CN105481663B - A kind of clean diesel fuel additive polymethoxy methylal separation method - Google Patents
A kind of clean diesel fuel additive polymethoxy methylal separation method Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/58—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/10—Liquid carbonaceous fuels containing additives
- C10L1/14—Organic compounds
- C10L1/18—Organic compounds containing oxygen
- C10L1/185—Ethers; Acetals; Ketals; Aldehydes; Ketones
- C10L1/1852—Ethers; Acetals; Ketals; Orthoesters
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L2200/00—Components of fuel compositions
- C10L2200/04—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L2230/00—Function and purpose of a components of a fuel or the composition as a whole
- C10L2230/22—Function and purpose of a components of a fuel or the composition as a whole for improving fuel economy or fuel efficiency
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Abstract
The invention discloses a kind of polymethoxy methylal separation method；Due to thermal source of the process using the overhead vapours of dilute aldehyde concentration tower as lightness-removing column reboiler, product tower employs tower reactor reboiler and intermediate reboiler, using the thermal source of two kinds of different tastes, exactly because employ high-low pressure thermal coupling rectifying and intermediate reboiler technique, its process energy consumption is very low, and energy utilization is more reasonable；Material benzenemethanol consumes low, DMM in product3~8Purity is high, and process does not introduce the big extractant of toxicity, and caused Formaldehyde In Wastewarter meets environmental emission standard, is a kind of environment-friendly type technique for being suitable for the production of Large scale processes metaplasia.
Description
Technical field
The invention belongs to clean diesel fuel additive field, more particularly to a kind of clean diesel fuel additive polymethoxy methylal point
From method.
Background technology
China's derv fuel quality is relatively low, is mainly manifested in the content of sulfur content, Cetane number and aromatic hydrocarbons.Due to oil product
Of poor quality, tail gas pollution of motor-driven vehicle is serious caused by incomplete combustion, and this is also that PM2.5 values are higher, causes city haze to be formed
One of principal element.For this, China has put into effect new derv fuel standard in 2013（GB19147-2013）, but it is existing
Some oil refining process are difficult to produce satisfactory derv fuel.Chinese Diesel car implements in full the discharge standard of state four, to oil
The upgrading of quality is imperative.
Polymethoxy methylal（DMMn, n=3~8）It is generally acknowledged in the world to reduce oil consumption and reduce the new of fume emission
Environmental protection fuel oil blend component.DMMn has the following advantages that as diesel fuel additives:（1）With good fuel performance：Ten
Six alkane values are high, and oxygen content is high, make its burning abundant, remain few.This oxycompound of addition 20%, smoke intensity highest can reduce by 80%
~90%, NOx can reduce by 50%, and the thermal efficiency is also higher；（2）There is preferable engine cold-starting performance, there is preferable lubrication
Performance, the wear rate of injection pump, engine cylinder-body and connecting rod can be reduced, extend its service life；（3）With preferable security
Energy.It is obvious again in the security of transport, storage, use because flash-point is high；（4）Easily biological-degradable, to environment
Endanger small；Diesel engine need not be changed, can directly add use, while without separately add fuel-servicing equipment, storage facilities and personnel
Special technique is trained；（5）There is good compatibility with diesel oil, reconciled and used with certain proportion and diesel oil, oil consumption can be reduced, because
A kind of but really green diesel additive.
At present, DMMn synthesis is with separation method also in research or pilot scale stage, and there has been no industrialized unit operation.
The primary raw material of DMMn synthesis is methanol and formaldehyde, corresponding process route include ionic liquid-catalyzed method, liquid acid catalyzed process,
Solid acid catalysis method etc..
The ionic liquid that most category Lanzhou Inst. of Chemical Physics, Chinese Academy of Sciences uses is reported in DMMn synthesis technique
Body Catalytic processes.The A of the Chinese patent CN 104045530 and A of CN 104016838 describe ionic-liquid catalyst synthesis DMMn
Synthesis and separation method.Although the technique has pilot-plant success of the test, it is proposed using the technique that the country has also begun to enterprise
Industrialize demonstration plant.But be intermediate reaction raw material the process employs dimethoxym ethane and metaformaldehyde, corresponding follow-up point
Long from method route, process energy consumption is very high, and using the higher extractant of toxicity as separation medium, while to environment and people
Body security threat is larger, needs extra emission-control equipment.
