ostreidae Species 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- ZMZINYUKVRMNTG-UHFFFAOYSA-N acetic acid;formic acid Chemical compound OC=O.CC(O)=O ZMZINYUKVRMNTG-UHFFFAOYSA-N 0.000 description 1
- 244000245420 ail Species 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- ODLMAHJVESYWTB-UHFFFAOYSA-N ethylmethylbenzene Natural products CCCC1=CC=CC=C1 ODLMAHJVESYWTB-UHFFFAOYSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000004611 garlic Nutrition 0.000 description 1
- ZFSXZJXLKAJIGS-UHFFFAOYSA-N halocarban Chemical compound C1=C(Cl)C(C(F)(F)F)=CC(NC(=O)NC=2C=CC(Cl)=CC=2)=C1 ZFSXZJXLKAJIGS-UHFFFAOYSA-N 0.000 description 1
- 229950006625 halocarban Drugs 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000020636 oyster Nutrition 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
Abstract
The utility model discloses a kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system, and waste liquid is preheated through feed preheater, continuously fed from falling film evaporator；In gas-liquid separation chamber's gas-liquid separation after falling film evaporator heats, vapour phase enters MVR concentration tower；MVR heat pump group carries out pressurization heating as the heat source of falling film evaporator to the waste liquid steam that MVR concentration tower generates and uses, and the low concentration waste liquid that will be delivered to MVR upgrading unit carries out concentration raising, and the low concentration waste liquid after concentration raising is delivered to dewatering unit and is dehydrated；MVR upgrading unit and dewatering unit extracted waste water go stripping to take off light unit stripping lightness-removing column, heat through primary steam, and the steam for rising to tower top is condensed back through stripping condenser of light component removal column；The de- weight unit of evaporation and crude product unit extraction reboiling object remove reboiling processing unit.The utility model to low concentration waste liquid carry out solvent recovery, can remove containing trace metal ion.
Description
Technical field
The utility model relates to a kind of waste liquid dehydration refining and reclaiming technology and system, more particularly to can be used for low concentration
The waste liquids such as DMAC, DMF or DMSO dehydration purification recovery system.
Background technique
DMAC scientific name dimethyl acetamide, in organic synthesis, dimethyl acetamide is fabulous catalyst, can make ring
The reactions such as change, halogenation, cyaniding, alkylation and dehydrogenation accelerate, and can improve primary product yield.Medicine and pesticide producing in part
In, dimethyl acetamide can also be used as solvent or co-catalyst, compared with conventional organic solvents, to product quality and yield
The effect of being improved.
DMF scientific name dimethylformamide, be both a kind of industrial chemicals that purposes is extremely wide and it is a kind of have many uses it is excellent
Solvent.Dimethylformamide is good to a variety of high polymers such as polyethylene, polyvinyl chloride, polyacrylonitrile, polyamide etc.
Solvent can be used for the synthesis of the wet spinning silk, polyurethane of the synthetic fibers such as polyacrylonitrile fibre；It is film-made for plastics；It can also go
The paint stripper of paint-removing；It can also dissolve the pigment of certain low solubilities, make the characteristics of pigment is with dyestuff.
DMSO scientific name dimethyl sulfoxide, is a kind of organic compounds containing sulfur, is the transparency liquid of no color or smell under room temperature, has
Strong garlic or oyster taste, existing highly polar, higher boiling is non-proton, and in the miscible characteristic of water, toxicity is extremely low, and heat is steady
It is qualitative good, it can be dissolved in ethyl alcohol, propyl alcohol, benzene and chloroform etc. are most, count organic matter, are known as " alembroth ".Dimethyl sulfoxide is wide
It is general be used as make process solvent in solvent and reaction reagent, especially acrylonitrile polymerization reaction and reel off raw silk from cocoons solvent, make polyurethane synthesis
And the solvent that reels off raw silk from cocoons, make polyamide, the synthetic and aromatic hydrocarbons of polyimides and polysulfone resin, Butadiene Extraction solvent and conjunction
At the solvent etc. of cloflucarban.
Ecological problem caused by Environmental pollution is increasingly paid attention at present, and the chemical substances such as DMAC, DMF or DMSO make
Lot of trace can be contained with the waste liquid containing DMAC, DMF or DMSO that can generate more low concentration in the process, while in waste liquid
Metallic element, these waste liquids, which are directly discharged into environment, will cause the pollution of environment, influence the health of animals and plants.Publication No.
The Chinese patent of CN107098826A discloses the ten towers six effect distillation system and method for a kind of DMAC or DMF waste liquid, the patent
Equipped with feed preheater, the first concentration tower, the second concentration tower, third concentration tower, the 4th concentration tower, the 5th concentration tower, the 6th dense
Contracting tower, rectifying column, extracting tower, acetic acid (formic acid) decomposition tower, de- amine tower, flash tank, drying machine and gas water separation tank, incinerator,
Although the patent can recycle the DMAC or DMF contained, be not suitable for concentration for the treatment of lower DMAC, DMF or
DMSO waste liquid, such as the low concentration solution that solvent strength is 3-15%, while regenerant contains micro metal member in treatment process
Element, purity is low, how to be to need to processing is carried out with DMAC, DMF or DMSO of metallic element or similar waste liquid containing low concentration
It solves the problems, such as.
Utility model content
The utility model refines back in view of the deficienciess of the prior art, providing a kind of dehydration of DMAC, DMF or DMSO waste liquid
Receipts system is handled for DMAC, DMF or DMSO containing substances such as metallic element, acid or similar waste liquid, can be right
DMAC, DMF or DMSO or similar waste liquid carry out solvent recovery, at the same can remove the trace metal ion contained in regenerant and
Acid etc..
