CN208414290U - A kind of dewatering system of novel propylene glycol methyl ether acetate production - Google Patents
A kind of dewatering system of novel propylene glycol methyl ether acetate production Download PDFInfo
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Abstract
The utility model provides a kind of dewatering system of novel propylene glycol methyl ether acetate production, it include: tower reactor reboiler, the tower reactor reboiler gas phase mouth is connect with the lateral gas phase mouth of atmospheric distillation tower by pipeline A, tower reactor reboiler liquid phase mouth is connect with atmospheric distillation tower tower bottom liquid phase mouth by pipeline B, and atmospheric distillation tower top gaseous phase mouth is connect with the import of overhead condenser gas phase by pipeline D；Atmospheric distillation tower tower bottom liquid-phase outlet is connect with tower reactor extraction pump inlet by pipeline C；Overhead condenser condensate liquid extraction mouth is connect with phase separation tank feed inlet by pipeline E；Phase separation tank side take-off mouth is connect with return tank feed inlet by pipeline F；Phase separation tank discharge port is connect with reflux pump inlet by pipeline G；Reflux pump outlet conduit is connect with rectifier column reflux mouth by pipeline H；Phase separation tank tank bottom extraction mouth is produced waste water by pipeline K.The utility model has adapted to environmental requirement, and master operation does not increase the consumption of energy: postprocessing working procedures reduce the consumption of energy.
Description
Technical field
The utility model relates to technical field of fine chemical production, specially a kind of novel propylene glycol methyl ether acetate
The dewatering system of production.
Background technique
With the rapid development of global economy, while chemical industry is created the wealth to the mankind, also depend on for existence to the mankind
Environment cause many negative effects, especially lack of energy and environmental degradation these two aspects.China is also continuous appealing enterprise
Industry reform and transition, country also require a part to have while the mandatory enterprise for shutting down a part of high energy consumption and high pollution
The enterprise independent innovation for the value that makes the transition is encouraged to replace high energy consumption technique using new energy or energy saving technique, be encouraged using environmental protection
Type technology generations replace contamination type technique.
Propylene glycol methyl ether acetate is the less toxic advanced industrial solvent of function admirable, is had to polarity and nonpolar substance
Very strong solvability, suitable for high-grade paint, the solvent of the various polymer of ink, including it is amino methyl acid esters, vinyl, poly-
Ester, cellulose ethanoate, alkyd resin, acrylic resin, epoxy resin and nitrocellulose etc..Wherein.Propylene glycol monomethyl ether third
Acid esters is coating, solvent best in ink, is suitable for unsaturated polyester (UP), polyurethane based resin, acrylic resin, epoxy resin
Deng.
Propylene glycol methyl ether acetate itself is the requirement for adapting to international environmental law, substitution as environment-friendly type organic solvent
Application of the organic solvent glycol ether acetate being more toxic with similar solubility property in high-grade paint, so production
Should more require environmental protection in technique, and we it is conventionally produced during will use a kind of benzene being more toxic as dehydrated
Entrainer in journey, and this entrainer can consume a large amount of energy during subsequent recovery, and especially discharge contains benzene
The tail gas of steam is difficult that the modes such as absorption or biochemistry is taken to handle, and environmental law is to the tail gas content discharge index requirement containing benzene
It is more strict more than discharge index of the low poison solvent in tail gas.It is therefore necessary to select a kind of azeotropic dehydration substance, Ji Neng
Close or better than benzene azeotropic dehydration function in performance, and energy consumption can be reduced during recovery processing, and in tail
Gas discharge aspect meets environmental requirement.
Utility model content
The technical issues of the utility model is solved is to provide a kind of taking off for novel propylene glycol methyl ether acetate production
Water system, to solve the problems in above-mentioned background technique.