United States Patent (USP) US 20080207954A1 and US20070260094A1 are reported using sulfuric acid, trifluoromethanesulfonic acid etc.
Acidic catalyst, with methanol, formaldehyde（Or metaformaldehyde）For raw material, the DMM of purity >=99% is obtained3And DMM4Product.Although its
Technological process is simple, but reaction condition is harsher, the target product DMM of reaction3~8Yield is relatively low, the circulation that process needs
Amount is big, and corresponding energy consumption is also high.Further, since using the higher acid catalyst of boiling point, serious corrosion, involved equipment
Pipeline needs the material using expensive resistant to catalyst corrosion.
Chinese patent CN 103626640A are described using formaldehyde and dimethoxym ethane as raw material, using being filled with solid acid tree
The fixed bed reactors of fat catalyst prepare DMMn method.Its process route is relatively simple, and catalyst cost is low, still
Process Energy fails rationally to utilize, and energy consumption is higher, and use hexamethylene be used as extractant, to environment and personal safety threat compared with
Greatly, a small amount of extractant is introduced in waste discharge, it is necessary to which extra device is handled.
In summary, for current DMMn synthesis route, there is process flow routes length, process high energy consumption, three
It is useless to handle the problems such as difficult, consider defect present in the DMMn market factor and the current techniques of DMMn, it is therefore necessary to develop
Go out a kind of process route is simple, energy consumption is low, the DMMn of environment-friendly type synthesis and separation method.
The content of the invention
The purpose of the present invention is for current DMMn synthesis and problem defect present in separation method, to Chinese patent CN
A kind of process route of solid acid catalyst technique synthesis DMMn offers is simple and direct used by 103848729 A, energy consumption is low, environment-friendly type
DMMn synthesis and separation method.
The technique directly uses methanol and formalin（Concentration >=37%）For raw material, using solid acid catalyst direct one
Footwork synthesis purpose product DMMn.Synthesis crude product from synthesis reactor（Containing methanol, formaldehyde, water and DMM1-10）Through synthesis
The separation circuit in downstream is pumped to after product pans by synthetic product conveying, realizes that DMMn is produced by a series of rectifying tower systems
Product refine.
A kind of clean diesel fuel additive polymethoxy methylal separation method, it is characterised in that：
Comprise the following steps：
（1）Synthesis crude product from upstream reaction system deliver to lightness-removing column system remove methanol therein, formaldehyde,
DMM1~2Light component, the light component of overhead extraction remove methanol distillation column, and the thick DMMn products of tower reactor go to product Tower System；
（2）In product Tower System, removing feeds the water in thick DMMn products, and overhead extraction contains micro DMM2~3Waste water
Sewage-treatment plant is gone to, tower bottoms obtains satisfactory polymethoxy methylal product DMM after cooling3~8；
（3）Methanol Recovery Tower System fully reclaims unreacted methanol, and the recovery methanol of overhead extraction returns to the anti-of upstream
System circulation is answered to utilize, the dilute formaldehyde of tower reactor delivers to dilute aldehyde concentration Tower System in downstream；
（4）Dilute aldehyde concentration Tower System concentrates to dilute aldehyde, and the formalin of concentration 36.5~37.4% that tower top obtains goes first
Aldehyde device or tank field, tower reactor waste water containing trace formaldehyde go to sewage-treatment plant after cooler cools down.
A kind of described clean diesel fuel additive polymethoxy methylal separation method, it is characterised in that：Described is de- light
Tower uses high-low pressure thermal coupling distillation technology, and lightness-removing column uses two kinds of thermals source, wherein the reboiler of lightness-removing column first using steam or
Other thermals source, the reboiler of lightness-removing column second, as thermal source, are reduced using the overhead vapours of dilute aldehyde concentration tower using thermal coupling methods
Rectifier unit comprehensive energy consumption.
A kind of described clean diesel fuel additive polymethoxy methylal separation method, it is characterised in that：Described product
Tower employs tower reactor reboiler and intermediate reboiler, and wherein product tower tower reactor reboiler uses the thermal source of GOOD TASTE, and product tower
Intermediate reboiler uses the thermal source of low taste.