The technical solution that the utility model solves above-mentioned technical problem is as follows：The utility model provide a kind of DMAC, DMF or
DMSO waste liquid dehydration purification recovery system, the recovery system include MVR upgrading unit, dewatering unit, evaporate de- weight unit, is thick
Article unit, product purification unit, stripping take off light unit and reboiling processing unit；
The MVR upgrading unit is equipped with feed preheater, falling film evaporator, gas-liquid separation chamber, MVR concentration tower, MVR heat pump
Group and MVR concentration tower return tank, the feed preheater connect falling film evaporator；The falling film evaporator lower end is connected with gas-liquid
Separation chamber, vapour phase enter MVR concentration tower；The MVR heat pump group is connected between the MVR concentration tower and falling film evaporator, institute
MVR concentration tower is stated for the low concentration waste liquid of MVR upgrading unit to be carried out concentration raising, the low concentration waste liquid after concentration improves is defeated
It send to dewatering unit and is dehydrated；The MVR concentration tower return tank connects the falling film evaporator；
The dewatering unit includes several sequentially connected dehydrating towers, and the lower part of each dehydrating tower is connected with dehydrating tower and boils again
The steam of device, dehydration column overhead is connected to form multiple-effect coupling as the heat source of next effect dehydrating tower with next effect dehydration column reboiler
It closes；
The de- weight unit of evaporation includes forced circulating reboiler, forced circulation pump, evaporator and gas-liquid separator, described
Forced circulating reboiler connects last effect dehydrating tower of the dewatering unit, and forced circulating reboiler is connected by forced circulation pump
The evaporator；The evaporator top connects the crude product tower of the crude product unit through the gas-liquid separator；
The crude product unit is equipped with crude product tower, crude product tower reboiler, crude product tower return tank and crude product tower condenser, described thick
Product tower lower part connects the crude product tower reboiler, and crude product tower top connects the crude product tower through crude product tower condenser and flows back
Tank；The crude product tower return tank returns and is connected to the crude product tower；
The product purification unit includes an effect product tower, an effect product tower reboiler, an effect product tower return tank, two effects
Product tower, two effect product tower reboilers, two effect product tower condensers, two effect product tower return tanks, absorber and depickling device, it is described
The one effect product tower connection two effects product tower, an effect product tower lower part connection one effect product tower reboiler；One effect
Product tower return tank is connected between an effect product tower and two effect product tower reboilers, and an effect product tower return tank is also connected with
To the absorber；The two effects product tower connects the crude product tower tower reactor gas-phase space；Two effects product tower connection, two effect
Product tower reboiler, the two effect product column overhead connection two effects product tower condensers, the two effects product tower condenser connection
The two effects product tower return tank；The absorber connection two effects product tower, absorber is for passing through nonionic adsorption resin
The microelement absorption that condensate liquid is contained；The depickling device is connected to an effect product tower lower part, for removing in Produced Liquid
Acid；
It includes stripping lightness-removing column reboiler, stripping lightness-removing column and stripping condenser of light component removal column, institute that the stripping, which takes off light unit,
It states stripping lightness-removing column reboiler and is placed in the stripping lightness-removing column lower part as stripping lightness-removing column heating, the stripping condenser of light component removal column
Stripping lightness-removing column top is placed in for condensed steam and conveying fixed gas；
The reboiling processing unit includes scraper evaporator, thick evaporation condenser and crude product receiving tank, the scraper evaporator
It is connected with thick evaporation condenser, the thick evaporation condenser is connected to crude product receiving tank.
A kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system as described above, the dewatering unit are equipped with an effect
Dehydrating tower, two effect dehydrating towers and triple effect dehydrating tower, it is that two effects are de- that an effect dehydration column overhead steam, which enters two effect dehydration column reboilers,
Water tower heating, two effect dehydration column reboiler condensate liquids enter an effect dehydrating tower return tank, then through effect dehydrating tower reflux pump one
Divide and is back to an effect dehydration column overhead；One effect dehydrating tower kettle liquid is delivered to two effect dehydrating towers, and two effect dehydration column overhead steam enter
Triple effect dehydration column reboiler is the heating of triple effect dehydrating tower, and triple effect dehydrating tower condensate liquid is delivered to two effect dehydrating tower return tanks, then passes through
Two effect dehydrating tower reflux pump a part are back to two effect dehydration column overheads；Triple effect dehydration column overhead steam enters forced circulation and boils again
Device is evaporator heating, and evaporator condensate liquid is delivered to triple effect dehydrating tower return tank, then through triple effect dehydrating tower reflux pump a part
It is back to triple effect dehydration column overhead, another part, which is produced to stripping, takes off light unit.
A kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system as described above, the evaporator, which continuously produces, to be contained
The solution of solid high-boiling components enters scraper evaporator；Into scraper evaporator solid high-boiling components solution in vacuum degree -0.08Mpa
It under conditions of~-0.1MPa, is heated using primary steam, steams thick matter product and water, entered after the condensation of thick evaporation condenser thick
Product receiving tank returns to preamble workshop section and continues to recycle.
A kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system as described above, the falling film evaporator are only driven
Initial stage uses, an effect dehydration column reboiler, two effect dehydration column reboilers, triple effect dehydration column reboiler, forced circulating reboiler, thick
Product tower reboiler and scraper evaporator are heated using primary steam, adjust steam heating amount by respective steam control valve.
A kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system as described above, the MVR upgrading unit and de-
Water unit removed overhead waste water takes off light cell processing through stripping and removes ammonia nitrogen waste therein, and water, which is further continued for return preamble workshop section, to be made
With.
Recovery process using the utility model recovery system includes MVR upgrading unit, dewatering unit, the de- weight list of evaporation
Member, crude product unit, product purification unit, stripping take off light unit and reboiling processing unit, and it is pre- that the MVR upgrading unit is equipped with charging
Hot device, falling film evaporator, gas-liquid separation chamber, MVR concentration tower, MVR heat pump group and MVR concentration tower return tank, waste liquid are pre- through feeding
Hot device preheating, continuously feeds from falling film evaporator；Gas-liquid separation, vapour phase are carried out in gas-liquid separation chamber after falling film evaporator heats
Into MVR concentration tower；The waste liquid steam that the MVR heat pump group generates the MVR concentration tower carries out described in pressurization heating conduct
The heat source of falling film evaporator uses, and the low concentration waste liquid that will be delivered to MVR upgrading unit carries out concentration raising, after concentration improves
Low concentration waste liquid is delivered to dewatering unit and is dehydrated；The dewatering unit is equipped with several sequentially connected dehydrating towers, Ruo Ganyi
The dehydrating tower of secondary connection uses multiple-effect fair current coupling, adverse current or advection mode；The first dehydrating tower of dewatering unit is by being transported to again
The primary steam heat temperature raising for boiling device, the steam for rising to dehydration column overhead are de- as the heat source of next effect dehydrating tower and next effect
Water tower reboiler is connected to form multiple-effect coupling, and multiple-effect is dehydrated last effect dehydrating tower kettle liquid and turns to expect to be transported to evaporation by transfering material pump
De- weight unit evaporates de- weight unit and is heated by forced circulation pump circulation and forced circulating reboiler, and gas-liquid mixed is mutually by steaming
It sends out tank and gas-liquid separator carries out gas-liquid separation, vapour phase is delivered to crude product tower；Crude product column overhead steam is condensed through overhead condenser
Rear portion is back to crude product tower, a part extraction；Crude product unit crude product tower bottoms is produced to product purification unit, product purification
One effect product column overhead of unit obtains product and is transported to absorber, and absorber contains product by nonionic adsorption resin micro-
Secondary element absorption, an effect product tower tower reactor extraction return to preamble workshop section containing acid solution after depickling device depickling and continue rectifying recycling；MVR
Upgrading unit and dewatering unit extracted waste water go stripping to take off light unit stripping lightness-removing column, heat through primary steam, rise to tower top
Steam be condensed back through stripping condenser of light component removal column, fixed gas removes engine manifold, and stripping lightness-removing column tower reactor water returns to preamble work
Section is recycled；The de- weight unit of evaporation and crude product unit extraction reboiling object remove reboiling processing unit, are heated, are steamed using primary steam
Vapour is recycled to crude product receiving tank after the condensation of thick evaporation condenser.