The technical problem solved by the utility model is implemented by the following technical solutions: a kind of novel propylene glycol monomethyl ether
Acetic acid esters production dewatering system, comprising: tower reactor reboiler, atmospheric distillation tower, overhead condenser, tower reactor extraction pump, return tank,
Reflux pump, layering slot, the tower reactor reboiler gas phase mouth are connect with the lateral gas phase mouth of atmospheric distillation tower by pipeline A, and tower reactor is again
Boiling device liquid phase mouth is connect with atmospheric distillation tower tower bottom liquid phase mouth by pipeline B, atmospheric distillation tower top gaseous phase mouth and overhead condensation
The import of device gas phase is connected by pipeline D；Atmospheric distillation tower tower bottom liquid-phase outlet is connect with tower reactor extraction pump inlet by pipeline C；
Overhead condenser condensate liquid extraction mouth is connect with phase separation tank feed inlet by pipeline E；Phase separation tank side take-off mouth and return tank into
Material mouth is connected by pipeline F；Phase separation tank discharge port is connect with reflux pump inlet by pipeline G；Reflux pump outlet conduit and rectifying
Tower refluxing opening is connected by pipeline H；Phase separation tank tank bottom extraction mouth is produced waste water by pipeline K.
The return tank upper end is connected with emptying and goes system, and layering slot upper end is connected with waste water subsequent recovery processing system,
Overhead condenser, layering slot upper end are connected with tail gas and go total processing system.
The tower reactor reboiler is equipped with steam heater, steam condensate recovering device, sets on steam heater
There is steam pressure gauge PI.
The overhead condenser is equipped with circulating backwater system, recirculated water water-feeding system.
Subsequent distillation system is connected on the tower reactor extraction pump, tower reactor extraction pump, reflux pump are equipped with steam pressure gauge
PI。
The return tank, tower reactor reboiler, layering slot are equipped with liquid level sensor LI.
The dehydration distillation column bottom liquid phase pipeline B is equipped with sample tap AI, and phase separation tank tank bottom water gathering tube road K is equipped with sampling
Mouth AII, rectifier column reflux pipeline H are equipped with sample tap AIII, dehydration rectifier column reflux flow rates meter FT1 on H pipeline.
It is compared to open technology, there are following advantages for the utility model:
1) environmental requirement has been adapted to: according to Jiangsu Province about chemical industry Volatile organic emissions standard DB32/
The requirement of 3151-2016, dehydrating agent-benzene highest that original process use allow concentration of emission to be 6mg/m3, and the utility model
Used in ethyl acetate highest allow concentration of emission be 50mg/m3, select environment-friendly type dehydrating agent that can mitigate enterprise significantly
Exhaust emissions pressure；Generally there is water spray absorption plant additionally, due to tail gas, ethyl acetate is easier under trapping relative to benzene
Come, and the waste water ratio with ethyl acetate is easier biochemical treatment with the waste water of benzene.Simultaneously for toxicological point, ethyl acetate
With more preferably safety.
2) meet process to the performance requirement of dehydrating agent: dehydrating agent first has to that azeotropic can be formed with water, and azeotropic point is lower
More energy saving, in addition the azeotropic ratio of azeotropic substance and water is suitable；In addition best azeotropic mixture mass-energy direct layering, in this way can be big
It is big to reduce energy consumption；And ethyl acetate all has such advantage as benzene, so ethyl acetate and benzene are two kinds comparable de-
Water entrainer.
3) master operation does not increase the consumption of energy: being calculated according to the latent heat of vaporization, latent heat of vaporization when benzene boils is
394.1KJ/KG, and latent heat of vaporization when ethyl acetate boiling is 368KJ/KG, it is total according further to the component benzene water of two kinds of azeotropic
Boiling ratio is 91.1/8.9, and azeotropic point is 69.3 DEG C, and the azeotropic ratio of ethyl acetate and water is 93.9/6.1, and azeotropic point is
70.4℃；It knows that two kinds of entrainers are suitable using consumption energy by comparing and calculating, does not increase energy in dehydration procedure and disappear
Consumption.
4) postprocessing working procedures reduce the consumption of energy: since the subsequent waste water to dehydration procedure has recovery process, recycling
Mainly with steam heating the organic matter in waste water is stripped, due to ethyl acetate the latent heat of vaporization than benzene the latent heat of vaporization
It is low, so the consumption of energy can be reduced in stripping process.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the utility model.