A kind of described clean diesel fuel additive polymethoxy methylal separation method, it is characterised in that：Wherein lightness-removing column
20~100 pieces of number of theoretical plate, operating pressure normal pressure~0.5MPaG；30~100 pieces of product tower number of theoretical plate, operating pressure -0.09
~0.3MPaG；15~60 pieces of methanol distillation column number of theoretical plate, operating pressure normal pressure~0.5MPaG；Dilute aldehyde concentration tower theoretical plate 20
~80 pieces, operating pressure normal pressure~1.0MPaG.
A kind of described clean diesel fuel additive polymethoxy methylal separation method, it is characterised in that：
It is cold that described lightness-removing column system includes lightness-removing column, the reboiler of lightness-removing column first, the reboiler of lightness-removing column second, lightness-removing column
Condenser, lightness-removing column return tank, lightness-removing column reflux pump, product tower feed pump；
Described product Tower System include product tower, product tower reboiler, product tower intermediate reboiler, product delivery pump and
Product tower condenser, product tower return tank, product tower reflux pump, reactor product cooler；
Described Methanol Recovery Tower System include methanol distillation column, methanol distillation column reboiler, methanol distillation column reflux pump,
Methanol distillation column condenser and methanol distillation column return tank, dilute aldehyde concentration tower feed pump；
It is dense that described dilute aldehyde concentration Tower System includes dilute aldehyde concentration tower, dilute aldehyde concentration tower reboiler, gaseous effluent cooler, dilute aldehyde
Contracting tower return tank, dilute aldehyde concentration tower reflux pump, waste water delivery pump.
Polymethoxy methylal separation method of the present invention includes following unit：
1）Lightness-removing column system
Lightness-removing column C-10001 is mainly used in comparing DMM in removing synthesis crude product3The light component of low boiling point（Methanol, formaldehyde,
DMM1~2And part water）, while DMM as far as possible in recovery synthesis crude product3~10.Lightness-removing column overhead vapours is through condenser of light component removal column
Lightness-removing column return tank V-10001 is removed after E-10001 condensations, phegma is partly adopted after lightness-removing column reflux pump P-10001A/B boostings
Go out methanol distillation column C-10003, and remaining is as backflow.Lightness-removing column uses two kinds of thermals source, wherein the first reboiler of lightness-removing column E-
10002 use steam or other thermals source, and the second reboiler of lightness-removing column E-10003 is using the overhead vapours of dilute aldehyde concentration tower as heat
Source, to reduce the consumption of device.Lightness-removing column tower reactor crude product send downstream product after product tower feed pump P-10002A/B boostings
Tower C-10002.
2）Product Tower System
Product tower C-10002 is used to remove lightness-removing column C-10001 tower reactor crude product reclaimed waters, to ensure DMMnProduct reclaimed water contains
Amount is less than diesel oil reclaimed water content standard.Product tower C-10002 overhead vapours goes to produce after product tower condenser E-10004 condensations
Product tower return tank V-10002.Partly gaseous effluent cooler E- is removed in extraction to phegma after product tower reflux pump P-10003A/B boostings
10007, remaining is as backflow.Product tower is also used using the thermal source of two kinds of different tastes, wherein product tower reboiler E-10006
The thermal source of GOOD TASTE, and product tower intermediate reboiler E-10005 uses the thermal source of low taste.Product tower tower reactor DMMn products are through production
After product delivery pump P-10004A/B boostings tank field is delivered to through reactor product cooler E-10007.
3）Methanol Recovery Tower System
Methanol distillation column C-10003 is used to reclaim unreacted methanol and a small amount of formaldehyde, and recovery methanol returns after pump boosts
Reaction system is returned, to improve the conversion ratio of methanol.Methanol distillation column C-10003 overhead vapours is through methanol distillation column condenser E-
Methanol distillation column return tank V-10003 is removed after 10008 condensations.Phegma after the boosting of methanol distillation column reflux pump partly return by extraction
Reaction system is returned, remaining is as backflow.Thermal source needed for methanol distillation column separation carries by methanol distillation column reboiler E-10009
For the dilute aldehyde liquid of tower reactor delivers to dilute aldehyde concentration tower C-10004 after the boosting of dilute aldehyde concentration tower feed pump.