A kind of DMAC, DMF or DMSO waste liquid as described above is dehydrated refining and reclaiming technology, and the dewatering unit is using multistage
Fair current dehydration, adverse current or advection dehydration, the dewatering unit include using Multi-stage downstream dehydration recovery process：
1) waste liquid is preheated through feed preheater, is continuously fed from falling film evaporator；
2) gas-liquid separation is carried out in gas-liquid separation chamber after falling film evaporator heats, vapour phase enters MVR concentration tower；
3) MVR concentration tower overhead vapours pressurizes through MVR heat pump group, and the MVR concentration tower overhead vapours temperature after pressurization increases
And enter falling film evaporator and heat, falling film evaporator condensate liquid is delivered to MVR concentration tower return tank, then concentrated tower reflux pump one
It is partly refluxed to MVR concentration column overhead, another part, which is produced to stripping, takes off light unit；
4) MVR is concentrated tower bottoms and is delivered to an effect dehydrating tower, and an effect dehydration column overhead steam enters two effect dehydrating towers and boils again
Device is two effect dehydrating tower heating, and two effect dehydration column reboiler condensate liquids are returned into an effect dehydrating tower return tank, then through an effect dehydrating tower
Stream pump a part is back to an effect dehydration column overhead, and another part, which is produced to stripping, takes off light unit；
5) an effect dehydrating tower tower bottoms is delivered to two effect dehydrating towers, and two effect dehydration column overhead steam enter triple effect dehydrating tower again
Device is boiled for the heating of triple effect dehydrating tower, and triple effect dehydration column reboiler condensate liquid imitates dehydrating towers into two effect dehydrating tower return tanks, then through two
Reflux pump a part is back to two effect dehydration column overheads, and another part, which is produced to stripping, takes off light unit；
6) two effect dehydrating tower tower bottoms are delivered to triple effect dehydrating tower, and triple effect dehydration column overhead steam enters forced circulation and boils again
Device is evaporator heating, and evaporator condensate liquid is delivered to triple effect dehydrating tower return tank, then through triple effect dehydrating tower reflux pump a part
It is back to triple effect dehydration column overhead, another part, which is produced to stripping, takes off light unit；
7) triple effect dehydrating tower kettle liquid turns material through transfering material pump and enters evaporator, evaporation pot liquid through forced circulation pump circulation,
It being heated through forced circulating reboiler, gas phase carries out gas-liquid separation using gas-liquid separator by wire mesh demister in evaporator,
Gas-phase transport to crude product tower, crude product tower is heated by crude product tower reboiler using external steam, and crude product column overhead steam is through tower top
Enter crude product tower return tank after condenser condensation, crude product tower return tank material is back to crude product tower through crude product tower reflux pump a part
Tower top, a part extraction to wastewater treatment；
8) crude product tower tower reactor liquid phase is delivered to product purification unit, and from charging in the middle part of two effect product towers, two effect product towers are set
Have using the steam-heated two effects product tower reboiler of an effect product column overhead, two effect product column overhead steam are through two effect product towers
After condenser condensation, into two effect product tower return tanks, a part is back to two effect product column overheads, and another part enters suction
Adnexa absorption；
9) an effect product tower is heated using primary steam, and it is two that an effect product column overhead steam, which goes two effect product tower reboilers,
The heating of product tower is imitated, condensate liquid a part is back to two effect product column overheads, and another part enters absorber absorption；
10) be delivered to the condensate liquid of absorber and the microelement contained adsorbed by nonionic adsorption resin, obtain DMAC,
DMF or DMSO content >=99.97%, 0.01 μ s/cm of water < 50PPM, conductance <, iron content≤0.05ppm, acid value≤50PPM
DMAC, DMF or DMSO product；
11) an effect product tower tower reactor continuous micro of product purification unit produces DMAC, DMF or DMSO containing acid, goes depickling
Preamble workshop section is returned after device depickling, continues rectifying recycling；
12) nitrogen-containing wastewater that MVR upgrading unit and dewatering unit obtain takes off light unit, tower after removal of ammonia and nitrogen into stripping
Kettle obtains the recycle-water without ammonia nitrogen, returns to preamble workshop section and is recycled；
13) the de- weight unit extraction reboiling of evaporation removes reboiling recovery unit scraper evaporator, in -0.08~-0.1MPa vacuum
Under degree, medium temperature heating recovery DMAC, DMF or DMSO therein.
A kind of DMAC, DMF or DMSO waste liquid as described above is dehydrated refining and reclaiming technology, the recovery process further include with
Lower step：
1) falling film evaporator only drive initial stage use, one effect dehydration column reboiler, two effect dehydration column reboilers, triple effect dehydration
Tower reboiler, forced circulating reboiler, crude product tower reboiler and scraper evaporator are heated using primary steam, by respective steam
Adjust valve regulation steam heating amount；
2) falling film evaporator is heated using primary steam, and the water vapor in MVR concentration tower tower reactor rises to form MVR concentration tower
Overhead vapours；After MVR heat pump group compresses 0.3~0.5MPa, falling film evaporator is returned again to for concentration tower heating, after driving
MVR concentration tower does not recycle primary steam；
3) an effect dehydration column reboiler is heated using primary steam, and the water vapor in an effect dehydrating tower tower reactor rises to form one
Imitate dehydration column overhead steam；
4) an effect dehydration column overhead steam is two effect dehydrating tower heating, and the water vapor in two effect dehydrating tower tower reactors rises to be formed
Two effect dehydration column overhead steam, when being equipped with the situation greater than three dehydrating towers, heating method is with step 2 or 3)；
5) the last one dehydration column overhead steam is evaporating kettle heating, and thick matter product and water vapor are through gas-liquid point in evaporating kettle
Enter crude product tower from rear.
A kind of DMAC, DMF or DMSO waste liquid as described above is dehydrated refining and reclaiming technology, generates in the recovery process
Solid impurity dangerous waste processing method is：The solution that evaporator and crude product tower continuously produce the high-boiling components containing solid enters scraper plate evaporation
Device；Into scraper evaporator solid high-boiling components solution under conditions of vacuum degree -0.08Mpa~-0.1MPa, utilize primary steam
Vapour heating, steams product coarse matter, enters crude product receiving tank after the condensation of thick evaporation condenser, returns to preamble workshop section and continues to recycle.
The utility model to low concentration waste liquid carry out solvent recovery, can remove containing acid and trace metal ion, significantly
Product index is improved, national standard, DMAC >=99.98%, acid≤10PPM, water≤50PPM, conductance≤0.01 are higher than.Dehydration is single
The ammonia-containing water that member obtains can go stripping to take off light unit removing ammonia, then return to preamble workshop section and continue to use.The de- weight unit of evaporation
Enter reboiling processing unit scraper evaporator with crude product unit extraction reboiling solution, the low temperature (< in high vacuum (- 0.099MPa)
100 DEG C) under evaporation recycling DMAC, DMF or DMSO, improve comprehensive yield.The utility model is used for containing objects such as metallic element, acid
DMAC, DMF or DMSO of matter or similar waste liquid are handled, and can be carried out solvent to DMAC, DMF or DMSO or similar waste liquid and be returned
Receive, while the trace metal ion contained in regenerant and acid can be removed etc., it is widely used in polyimides production industry, virtue
It is pure to improve devil liquor recovery object for synthetic fibre industry, PU Fiber Industry, carbon fiber industry, glove industry, the industries such as environmental protection and regenerated resources
Degree, while pollution of the waste liquid to environment is reduced, energy consumption is reduced, the use of a water is reduced.