Specific embodiment
In order to make, the technological means, creation characteristic, workflow, application method of the utility model reach purpose and effect is easy
Understand in understanding, below in conjunction with the utility model embodiment, to the technical scheme in the embodiment of the utility model carry out it is clear,
It is fully described by, it is clear that the described embodiments are only a part of the embodiments of the utility model, rather than whole implementation
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without making creative work
The every other embodiment obtained, fall within the protection scope of the utility model.
A kind of dewatering system of novel propylene glycol methyl ether acetate production, comprising: tower reactor reboiler 1, atmospheric distillation tower
2, overhead condenser 3, tower reactor extraction pump 4, return tank 5, reflux pump 6, layering slot 7,1 gas phase mouth of tower reactor reboiler and normal pressure
2 side of rectifying column is connected to gas phase mouth by pipeline A, and 1 liquid phase mouth of tower reactor reboiler passes through with 2 tower bottom liquid phase mouth of atmospheric distillation tower
Pipeline B connection, 2 top gaseous phase mouth of atmospheric distillation tower are connect with 3 gas phase import of overhead condenser by pipeline D；Atmospheric distillation tower 2
Tower bottom liquid-phase outlet produces 4 imports of pump with tower reactor and is connect by pipeline C；3 condensate liquid of overhead condenser produce mouth and phase separation tank 7 into
Material mouth is connected by pipeline E；7 side take-off mouth of phase separation tank is connect with 5 feed inlet of return tank by pipeline F；5 discharge port of phase separation tank
It is connect with 6 import of reflux pump by pipeline G；6 outlet conduit of reflux pump is connect with 2 refluxing opening of rectifying column by pipeline H；Split-phase
7 tank bottom of tank extraction mouth is produced waste water by pipeline K.
5 upper end of return tank is connected with emptying and goes system, and layering 7 upper end of slot is connected with waste water subsequent recovery processing system
System, overhead condenser 3, layering 7 upper end of slot are connected with tail gas and go total processing system.
The tower reactor reboiler 1 is equipped with steam heater, steam condensate recovering device, sets on steam heater
There is steam pressure gauge PI.
The overhead condenser 3 is equipped with circulating backwater system, recirculated water water-feeding system.
Subsequent distillation system is connected on the tower reactor extraction pump 4, tower reactor extraction pump 4, reflux pump 6 are equipped with steam pressure
Table PI.
The return tank 5, tower reactor reboiler 1, layering slot 7 are equipped with liquid level sensor LI.
The dehydration distillation column bottom liquid phase pipeline B is equipped with sample tap AI, and phase separation tank tank bottom water gathering tube road K is equipped with sampling
Mouth AII, rectifier column reflux pipeline H are equipped with sample tap AIII, dehydration rectifier column reflux flow rates meter FT1 on H pipeline.
A kind of dewatering of novel propylene glycol methyl ether acetate production, comprising the following steps:
(1) dehydrating agent is added into return tank in advance, the water of certain liquid level is added into phase separation tank, do standard for subsequent reflow
It is standby
(2) it is started to warm up, after tower reactor liquid level reaches 80% according to essence to dehydration treating column into esterification reaction solution first
Startup procedure is evaporated, total reflux operation is carried out；
(3) start the continuous feed into dehydration treating column, inlet amount is controlled according to production capacity；
(4) bottom temperature controls 130~150 DEG C or so, and tower top temperature controls 65~75 DEG C, and return flow FT1 control is
12~16m3/h；
(5) the sampling liquid of sampling analysis sample tap AI, sample tap AII, sample tap AIII, judges dehydrating effect；
(6) phase separation tank tank bottom extracted waste water enters recycling processing system-stripper and is stripped, and tower top light component is again
Enter dehydration rectifying column circulation；
(7) it continuously runs 24 hours or more, observation and the case where sampling analysis dehydrating agent；
(8) material content at each control point known to sampling analysis, when using benzene water azeotropic, tower reactor known to AI point sampling analysis
The moisture content of liquid be 40000 less than the COD in phase separation tank tank bottom extracted waste water known to 0.5%, AII point sampling analysis~
60000, i.e. the content of dissolved organic matter is that 4%~6%, AIII point sampling analysis knows water content < in phegma (dehydrating agent)
1%.When using ethyl acetate azeotrope with water, the moisture content of tower bottoms is < 0.2% known to AI point sampling analysis, and AII point takes
COD known to sample analysis in phase separation tank tank bottom extracted waste water is 40000~60000, i.e., the content of dissolved organic matter be 4%~
Water content < 1% in phegma known to 6%, AIII point sampling analysis.