4）Dilute aldehyde concentrates Tower System
Dilute aldehyde concentration tower C-10004 concentrates dilute formaldehyde of methanol distillation column tower reactor, formalin after concentration（Concentration ~
37wt%）Formaldehyde plant is returned, improves the conversion ratio of formaldehyde, while formaldehyde in waste water is removed to and reaches wastewater discharge standard.It is dilute
Aldehyde concentration tower C-10004 overhead vapours removes dilute aldehyde concentration tower return tank V- after the second reboiler of lightness-removing column E-10002 condensations
10004.Formaldehyde plant or tank are removed in the dilute formaldehyde extraction in phegma part after dilute aldehyde concentration tower reflux pump P-10007A/B boostings
Area, remaining is as backflow.Thermal source needed for dilute aldehyde concentration tower separation is provided by dilute aldehyde concentration tower reboiler E-10010, and tower reactor is given up
Water is cold through gaseous effluent cooler E-10007 after merging with the waste water from product tower after waste water delivery pump P-10008A/B boostings
But decontamination water treatment facilities after.
Its core apparatus-rectifying column is conventional design in polymethoxy methylal separation method of the present invention
Plate column or packed tower.
Wherein 20 ~ 100 pieces of lightness-removing column number of theoretical plate, operating pressure normal pressure ~ 0.5MPaG；
30 ~ 100 pieces of product tower number of theoretical plate, operating pressure -0.09 ~ 0.3MPaG；
15 ~ 60 pieces of methanol distillation column number of theoretical plate, operating pressure normal pressure ~ 0.5MPaG；
Dilute 20 ~ 80 pieces of aldehyde concentration tower theoretical plate, operating pressure normal pressure ~ 1.0MPaG.
Its technological process of polymethoxy methylal separation method of the present invention is simple and direct；Because process concentrates dilute aldehyde
Thermal source of the overhead vapours of tower as lightness-removing column reboiler, product tower employs tower reactor reboiler and intermediate reboiler, using two
The thermal source of the different tastes of kind, exactly because employing high-low pressure thermal coupling rectifying and intermediate reboiler technique, its process energy consumption is very
Low, energy utilization is more reasonable；Material benzenemethanol consumes low, DMM in product3~8Purity is high, and process does not introduce the big extraction of toxicity
Agent, caused Formaldehyde In Wastewarter meet environmental emission standard, are a kind of environment-friendly types for being suitable for the production of Large scale processes metaplasia
Technique.
Brief description of the drawings
Fig. 1 is the FB(flow block) of polymethoxy methylal separation method of the present invention；
Fig. 2 is lightness-removing column system flow chart in polymethoxy methylal separation method of the present invention, wherein：
E-10003 is the reboiler of lightness-removing column second；
C-10001 is lightness-removing column；
E-10002 is the reboiler of lightness-removing column first；
E-10001 is condenser of light component removal column；
V-10001 is lightness-removing column return tank；
P-10001A/B is lightness-removing column reflux pump；
P-10002A/B is product tower feed pump；
Fig. 3 is product Tower System flow chart in polymethoxy methylal separation method of the present invention；
Wherein, E-10006 is product tower reboiler；
C-10002 is product tower；
E-10005 is product tower intermediate reboiler；
P-10004A/B is product delivery pump；
E-10004 is product tower condenser；
V-10002 is product tower return tank；
P-10003A/B is product tower reflux pump；
E-10007 is reactor product cooler；
Fig. 4 is methanol distillation column system flow chart in polymethoxy methylal separation method of the present invention；
Wherein, E-10009 is methanol distillation column reboiler；
C-10003 is methanol distillation column；
P-10005A/B is methanol distillation column reflux pump；
E-10008 is methanol distillation column condenser；
V-10003 is methanol distillation column return tank；
P-10006A/B is dilute aldehyde concentration tower feed pump；
Fig. 5 is dilute aldehyde concentration tower system flow chart in polymethoxy methylal separation method of the present invention；
E-10010 is dilute aldehyde concentration tower reboiler；
C-10004 is dilute aldehyde concentration tower；
E-10011 is gaseous effluent cooler；
V-10004 is dilute aldehyde concentration tower return tank；
P-10007A/B is dilute aldehyde concentration tower reflux pump；
P-10008A/B is waste water delivery pump.
Embodiment
Embodiment 1,
The raw material of the separation method comes from upstream synthesis reactor, and synthesis crude product mainly contains DMM3~10And water, containing a small amount of
DMM1~2The methanol and formaldehyde complete with unreacted.Synthesis crude product is pumped to lightness-removing column C-10001 by synthetic product conveying.