Detailed description of the invention
Fig. 1 is DMAC, DMF or DMSO waste liquid dehydration purification recovery system schematic diagram.
Specific embodiment
To keep the above objects, features, and advantages of the utility model more obvious and easy to understand, with reference to the accompanying drawing to this
The specific embodiment of utility model is described in detail.Many details are explained in the following description in order to abundant
Understand the utility model.But the utility model can be implemented with being much different from other way described herein, this field
Technical staff can do similar improvement without prejudice to the utility model connotation, therefore the utility model is not by following public affairs
The limitation for the specific embodiment opened.
Unless otherwise defined, all technical and scientific terms used herein are led with the technology for belonging to the utility model
The normally understood meaning of the technical staff in domain is identical.Terminology used in the description of the utility model herein only be
The purpose of description specific embodiment, it is not intended that in limitation the utility model.
Referring to Fig. 1, the utility model also provides a kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system, and described time
Receipts system includes that MVR upgrading unit, dewatering unit, the de- weight unit of evaporation, crude product unit, product purification unit, stripping are de- light single
Member and reboiling processing unit；
The MVR upgrading unit is equipped with feed preheater 2, falling film evaporator 3, gas-liquid separation chamber 4, MVR concentration tower 5, MVR
Heat pump group 6 and MVR concentration tower return tank 7, the feed preheater 2 connect falling film evaporator 3；3 lower end of falling film evaporator
It is connected with gas-liquid separation chamber 4, vapour phase enters MVR concentration tower 5；The MVR heat pump group 6 is connected to the MVR concentration tower 5 and falling liquid film
Between evaporator 3, the MVR concentration tower 5 is used to carrying out the low concentration waste liquid of MVR upgrading unit into concentration raising, and concentration improves
Low concentration waste liquid afterwards is delivered to dewatering unit and is dehydrated；The MVR concentration tower return tank 7 connects the falling film evaporator 3；
The dewatering unit includes several sequentially connected dehydrating towers, and the lower part of each dehydrating tower is connected with dehydrating tower and boils again
The steam of device, dehydration column overhead is connected to form multiple-effect coupling as the heat source of next effect dehydrating tower with next effect dehydration column reboiler
It closes；
The de- weight unit of evaporation includes forced circulating reboiler 18, forced circulation pump 19, evaporator 20 and gas-liquid separation
Device 21, the forced circulating reboiler 18 connect last effect dehydrating tower of the dewatering unit, and forced circulating reboiler 18 passes through
Forced circulation pump 19 connects the evaporator 20；20 top of evaporator connects the crude product list through the gas-liquid separator 21
The crude product tower 23 of member；
The crude product unit is equipped with crude product tower 23, crude product tower reboiler 22, crude product tower return tank 25 and crude product tower condenser
24,23 lower part of crude product tower connects the crude product tower reboiler 22, and 23 top of crude product tower connects through crude product tower condenser 24
Connect the crude product tower return tank 25；The crude product tower return tank 25, which returns, is connected to the crude product tower 23；
The product purification unit includes that an effect product tower 34, one imitates the effect product tower return tank of product tower reboiler 33, one
35, two effect product towers 30, two imitate product tower reboiler 29, two and imitate the effect of product tower condenser 31, two product tower return tank 32, absorption
Device 36 and depickling device 37, the effect product tower 34 connect the two effects product tower 30, and one imitates described in the connection of 34 lower part of product tower
One effect product tower reboiler 33；The one effect product tower return tank 35 is connected to an effect product tower 34 and two effect product towers again
It boils between device 29, an effect product tower return tank 35 is also connected to the absorber 36；The two effects product tower 30 connects described thick
23 tower reactor gas-phase space of product tower；Two effects product tower 30 connection, the two effect product tower reboiler 29, two effect 30 tower tops of product tower connect
The two effects product tower condenser 31 is connect, the two effects product tower condenser 31 connects the two effects product tower return tank 32；Institute
It states absorber 36 and connects the two effects product tower 30, absorber 36 is micro for being contained by nonionic adsorption resin to condensate liquid
Element absorption；The depickling device 37 is connected to 34 lower part of an effect product tower, for removing the acid in Produced Liquid；
It includes stripping lightness-removing column reboiler 40, stripping lightness-removing column 17 and stripping condenser of light component removal column that the stripping, which takes off light unit,
1, the stripping lightness-removing column reboiler 40 is placed in 17 lower part of stripping lightness-removing column and heats for stripping lightness-removing column 17, and the stripping is de-
Light tower condenser 1 is placed in stripping 17 top of lightness-removing column for condensed steam and conveying fixed gas；
The reboiling processing unit includes scraper evaporator 26, thick evaporation condenser 27 and crude product receiving tank 28, the scraper plate
Evaporator 26 is connected with thick evaporation condenser 27, and the thick evaporation condenser 27 is connected to crude product receiving tank 28.
In one embodiment of DMAC, DMF or DMSO waste liquid dehydration purification recovery system, the dewatering unit is equipped with an effect
Dehydrating tower 9, two imitates dehydrating tower 12 and triple effect dehydrating tower 15, and effect 9 overhead vapours of dehydrating tower enters two effect dehydration column reboilers 11
It is heated for two effect dehydrating towers 12, two effect 11 condensate liquids of dehydration column reboiler enter an effect dehydrating tower return tank 10, then de- through an effect
Water tower reflux pump a part is back to 9 tower top of an effect dehydrating tower；One effect 9 kettle liquid of dehydrating tower is delivered to two effect dehydrating towers 12, two effects
12 overhead vapours of dehydrating tower enters triple effect dehydration column reboiler 14 for the heating of triple effect dehydrating tower 15, and 15 condensate liquid of triple effect dehydrating tower is defeated
It send to two effect dehydrating tower return tanks 13, then is back to two effect dehydrating towers, 12 tower top through two effect dehydrating tower reflux pump a part；Triple effect
15 overhead vapours of dehydrating tower enters forced circulating reboiler 18 for the heating of evaporator 20, and it is de- that 20 condensate liquid of evaporator is delivered to triple effect
Water tower return tank 16, then 15 tower top of triple effect dehydrating tower, another part extraction are back to through triple effect dehydrating tower reflux pump a part
Light unit is taken off to stripping.
In one embodiment of DMAC, DMF or DMSO waste liquid dehydration purification recovery system, the continuously extraction of evaporator 20
The solution of the high-boiling components containing solid enters scraper evaporator 26；Into scraper evaporator 26 solid high-boiling components solution in vacuum degree-
It under conditions of 0.08Mpa~-0.1MPa, is heated using primary steam, steams thick matter product and water, condensed through thick evaporation condenser 27
Enter crude product receiving tank 28 afterwards, returns to preamble workshop section and continue to recycle.