Comparative example 1
Traditional Direct Dehydration mode: 80% water will be added in return tank in advance as phegma, prepare for subsequent reflow.
1) it is started to warm up, after tower reactor liquid level reaches 80% according to rectifying to dehydration treating column into esterification reaction solution first
Startup procedure gradually opens reflux pump, and regurgitant volume is by 1m3/ h, steps up 15m3/ h, until return tank level stability, i.e., entirely
Reflux operation is completed；
2) start the continuous feed into dehydration treating column, be 15m according to production capacity control charging3/ h, the constituent mass of thick ester
Content distribution is about (propylene glycol monomethyl ether 21%, acetic acid 24%, propylene glycol methyl ether acetate 50%, water 4%)；
3) bottom temperature controls 160 DEG C or so, and tower top temperature controls 105 DEG C, and water return flow FT1 control is 15m3/h；
4) moisture content of tower bottoms known to sampling analysis AI point sampling analysis is less than known to 1%, AII point sampling analysis
The content of dissolved organic matter is 5%~10% in water phase tank extracted waste water.
5) water phase tank extracted waste water enters recycling processing system-stripper and carries out stripping progress reuse.(here not to vapour
Stripper operation is repeated)
6) it continuously runs 24 hours or more, observation and sampling analysis, the above parameter are basicly stable.
Comparative example 2
Using benzene as azeotropy dehydrant: the benzene of 80% liquid level will be added in return tank in advance as dehydrating agent, it will be in phase separation tank
The water of 80% liquid level is added, prepares for subsequent reflow.
1) it is started to warm up, after tower reactor liquid level reaches 80% according to rectifying to dehydration treating column into esterification reaction solution first
Startup procedure gradually opens reflux pump, and regurgitant volume is by 1m3/ h, steps up 15m3/ h, until liquid in return tank and phase separation tank
Position is stablized, i.e. total reflux operation is completed；
2) start the continuous feed into dehydration treating column, be 15m according to production capacity control charging3/ h, the constituent mass of thick ester
Content distribution is about (propylene glycol monomethyl ether 21%, acetic acid 24%, propylene glycol methyl ether acetate 50%, water 4%)；
3) bottom temperature controls 140 DEG C or so, and tower top temperature controls 69 DEG C, and benzene return flow FT1 control is 14m3/h；
4) moisture content of tower bottoms known to sampling analysis AI point sampling analysis be can less than 0.5%, AII point sampling analysis
The content for knowing dissolved organic matter in phase separation tank tank bottom extracted waste water is that phegma is (de- known to 4%~6%, AIII point sampling analysis
Aqua) in water content < 1%.
5) phase separation tank tank bottom extracted waste water enters recycling processing system-stripper and is stripped, tower top light component (benzene, third
Glycol methyl ether, acetic acid and part water) re-enter into dehydration rectifying column circulation.(stripper operation not being repeated here)
6) it continuously runs 24 hours or more, observation and sampling analysis, the above parameter are basicly stable.
Embodiment 1
As shown in Fig. 1, will divide using the ethyl acetate that 80% liquid level is added in return tank as dehydrating agent in advance
The water of 80% liquid level is added in phase tank, prepares for subsequent reflow；
1) it is started to warm up, after tower reactor liquid level reaches 80% according to rectifying to dehydration treating column into esterification reaction solution first
Startup procedure gradually opens reflux pump, and regurgitant volume is by 1m3/ h, steps up 14m3/ h, until liquid in return tank and phase separation tank
Position is stablized, i.e. total reflux operation is completed；
2) start the continuous feed into dehydration treating column, be 15m according to production capacity control charging3/ h, the constituent mass of thick ester
Content distribution is about (propylene glycol monomethyl ether 21%, acetic acid 24%, propylene glycol methyl ether acetate 50%, water 4%)；
3) bottom temperature controls 135 DEG C or so, and tower top temperature controls 71 DEG C, and ethyl acetate backflow flow FT1 control is
14m3/h；
4) moisture content of tower bottoms known to sampling analysis AI point sampling analysis be can less than 0.2%, AII point sampling analysis
The content for knowing dissolved organic matter in phase separation tank tank bottom extracted waste water is that phegma is (de- known to 5%~8%, AIII point sampling analysis
Aqua) in water content < 1%.