Lightness-removing column C-10001 operating pressures normal pressure~0.5Mpa.Lightness-removing column uses two kinds of thermals source, wherein lightness-removing column first
Reboiler E-10002 uses steam or other thermals source, and the second reboiler of lightness-removing column E-10003 is steamed using the tower top of dilute aldehyde concentration tower
Vapour is as thermal source.Separated by rectifying, by methanol, formaldehyde, DMM in raw material1~2Lights removal, tower reactor crude product are mainly
DMM3~10, containing a small amount of water.Crude product send downstream product tower C-10002 after product tower feed pump P-10002A/B boostings.
- 0.09~0.3MPaG of product tower C-10002 operating pressures.The thermals source that product tower is also sampled using two kinds of differences, its
Middle product tower reboiler E-10006 uses the thermal source of GOOD TASTE, and product tower intermediate reboiler E-10005 uses the heat of low taste
Source.DMM in product tower tower reactor DMMn products3~8>=99.5%, containing a small amount of heavy constituent DMM9~10And water.DMMn products are defeated through product
Pump P-10004A/B is sent through reactor product cooler E-10007 to deliver to tank field after boosting.DMM in the waste water of overhead extraction simultaneously3Content
Less than industrial wastewater discharge standard.
Recovery methanol from lightness-removing column tower top delivers to methanol distillation column C-10003, methanol distillation column operating pressure normal pressure
~0.5MPaG, the recovery methanol of overhead extraction return to synthesis reaction system to improve the conversion ratio of methanol, tower reactor after pump boosts
Dilute formaldehyde delivers to dilute aldehyde concentration tower in downstream.
Dilute aldehyde concentration tower C-10004 operating pressures normal pressure~1.0MPaG.Dilute aldehyde concentration tower C-10004 overhead vapours conducts
The second reboiler of lightness-removing column E-10003 thermal source, tower top dilute formaldehyde after being concentrated（Concentration 37wt%）Formaldehyde plant is returned, is carried
The conversion ratio of high formaldehyde.Tower reactor formaldehyde in waste water is removed to less than 1ppm, cold through waste water after merging with the waste water from product tower
But decontamination water treatment facilities after device E-10007 coolings.
Embodiment 2,
A kind of clean diesel fuel additive polymethoxy methylal separation method,
Comprise the following steps：
（1）Synthesis crude product from upstream reaction system deliver to lightness-removing column system remove methanol therein, formaldehyde,
DMM1~2Light component, the light component of overhead extraction remove methanol distillation column, and the thick DMMn products of tower reactor go to product Tower System；
（2）In product Tower System, removing feeds the water in thick DMMn products, and overhead extraction contains micro DMM2~3Waste water
Sewage-treatment plant is gone to, tower bottoms obtains satisfactory polymethoxy methylal product DMM after cooling3~8；
（3）Methanol Recovery Tower System fully reclaims unreacted methanol, and the recovery methanol of overhead extraction returns to the anti-of upstream
System circulation is answered to utilize, the dilute formaldehyde of tower reactor delivers to dilute aldehyde concentration Tower System in downstream；
（4）Dilute aldehyde concentration Tower System concentrates to dilute aldehyde, and the formalin of concentration 36.5~37.4% that tower top obtains goes first
Aldehyde device or tank field, tower reactor waste water containing trace formaldehyde go to sewage-treatment plant after cooler cools down.
Described lightness-removing column uses high-low pressure thermal coupling distillation technology, and lightness-removing column uses two kinds of thermals source, wherein lightness-removing column
One reboiler uses steam or other thermals source, the reboiler of lightness-removing column second using the overhead vapours of dilute aldehyde concentration tower as thermal source,
Rectifier unit comprehensive energy consumption is reduced using thermal coupling methods.
Described product tower employs tower reactor reboiler and intermediate reboiler, and wherein product tower tower reactor reboiler uses Gao Pin
The thermal source of taste, and product tower intermediate reboiler uses the thermal source of low taste.
Wherein 20~100 pieces of lightness-removing column number of theoretical plate, operating pressure normal pressure~0.5MPaG；Product tower number of theoretical plate 30~
100 pieces, operating pressure -0.09~0.3MPaG；15~60 pieces of methanol distillation column number of theoretical plate, operating pressure normal pressure~
0.5MPaG；Dilute 20~80 pieces of aldehyde concentration tower theoretical plate, operating pressure normal pressure~1.0MPaG.