In one embodiment of DMAC, DMF or DMSO waste liquid dehydration purification recovery system, the falling film evaporator 3 is only opened
Vehicle initial stage uses, and an effect dehydration column reboiler 8, two imitates dehydration column reboiler 11, triple effect dehydration column reboiler 14, forced circulation again
It boils device 18, crude product tower reboiler 22 and scraper evaporator 26 to heat using primary steam, is adjusted and steamed by respective steam control valve
Vapour heating amount.
In one embodiment of DMAC, DMF or DMSO waste liquid dehydration purification recovery system, the MVR upgrading unit and de-
Water unit removed overhead waste water takes off light cell processing through stripping and removes ammonia nitrogen waste therein, and water, which is further continued for return preamble workshop section, to be made
With.
Recovery process using the utility model includes MVR upgrading unit, dewatering unit, the de- weight unit, crude product list of evaporation
Member, product purification unit, stripping take off light unit and reboiling processing unit, and the MVR upgrading unit is equipped with feed preheater 2, drop
Film evaporator 3, gas-liquid separation chamber 4, MVR concentration tower 5, MVR heat pump group 6 and MVR concentration tower return tank 7, waste liquid is through feeding preheating
Device 2 preheats, and continuously feeds from falling film evaporator 3；Gas-liquid separation, vapour are carried out in gas-liquid separation chamber 4 after the heating of falling film evaporator 3
Mutually enter MVR concentration tower 5；The waste liquid steam that the MVR heat pump group 6 generates the MVR concentration tower 5 carries out pressurization heating conduct
The heat source of the falling film evaporator 3 uses, and the low concentration waste liquid that will be delivered to MVR upgrading unit carries out concentration raising, and concentration mentions
Low concentration waste liquid after height is delivered to dewatering unit and is dehydrated；The dewatering unit is equipped with several sequentially connected dehydrating towers,
Several sequentially connected dehydrating towers use multiple-effect fair current coupling, adverse current or advection mode；The first dehydrating tower of dewatering unit passes through defeated
It is sent to the primary steam heat temperature raising of reboiler, rises to the steam of dehydration column overhead as the heat source of next effect dehydrating tower under
One effect dehydration column reboiler is connected to form multiple-effect coupling, and multiple-effect is dehydrated last effect dehydrating tower kettle liquid and turns material conveying by transfering material pump
To the de- weight unit of evaporation, evaporates de- weight unit and heated by the circulation of forced circulation pump 19 and forced circulating reboiler 18, gas-liquid is mixed
It closes and mutually carries out gas-liquid separation by evaporator 20 and gas-liquid separator 21, vapour phase is delivered to crude product tower 23；23 tower top of crude product tower steams
Vapour is back to crude product tower 23, a part extraction through overhead condenser condensation rear portion；The extraction of 23 kettle liquid of crude product unit crude product tower
To product purification unit, effect 34 tower top of product tower of product purification unit obtains product and is transported to absorber 36, absorber 36
The microelement that product contains is adsorbed by nonionic adsorption resin, effect 34 tower reactor of a product tower extraction is containing acid solution through depickling device 37
Preamble workshop section is returned after depickling continues rectifying recycling；MVR upgrading unit and dewatering unit extracted waste water go stripping to take off light unit vapour
Lightness-removing column 17 is mentioned, is heated through primary steam, the steam for rising to tower top is condensed back through stripping condenser of light component removal column 1, fixed gas
Engine manifold is removed, stripping 17 tower reactor water of lightness-removing column returns to preamble workshop section and is recycled；The de- weight unit of evaporation and the extraction of crude product unit
Reboiling object removes reboiling processing unit, is heated using primary steam, and steam is recycled to crude product after the condensation of thick evaporation condenser 27 and receives
Tank 28.
DMAC, DMF or DMSO waste liquid are dehydrated in one embodiment of refining and reclaiming technology, and the dewatering unit is using multistage
Fair current dehydration, adverse current or advection dehydration, the dewatering unit include using Multi-stage downstream dehydration recovery process：
1) waste liquid is preheated through feed preheater 2, is continuously fed from falling film evaporator 3；
2) gas-liquid separation is carried out in gas-liquid separation chamber 4 after the heating of falling film evaporator 3, vapour phase enters MVR concentration tower 5；
3) 5 overhead vapours of MVR concentration tower pressurizes through MVR heat pump group 6, the 5 overhead vapours temperature liter of MVR concentration tower after pressurization
Height simultaneously enters the heating of falling film evaporator 3, and 3 condensate liquid of falling film evaporator is delivered to MVR concentration tower return tank 7, then concentrated tower returns
Stream pump a part is back to 5 tower top of MVR concentration tower, and another part, which is produced to stripping, takes off light unit；
4) 5 kettle liquid of MVR concentration tower is delivered to an effect dehydrating tower 9, and effect 9 overhead vapours of dehydrating tower enters two effect dehydrating towers again
Boiling device 11 is that two effect dehydrating towers 12 heat, and two imitate 11 condensate liquids of dehydration column reboiler into an effect dehydrating tower return tank 10, then through one
Effect dehydrating tower reflux pump a part is back to 9 tower top of an effect dehydrating tower, and another part, which is produced to stripping, takes off light unit；
5) effect 9 tower bottoms of dehydrating tower is delivered to two effect dehydrating towers 12, and it is de- that two effect 12 overhead vapours of dehydrating tower enter triple effect
Water tower reboiler 14 is the heating of triple effect dehydrating tower 15, and 14 condensate liquid of triple effect dehydration column reboiler imitates dehydrating tower return tanks 13 into two,
It is back to two effect dehydrating towers, 12 tower top through two effect dehydrating tower reflux pump a part again, another part produces de- light single to stripping
Member；
6) two effect 12 tower bottoms of dehydrating tower are delivered to triple effect dehydrating tower 15, and 15 overhead vapours of triple effect dehydrating tower enters pressure and follows
Ring reboiler 18 is the heating of evaporator 20, and 20 condensate liquid of evaporator is delivered to triple effect dehydrating tower return tank 16, then is dehydrated through triple effect
Tower reflux pump a part is back to 15 tower top of triple effect dehydrating tower, and another part, which is produced to stripping, takes off light unit；
7) 15 kettle liquid of triple effect dehydrating tower turns to expect to enter evaporator 20 through transfering material pump, and liquid is through forced circulation pump in evaporator 20
19 circulations, are heated through forced circulating reboiler 18, and gas phase is by wire mesh demister in evaporator 20 using gas-liquid separator 21
Gas-liquid separation, gas-phase transport to crude product tower 23 are carried out, crude product tower 23 is heated by crude product tower reboiler 22 using external steam, slightly
23 overhead vapours of product tower enters crude product tower return tank 25 after overhead condenser condenses, and 25 material of crude product tower return tank is through crude product tower
23 reflux pump a part are back to 23 tower top of crude product tower, a part extraction to wastewater treatment；
8) 23 tower reactor liquid phase of crude product tower is delivered to product purification unit, feeds in the middle part of two effect product towers 30, two effect products
Tower 30, which is equipped with, utilizes the steam-heated two effects product tower reboiler 29 of an effect product column overhead, two effect 30 overhead vapours of product tower warps
After two effect product tower condensers 31 condense, into two effect product tower return tanks 32, a part is back to two effect product towers, 30 tower top,
Another part enters the absorption of absorber 36；
9) an effect product tower is heated using primary steam, and one, which imitates product column overhead steam, goes the two effect product tower reboilers 29 to be
Two effect product towers 30 heat, and condensate liquid a part is back to two effect product towers, 30 tower top, and another part enters the suction of absorber 36
It is attached；
10) condensate liquid for being delivered to absorber 36 adsorbs the microelement contained by nonionic adsorption resin, obtains
DMAC, DMF or DMSO content >=99.97%, 0.01 μ s/cm of water < 50PPM, conductance <, iron content≤0.05ppm, acid value≤
DMAC, DMF or DMSO product of 50PPM；
11) an effect 34 tower reactor continuous micro of product tower of product purification unit produces DMAC, DMF or DMSO containing acid, goes to take off
Preamble workshop section is returned after sour device depickling, continues rectifying recycling；
12) nitrogen-containing wastewater that MVR upgrading unit and dewatering unit obtain takes off light unit, tower after removal of ammonia and nitrogen into stripping
Kettle obtains the recycle-water without ammonia nitrogen, returns to preamble workshop section and is recycled；
13) it evaporates de- weight unit extraction reboiling and removes reboiling recovery unit scraper evaporator 26, it is true in -0.08~-0.1MPa
Under reciprocal of duty cycle, medium temperature heating recovery DMAC, DMF or DMSO therein.