5) phase separation tank tank bottom extracted waste water enters recycling processing system-stripper and is stripped, tower top light component (acetic acid
Ethyl ester, propylene glycol monomethyl ether, acetic acid and part water) re-enter into dehydration rectifying column circulation.
6) it continuously runs 24 hours or more, observation and sampling analysis, the above parameter are basicly stable.
By implementing 1 and 2 comparisons of comparative example by comparing above:
1) tradition carries out Direct Dehydration with the mode that water flows back, and 165 DEG C of bottom temperature are significantly larger than benzene azeotropic dewatering type
135 DEG C of bottom temperature, from the consumption of the energy, it is known that, the far super benzene azeotropic mode of Direct Dehydration mode；
2) in the water for using Direct Dehydration mode to deviate from, the content of organic matter is 5~10%, is dehydrated higher than benzene azeotropic mode
Waste water in content of organics 4~6%, so the processing pressure of stripper can be mitigated by the way of azeotropic dehydration.
3) tower top temperature is distinguished, and controls 105 DEG C using Direct Dehydration mode tower top temperature, and uses benzene azeotropic dewatering type
When, control top temperature is 69 DEG C or so, thus it is fewer than the refrigerant that Direct Dehydration originating party formula needs using benzene azeotropic dewatering type, i.e.,
Energy conservation.
4) it is dehydrated using Direct Dehydration method, the water content of obtained tower reactor mixed liquor is < 1%, and uses benzene as azeotropic
When agent is dehydrated, the water content for obtaining tower reactor mixed liquor is < 0.5%, it is known that is substantially better than the former using the latter.
By implementing 2 and the comparison of embodiment 1 by comparing above:
1) when being dehydrated using benzene as entrainer, the water content for obtaining tower reactor mixed liquor is < 0.5%, using ethyl acetate
When as entrainer dehydration, the water content for obtaining tower reactor mixed liquor is < 0.2%, it is known that is substantially better than the former using the latter.
2) the dissolved organic matter content in phase separation tank tank bottom extracted waste water is almost the same, is all 5%~8%, i.e., and subsequent time
It is consumed energy with device stripper almost the same.
3) it is 14m that rectifier column reflux amount is almost the same3/ h, 135 DEG C when bottom temperature control is using ethyl acetate are low
140 DEG C when using benzene, latent heat of vaporization when boiling according further to benzene is 394.1KJ/KG, and vaporization when ethyl ester boiling is latent
Heat is 368KJ/KG, and same regurgitant volume, then the energy consumption ratio using benzene as dehydrating agent is consumed energy using ethyl acetate as dehydrating agent
Greatly, this is also as dehydrating agent comparison benzene using ethyl acetate as the big advantage of dehydrating agent one；
4) the other characteristic of two kinds of substances of comparison, it is known that either on tail gas qualified discharge or biochemical wastewater treatment
On, for the hypotoxicity of ethyl acetate compares the toxicity of benzene, there is greater advantage.
The utility model is since ethyl acetate with benzene has similar azeotrope performance with water together, so the regurgitant volume of control
It is close with tower top azeotropic temperature, for producing the device of 50,000 tons of propylene glycol methyl ether acetates per year, reflux that when benzene water azeotropic controls
Amount FT1 is 12~15m3/ h, the regurgitant volume FT1 that when ethyl acetate azeotropic controls are 13~16m3/ h, control tower when benzene water azeotropic
Pushing up temperature is 69 DEG C or so, and it is 71 DEG C or so that ethyl ester azeotrope with water, which controls tower top temperature control,.