It is cold that described lightness-removing column system includes lightness-removing column, the reboiler of lightness-removing column first, the reboiler of lightness-removing column second, lightness-removing column
Condenser, lightness-removing column return tank, lightness-removing column reflux pump, product tower feed pump；
Described product Tower System include product tower, product tower reboiler, product tower intermediate reboiler, product delivery pump and
Product tower condenser, product tower return tank, product tower reflux pump, reactor product cooler；
Described Methanol Recovery Tower System include methanol distillation column, methanol distillation column reboiler, methanol distillation column reflux pump,
Methanol distillation column condenser and methanol distillation column return tank, dilute aldehyde concentration tower feed pump；
It is dense that described dilute aldehyde concentration Tower System includes dilute aldehyde concentration tower, dilute aldehyde concentration tower reboiler, gaseous effluent cooler, dilute aldehyde
Contracting tower return tank, dilute aldehyde concentration tower reflux pump, waste water delivery pump.
Polymethoxy methylal separation method described in the present embodiment includes following unit：
1）Lightness-removing column system
Lightness-removing column C-10001 is mainly used in comparing DMM in removing synthesis crude product3The light component of low boiling point（Methanol, formaldehyde,
DMM1~2And part water）, while DMM as far as possible in recovery synthesis crude product3~10.Lightness-removing column overhead vapours is through condenser of light component removal column
Lightness-removing column return tank V-10001 is removed after E-10001 condensations, phegma is partly adopted after lightness-removing column reflux pump P-10001A/B boostings
Go out methanol distillation column C-10003, and remaining is as backflow.Lightness-removing column uses two kinds of thermals source, wherein the first reboiler of lightness-removing column E-
10002 use steam or other thermals source, and the second reboiler of lightness-removing column E-10003 is using the overhead vapours of dilute aldehyde concentration tower as heat
Source, to reduce the consumption of device.Lightness-removing column tower reactor crude product send downstream product after product tower feed pump P-10002A/B boostings
Tower C-10002.
2）Product Tower System
Product tower C-10002 is used to remove lightness-removing column C-10001 tower reactor crude product reclaimed waters, to ensure DMMnProduct reclaimed water contains
Amount is less than diesel oil reclaimed water content standard.Product tower C-10002 overhead vapours goes to produce after product tower condenser E-10004 condensations
Product tower return tank V-10002.Partly gaseous effluent cooler E- is removed in extraction to phegma after product tower reflux pump P-10003A/B boostings
10007, remaining is as backflow.Product tower is also used using the thermal source of two kinds of different tastes, wherein product tower reboiler E-10006
The thermal source of GOOD TASTE, and product tower intermediate reboiler E-10005 uses the thermal source of low taste.Product tower tower reactor DMMn products are through production
After product delivery pump P-10004A/B boostings tank field is delivered to through reactor product cooler E-10007.
3）Methanol Recovery Tower System
Methanol distillation column C-10003 is used to reclaim unreacted methanol and a small amount of formaldehyde, and recovery methanol returns after pump boosts
Reaction system is returned, to improve the conversion ratio of methanol.Methanol distillation column C-10003 overhead vapours is through methanol distillation column condenser E-
Methanol distillation column return tank V-10003 is removed after 10008 condensations.Phegma after the boosting of methanol distillation column reflux pump partly return by extraction
Reaction system is returned, remaining is as backflow.Thermal source needed for methanol distillation column separation carries by methanol distillation column reboiler E-10009
For the dilute aldehyde liquid of tower reactor delivers to dilute aldehyde concentration tower C-10004 after the boosting of dilute aldehyde concentration tower feed pump.