DMAC, DMF or DMSO waste liquid be dehydrated refining and reclaiming technology one embodiment in, the recovery process further include with
Lower step：
1) 3 driving initial stages of falling film evaporator use, and an effect dehydration column reboiler 8, two imitates dehydration column reboiler 11, triple effect
Dehydration column reboiler 14, forced circulating reboiler 18, crude product tower reboiler 22 and scraper evaporator 26 are heated using primary steam,
Steam heating amount is adjusted by respective steam control valve；
2) falling film evaporator 3 is heated using primary steam, and the water vapor in 5 tower reactor of MVR concentration tower rises to form MVR concentration
5 overhead vapours of tower；After MVR heat pump group 6 compresses 0.3~0.5MPa, falling film evaporator 3 is returned again to as concentration tower heating, is driven
MVR concentration tower 5 does not recycle primary steam later；
3) an effect dehydration column reboiler 8 is heated using primary steam, and the water vapor in effect 9 tower reactor of dehydrating tower rises to be formed
One effect 9 overhead vapours of dehydrating tower；
4) effect 9 overhead vapours of dehydrating tower is that two effect dehydrating towers 12 heat, in the water vapor in two effect 12 tower reactors of dehydrating tower
It rises and forms two effect 12 overhead vapours of dehydrating tower, when being equipped with the situation greater than three dehydrating towers, heating method is with step 2 or 3)；
5) the last one dehydration column overhead steam is evaporating kettle heating, and thick matter product and water vapor are through gas-liquid point in evaporating kettle
Enter crude product tower 23 from rear.
DMAC, DMF or DMSO waste liquid are dehydrated in one embodiment of refining and reclaiming technology, are generated in the recovery process
Solid impurity dangerous waste processing method is：The solution that evaporator 20 and crude product tower 23 continuously produce the high-boiling components containing solid enters scraper plate steaming
Send out device 26；Into scraper evaporator 26 solid high-boiling components solution under conditions of vacuum degree -0.08Mpa~-0.1MPa, utilize
Primary steam heating, steam product coarse matter, through thick evaporation condenser 27 condensation after enter crude product receiving tank 28, return preamble workshop section after
Continuous recycling.
By the utility model technique and using process flow shown in attached drawing 1, feed as 20000Kg/h, feed composition：Water
95%, DMAC4.9%, impurity 0.1%.Raw material is preheated to 80~85 DEG C through feed preheater, feeds from falling film evaporator, control
MVR be concentrated pressure tower be normal pressure, 100 DEG C of tower top temperature, 102 DEG C of bottom temperature, overhead extraction 11t/h, reflux ratio 0.1~1, tower
Top steam is compressed to 0.1~0.4MPa by MVR heat pump group, returns to falling film evaporator heating, and MVR concentration tower unit kettle liquid is from one
Charging in the middle part of dehydrating tower is imitated, an effect dehydrating tower controls 0.05-0.1MPa, and 112-120 DEG C of tower top, 114-122 DEG C of tower reactor, tower top is adopted
2t/h out, reflux ratio 0.1-1, an effect dehydration column overhead steam enter two effect dehydration column reboiler heating, two effect dehydrating tower of control
Interior pressure 0-0.05MPa, 100-112 DEG C of tower top, 102-114 DEG C of tower reactor, overhead extraction 2t/h, reflux ratio 0.1-1, two effect dehydrations
Column overhead steam enters the heating of triple effect dehydration column reboiler, triple effect dehydrating tower control -0.06MPa, and 86 DEG C of tower top temperature, tower reactor temperature
88 DEG C, reflux ratio 0.1-1, overhead extraction amount 2t/h of degree, triple effect dehydration column overhead steam, which enters, forces reboiler heating, and control is steamed
Send out pressure inside the tank 8KPa, 60-70 DEG C of temperature, reboiling object removes reboiling processing unit from bottom extraction, gas phase through gas-liquid separator it
Afterwards enter crude product tower, crude product tower reboiler using primary steam heat, control product pressure tower 8KPa, 42 DEG C of tower top temperature, tower
85 DEG C of kettle temperature degree, reflux ratio 0.3-1.5, overhead extraction 2t/h, tower reactor kettle liquid enters product purification unit, two effect product pressure towers
Control 5KPa, 60 DEG C of tower top temperature, 80-85 DEG C of bottom temperature, reflux ratio 0.2-1.5, overhead extraction 450Kg/h；One effect product
Pressure tower control 8KPa, 87 DEG C of tower top temperature, 90 DEG C of bottom temperature, reflux ratio 0.2-1.5, overhead extraction 540Kg/h；Tower top is adopted
990Kg/hDMAC out goes absorber to adsorb micro ferro element etc. and obtains product DMAC >=99.97%, water≤50PPM, and acid≤
0.01 μ s/cm of 10PPM, conductance <.One effect product tower bottoms extraction 50Kg/h returns to preamble workshop section through depickling device depickling.MVR is dense
Contracting unit, dehydrating tower unit tower top waste water go stripping to take off light unit and remove ammonia nitrogen therein, return to preamble workshop section and are recycled.