The material content at each control point known to sampling analysis, when using benzene water azeotropic, tower bottoms known to AI point sampling analysis
Moisture content be 40000 less than the COD in phase separation tank tank bottom extracted waste water known to 0.5%, AII point sampling analysis~
60000, i.e. the content of dissolved organic matter is that 4%~6%, AIII point sampling analysis knows water content < in phegma (dehydrating agent)
1%.When using ethyl acetate azeotrope with water, the moisture content of tower bottoms is < 0.2% known to AI point sampling analysis, and AII point takes
COD known to sample analysis in phase separation tank tank bottom extracted waste water is 40000~60000, i.e., the content of dissolved organic matter be 4%~
Water content < 1% in phegma known to 6%, AIII point sampling analysis.The moisture of dehydrating tower abjection enters recovery and processing system-
Stripper carries out stripping reuse, since content containing dissolved organic matter is consistent in water, so consumption energy is also the same.
The advantages of basic principles and main features and the utility model of the utility model have been shown and described above.Current row
The technical staff of industry is described in above embodiments and description it should be appreciated that the present utility model is not limited to the above embodiments
Only illustrate the principles of the present invention, on the premise of not departing from the spirit and scope of the utility model, the utility model is also
It will have various changes and improvements, these various changes and improvements fall within the scope of the claimed invention.The utility model
Claimed range be defined by the appending claims and its equivalent thereof.
Claims (7)
1. a kind of dewatering system of novel propylene glycol methyl ether acetate production, it is characterised in that: include: tower reactor reboiler, normal
Press rectifying column, overhead condenser, tower reactor extraction pump, return tank, reflux pump, layering slot, the tower reactor reboiler gas phase mouth with it is normal
The pressure lateral gas phase mouth of rectifying column is connected by pipeline A, and tower reactor reboiler liquid phase mouth and atmospheric distillation tower tower bottom liquid phase mouth pass through pipe
Road B connection, atmospheric distillation tower top gaseous phase mouth are connect with the import of overhead condenser gas phase by pipeline D；Atmospheric distillation tower tower bottom
Liquid-phase outlet is connect with tower reactor extraction pump inlet by pipeline C；Overhead condenser condensate liquid produces mouth and phase separation tank feed inlet is logical
Piping E connection；Phase separation tank side take-off mouth is connect with return tank feed inlet by pipeline F；Phase separation tank discharge port and reflux pump
Import is connected by pipeline G；Reflux pump outlet conduit is connect with rectifier column reflux mouth by pipeline H；Phase separation tank tank bottom produces mouth
Waste water is produced by pipeline K.
2. the dewatering system of the novel propylene glycol methyl ether acetate production of one kind according to claim 1, it is characterised in that:
The return tank upper end is connected with emptying and goes system, and layering slot upper end is connected with waste water subsequent recovery processing system, overhead condensation
Device, layering slot upper end are connected with tail gas and go total processing system.
3. the dewatering system of the novel propylene glycol methyl ether acetate production of one kind according to claim 1, it is characterised in that:
The tower reactor reboiler is equipped with steam heater, steam condensate recovering device, and steam heater is equipped with vapour pressure
Power table PI.
4. the dewatering system of the novel propylene glycol methyl ether acetate production of one kind according to claim 1, it is characterised in that:
The overhead condenser is equipped with circulating backwater system, recirculated water water-feeding system.
5. the dewatering system of the novel propylene glycol methyl ether acetate production of one kind according to claim 1, it is characterised in that:
Subsequent distillation system is connected on the tower reactor extraction pump, tower reactor extraction pump, reflux pump are equipped with steam pressure gauge PI.
6. the dewatering system of the novel propylene glycol methyl ether acetate production of one kind according to claim 1, it is characterised in that:
The return tank, tower reactor reboiler, layering slot are equipped with liquid level sensor LI.
7. the dewatering system of the novel propylene glycol methyl ether acetate production of one kind according to claim 1, it is characterised in that:
The atmospheric distillation tower bottom liquid pipe B is equipped with sample tap AI, and phase separation tank tank bottom water gathering tube road K is equipped with sample tap AII, essence
It evaporates tower reflux line H and is equipped with sample tap AIII, be dehydrated rectifier column reflux flow rates meter FT1 on H pipeline.
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