4）Dilute aldehyde concentrates Tower System
Dilute aldehyde concentration tower C-10004 concentrates dilute formaldehyde of methanol distillation column tower reactor, formalin after concentration（Concentration ~
37wt%）Formaldehyde plant is returned, improves the conversion ratio of formaldehyde, while formaldehyde in waste water is removed to and reaches wastewater discharge standard.It is dilute
Aldehyde concentration tower C-10004 overhead vapours removes dilute aldehyde concentration tower return tank V- after the second reboiler of lightness-removing column E-10002 condensations
10004.Formaldehyde plant or tank are removed in the dilute formaldehyde extraction in phegma part after dilute aldehyde concentration tower reflux pump P-10007A/B boostings
Area, remaining is as backflow.Thermal source needed for dilute aldehyde concentration tower separation is provided by dilute aldehyde concentration tower reboiler E-10010, and tower reactor is given up
Water is cold through gaseous effluent cooler E-10007 after merging with the waste water from product tower after waste water delivery pump P-10008A/B boostings
But decontamination water treatment facilities after.
Claims (4)
- A kind of 1. clean diesel fuel additive polymethoxy methylal separation method, it is characterised in that：Comprise the following steps：（1）Synthesis crude product from upstream reaction system delivers to lightness-removing column system removal methanol therein, formaldehyde, DMM1~2Gently Component, the light component of overhead extraction remove methanol distillation column, and the thick DMMn products of tower reactor go to product Tower System；（2）In product Tower System, removing feeds the water in thick DMMn products, and overhead extraction contains micro DMM2~3Waste water is gone to Sewage-treatment plant, tower bottoms obtain satisfactory polymethoxy methylal product DMM after cooling3~8；（3）Methanol Recovery Tower System fully reclaims unreacted methanol, and the recovery methanol of overhead extraction returns to the reaction system of upstream System recycles, and the dilute formaldehyde of tower reactor delivers to dilute aldehyde concentration Tower System in downstream；（4）Dilute aldehyde concentration Tower System concentrates to dilute aldehyde, and the formalin of concentration 36.5~37.4% that tower top obtains goes formaldehyde to fill Put or tank field, tower reactor waste water containing trace formaldehyde go to sewage-treatment plant after cooler cools down；Described lightness-removing column uses high-low pressure thermal coupling distillation technology, and lightness-removing column uses two kinds of thermals source, wherein lightness-removing column first again Boiling device uses steam or other thermals source, and the reboiler of lightness-removing column second, as thermal source, is used using the overhead vapours of dilute aldehyde concentration tower Thermal coupling methods reduce rectifier unit comprehensive energy consumption.
- A kind of 2. clean diesel fuel additive polymethoxy methylal separation method according to claim 1, it is characterised in that： Described product tower employs tower reactor reboiler and intermediate reboiler, and wherein product tower tower reactor reboiler uses the heat of GOOD TASTE Source, and product tower intermediate reboiler uses the thermal source of low taste.
- A kind of 3. clean diesel fuel additive polymethoxy methylal separation method according to claim 1, it is characterised in that： Wherein 20~100 pieces of lightness-removing column number of theoretical plate, operating pressure normal pressure~0.5MPaG；30~100 pieces of product tower number of theoretical plate, behaviour Make pressure -0.09~0.3MPaG；15~60 pieces of methanol distillation column number of theoretical plate, operating pressure normal pressure~0.5MPaG；Dilute aldehyde is dense 20~80 pieces of contracting tower theoretical plate, operating pressure normal pressure~1.0MPaG.
- A kind of 4. clean diesel fuel additive polymethoxy methylal separation method according to claim 1, it is characterised in that：Described lightness-removing column system includes lightness-removing column, the reboiler of lightness-removing column first, the reboiler of lightness-removing column second, lightness-removing column condensation Device, lightness-removing column return tank, lightness-removing column reflux pump, product tower feed pump；Described product Tower System includes product tower, product tower reboiler, product tower intermediate reboiler, product delivery pump and product Tower condenser, product tower return tank, product tower reflux pump, reactor product cooler；Described Methanol Recovery Tower System includes methanol distillation column, methanol distillation column reboiler, methanol distillation column reflux pump, methanol Recovery tower condenser and methanol distillation column return tank, dilute aldehyde concentration tower feed pump；Described dilute aldehyde concentration Tower System includes dilute aldehyde concentration tower, dilute aldehyde concentration tower reboiler, gaseous effluent cooler, dilute aldehyde concentration tower Return tank, dilute aldehyde concentration tower reflux pump, waste water delivery pump.
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| CN103848730B (en) * | 2014-01-09 | 2015-06-17 | 东营市润成碳材料科技有限公司 | Production device system and production process for polymethoxy dimethyl ether (PODE) |
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