By the utility model technique and using process flow shown in attached drawing 1, feed as 20000Kg/h, feed composition：Water
90%, DMSO9.9%, impurity 0.1%.Raw material is preheated to 80~85 DEG C through feed preheater, feeds from falling film evaporator, control
MVR be concentrated pressure tower be normal pressure, 100 DEG C of tower top temperature, 102 DEG C of bottom temperature, overhead extraction 10t/h, reflux ratio 0.1~1, tower
Top steam is compressed to 0.1~0.4MPa by MVR heat pump group, returns to falling film evaporator heating, and MVR concentration tower unit kettle liquid is from one
Charging in the middle part of dehydrating tower is imitated, an effect dehydrating tower controls 0.05-0.1MPa, and 112-120 DEG C of tower top, 112-122 DEG C of tower reactor, tower top is adopted
2t/h out, reflux ratio 0.1-1, an effect dehydration column overhead steam enter two effect dehydration column reboiler heating, two effect dehydrating tower of control
Interior pressure 0-0.05MPa, 100-112 DEG C of tower top, 102-114 DEG C of tower reactor, overhead extraction 2t/h, reflux ratio 0.1-1, two effect dehydrations
Column overhead steam enters the heating of triple effect dehydration column reboiler, triple effect dehydrating tower control -0.06MPa, and 86 DEG C of tower top temperature, tower reactor temperature
88 DEG C, reflux ratio 0.1-1, overhead extraction amount 2t/h of degree, triple effect dehydration column overhead steam, which enters, forces reboiler heating, and control is steamed
Send out pressure inside the tank 8KPa, 60-70 DEG C of temperature, reboiling object removes reboiling processing unit from bottom extraction, gas phase through gas-liquid separator it
Enter crude product tower afterwards, crude product tower reboiler is heated using primary steam, one effect product pressure tower 8KPa of control, tower top temperature 42
DEG C, 85 DEG C of bottom temperature, reflux ratio 0.5-2, overhead extraction 2t/h, tower reactor kettle liquid enters product purification unit, two effect product towers
Pressure control 1KPa, 66 DEG C of tower top temperature, 82-86 DEG C of bottom temperature, reflux ratio 0.2-1.5, overhead extraction 950Kg/h；One effect
Product pressure tower control 3KPa, 89 DEG C of tower top temperature, 98 DEG C of bottom temperature, reflux ratio 0.2-1.5, overhead extraction 970Kg/h；Tower
The 1920Kg/hDMSO of top extraction goes absorber to adsorb micro ferro element etc. and obtains product DMSO >=99.97%, water≤50PPM,
Acid≤10PPM, 0.01 μ s/cm of conductance <.One effect product tower bottoms extraction 50Kg/h returns to preamble workshop section through depickling device depickling.
MVR upgrading unit, dehydrating tower unit tower top waste water go stripping to take off light unit and remove ammonia nitrogen therein, and returning to preamble workshop section circulation makes
With.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
Above-described embodiments merely represent several embodiments of the utility model, the description thereof is more specific and detailed,
But it cannot be understood as the limitations to utility model patent range.It should be pointed out that for the common skill of this field
For art personnel, without departing from the concept of the premise utility, various modifications and improvements can be made, these are belonged to
The protection scope of the utility model.Therefore, the scope of protection shall be subject to the appended claims for the utility model patent.
Claims (5)
1. a kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system, which is characterized in that the recovery system includes MVR dense
Contracting unit, dewatering unit, the de- weight unit of evaporation, crude product unit, product purification unit, stripping take off light unit and reboiling processing is single
Member；
The MVR upgrading unit be equipped with feed preheater, falling film evaporator, gas-liquid separation chamber, MVR concentration tower, MVR heat pump group and
MVR concentration tower return tank, the feed preheater connect falling film evaporator；The falling film evaporator lower end is connected with gas-liquid separation
Room, vapour phase enter MVR concentration tower；The MVR heat pump group is connected between the MVR concentration tower and falling film evaporator, the MVR
Concentration tower is used to carrying out the low concentration waste liquid of MVR upgrading unit into concentration raising, and the low concentration waste liquid after concentration improves is delivered to
Dewatering unit is dehydrated；The MVR concentration tower return tank connects the falling film evaporator；
The dewatering unit includes several sequentially connected dehydrating towers, and the lower part of each dehydrating tower is connected with dehydration column reboiler,
The steam of dehydration column overhead, which is connected to as the heat source of next effect dehydrating tower with next effect dehydration column reboiler, to be formed multiple-effect and couples；
The de- weight unit of evaporation includes forced circulating reboiler, forced circulation pump, evaporator and gas-liquid separator, the pressure
It recycles reboiler and connects last effect dehydrating tower of the dewatering unit, forced circulating reboiler passes through described in forced circulation pump connection
Evaporator；The evaporator top connects the crude product tower of the crude product unit through the gas-liquid separator；
The crude product unit is equipped with crude product tower, crude product tower reboiler, crude product tower return tank and crude product tower condenser, the crude product tower
Lower part connects the crude product tower reboiler, and crude product tower top connects the crude product tower return tank through crude product tower condenser；Institute
It states crude product tower return tank time and is connected to the crude product tower；
The product purification unit includes an effect product tower, an effect product tower reboiler, an effect product tower return tank, two effect products
Tower, two effect product tower reboilers, two effect product tower condensers, two effect product tower return tanks, absorber and depickling device, an effect
The product tower connection two effects product tower, an effect product tower lower part connection one effect product tower reboiler；The one effect product
Tower return tank is connected between an effect product tower and two effect product tower reboilers, and an effect product tower return tank is also connected to institute
State absorber；The two effects product tower connects the crude product tower tower reactor gas-phase space；Two effects product tower connection, the two effect product
Tower reboiler, the two effect product column overhead connection two effects product tower condensers, described two imitate described in the connection of product tower condenser
Two effect product tower return tanks；The absorber connection two effects product tower, absorber are used for through nonionic adsorption resin to cold
The microelement absorption that lime set contains；The depickling device is connected to an effect product tower lower part, for removing the acid in Produced Liquid；
It includes stripping lightness-removing column reboiler, stripping lightness-removing column and stripping condenser of light component removal column, the vapour that the stripping, which takes off light unit,
It mentions lightness-removing column reboiler and is placed in the stripping lightness-removing column lower part as stripping lightness-removing column heating, the stripping condenser of light component removal column is placed in
Lightness-removing column top is stripped for condensed steam and conveying fixed gas；
The reboiling processing unit includes scraper evaporator, thick evaporation condenser and crude product receiving tank, the scraper evaporator and thick
Evaporation condenser is connected, and the thick evaporation condenser is connected to crude product receiving tank.
2. a kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system according to claim 1, which is characterized in that institute
Dewatering unit is stated equipped with an effect dehydrating tower, two effect dehydrating towers and triple effect dehydrating tower, it is de- that an effect dehydration column overhead steam enters two effects
Water tower reboiler is two effect dehydrating tower heating, and two effect dehydration column reboiler condensate liquids enter an effect dehydrating tower return tank, then through one
Effect dehydrating tower reflux pump a part is back to an effect dehydration column overhead；One effect dehydrating tower kettle liquid is delivered to two effect dehydrating towers, two effects
Dehydration column overhead steam enters triple effect dehydration column reboiler for the heating of triple effect dehydrating tower, and triple effect dehydrating tower condensate liquid is delivered to two effects
Dehydrating tower return tank, then two effect dehydration column overheads are back to through two effect dehydrating tower reflux pump a part；Triple effect dehydration column overhead is steamed
Vapour enters forced circulating reboiler for evaporator heating, and evaporator condensate liquid is delivered to triple effect dehydrating tower return tank, then through triple effect
Dehydrating tower reflux pump a part is back to triple effect dehydration column overhead, and another part, which is produced to stripping, takes off light unit.
3. a kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system according to claim 1, which is characterized in that institute
It states evaporator and continuously produces the solution of the high-boiling components containing solid and enter scraper evaporator；Solid high-boiling components into scraper evaporator are molten
Liquid is heated under conditions of vacuum degree -0.08Mpa~-0.1MPa using primary steam, is steamed thick matter product and water, is slightly steamed
Enter crude product receiving tank after condenser condensation, returns to preamble workshop section and continue to recycle.
4. a kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system according to claim 1, which is characterized in that institute
It states falling film evaporator only to drive initial stage use, an effect dehydration column reboiler, two effect dehydration column reboilers, triple effect dehydrating towers boil again
Device, forced circulating reboiler, crude product tower reboiler and scraper evaporator are heated using primary steam, by respective steam control valve
Adjust steam heating amount.
5. a kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system according to claim 1, which is characterized in that institute
It states MVR upgrading unit and dewatering unit removed overhead waste water and takes off light cell processing removing ammonia nitrogen waste therein through stripping, water is again
Continue to return to the use of preamble workshop section.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820456311.2U CN208166891U (en) | 2018-04-03 | 2018-04-03 | A kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820456311.2U CN208166891U (en) | 2018-04-03 | 2018-04-03 | A kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN208166891U true CN208166891U (en) | 2018-11-30 |
Family
ID=64371472
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201820456311.2U Withdrawn - After Issue CN208166891U (en) | 2018-04-03 | 2018-04-03 | A kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN208166891U (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110127789A (en) * | 2019-05-08 | 2019-08-16 | 河北德瑞化工有限公司 | A kind of waste water treatment system and its wastewater treatment method |
| CN110452125A (en) * | 2019-09-03 | 2019-11-15 | 天津科技大学 | A kind of toluenediamine dewatering and device based on mechanical steam recompression MVR |
| CN112142618A (en) * | 2019-06-28 | 2020-12-29 | 中国石油化工股份有限公司 | Low-concentration dimethyl formamide wastewater recovery system and method |
| CN113426151A (en) * | 2021-07-26 | 2021-09-24 | 常州乐研分离技术有限公司 | Device and method for solvent DMSO rectification recovery process in carbon fiber production process |
| CN114516816A (en) * | 2022-02-24 | 2022-05-20 | 深圳瑞华泰薄膜科技股份有限公司 | Method and device for recovering DMAC (dimethyl acetamide) and isoquinoline from solution |
-
2018
- 2018-04-03 CN CN201820456311.2U patent/CN208166891U/en not_active Withdrawn - After Issue
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110127789A (en) * | 2019-05-08 | 2019-08-16 | 河北德瑞化工有限公司 | A kind of waste water treatment system and its wastewater treatment method |
| CN112142618A (en) * | 2019-06-28 | 2020-12-29 | 中国石油化工股份有限公司 | Low-concentration dimethyl formamide wastewater recovery system and method |
| CN112142618B (en) * | 2019-06-28 | 2023-07-21 | 中国石油化工股份有限公司 | Low-concentration dimethylformamide wastewater recovery system and method |
| CN110452125A (en) * | 2019-09-03 | 2019-11-15 | 天津科技大学 | A kind of toluenediamine dewatering and device based on mechanical steam recompression MVR |
| CN113426151A (en) * | 2021-07-26 | 2021-09-24 | 常州乐研分离技术有限公司 | Device and method for solvent DMSO rectification recovery process in carbon fiber production process |
| CN114516816A (en) * | 2022-02-24 | 2022-05-20 | 深圳瑞华泰薄膜科技股份有限公司 | Method and device for recovering DMAC (dimethyl acetamide) and isoquinoline from solution |
| CN114516816B (en) * | 2022-02-24 | 2023-12-01 | 深圳瑞华泰薄膜科技股份有限公司 | Method and device for recycling DMAC and isoquinoline from solution |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN208166891U (en) | A kind of DMAC, DMF or DMSO waste liquid dehydration purification recovery system | |
| CN108276302A (en) | A kind of DMAC, DMF or DMSO waste liquid dehydration refining and reclaiming technology and system | |
| CN105418368B (en) | A kind of technique and device for producing high straight alcohol | |
| CN210085330U (en) | Separation device for recovering dimethyl sulfoxide | |
| CN101429288A (en) | Method for treating process liquid generated in production process of polyphenylene sulfide | |
| CN106045872B (en) | The pervaporation method recovery system and method for a kind of Dimethylformamide Residue | |
| CN109369444A (en) | Dimethylformamide is from backheat distillation system and recovery method | |
| CN110938047A (en) | Tetrahydrofuran-benzene-water mixture separation process and device | |
| CN108658051B (en) | Method and device for recovering nitration waste acid and sulfuric acid recovered by method and device | |
| CN110862330B (en) | Efficient energy-saving rectification process for recycling DMAC waste liquid | |
| CN102695675A (en) | Method for the separation of ammonia and carbon dioxide from aqueous solutions | |
| CN107311878A (en) | A kind of device for reclaiming glycine waste liquid and the method for reclaiming glycine waste liquid | |
| CN106978203A (en) | A kind of coal tar takes off slag and fraction seperation technique and device | |
| CN206304382U (en) | A kind of solvent DMAC vacuum recovering apparatus of aramid fiber production | |
| CN116947728A (en) | Novel method and device for energy-saving recovery of NMP (N-methyl pyrrolidone) by single tower | |
| CN209759339U (en) | Recovery unit of dichloromethane in cefuroxime acid production | |
| CN107098826A (en) | The ten towers six effect distillation system and recovery method of a kind of DMAC or DMF waste liquids | |
| CN108358754B (en) | Process method and system for separating ethanol, ethyl acetate and water mixture | |
| CN104478734B (en) | The method that in AKD production, crude product triethylamine recycles | |
| CN206646067U (en) | A kind of coal tar takes off slag and fraction seperation device | |
| CN104844420A (en) | Continuous treatment process and device of neopentyl glycol condensed washing mother liquor | |
| CN106966867B (en) | Energy-saving process for separating methanol, ethanol and benzene by three-tower heat integration pressure swing distillation | |
| CN215462094U (en) | Device for DMF (dimethyl formamide) concentration process | |
| CN107473932A (en) | A kind of separation method of butanol and butyl acetate | |
| CN112694409B (en) | Method and device for recycling triethylamine in wastewater |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned | ||
| AV01 | Patent right actively abandoned | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20181130 Effective date of abandoning: 20240119 |
|
| AV01 | Patent right actively abandoned |
Granted publication date: 20181130 Effective date of abandoning: 20240119 |