CN105481663A - Separation method of clean diesel additive polymethoxy methylal - Google Patents
Separation method of clean diesel additive polymethoxy methylal Download PDFInfo
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- CN105481663A CN105481663A CN201511003202.2A CN201511003202A CN105481663A CN 105481663 A CN105481663 A CN 105481663A CN 201511003202 A CN201511003202 A CN 201511003202A CN 105481663 A CN105481663 A CN 105481663A
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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 separation method of polymethoxy methylal. Overhead vapor of a dilute aldehyde concentrating tower is used as a heat source of a light component removal tower reboiler in the process, and the product tower adopts a tower bottom reboiler and a middle reboiler, thereby adopting two heat sources with different grades; and due to the adoption of the high/low-pressure thermal coupling rectification and middle reboiler technique, the process has the advantages of very low energy consumption and reasonable energy utilization. The raw material methanol consumption is low, the DMM3-8 purity in the product is high, no high-toxicity extractant is introduced in the process, the formaldehyde content in the generated wastewater conforms to the environment-friendly discharge standard, and thus, the method is an environment-friendly technique which is suitable for large-scale technical production.
Description
Technical field
The invention belongs to clean diesel fuel additive field, particularly relate to a kind of clean diesel fuel additive polymethoxy methylal separation method.
Background technology
China's derv fuel oil quality is lower, is mainly manifested on the content of sulphur content, cetane value and aromatic hydrocarbons.Because oil quality is poor, because incomplete combustion causes tail gas pollution of motor-driven vehicle serious, this is also that PM2.5 value is higher, one of principal element causing city haze to be formed.For this reason, China has put into effect new derv fuel oil standard (GB19147-2013) in 2013, but existing oil refining process is difficult to produce satisfactory derv fuel oil.State four emission standard implemented in full by Chinese Diesel car, imperative to the upgrading of oil quality.
Polymethoxy methylal (DMMn, n=3 ~ 8) is the reduction oil consumption of generally acknowledging in the world and the novel environment-friendly fuel oil blend component reducing fume emission.DMMn, as diesel-dope, has following advantage: (1) has good fuel performance: cetane value is high, and oxygen level is high, makes its sufficient combustion, residual few.Add this oxycompound of 20%, smoke intensity is the highest to be reduced by 80% ~ 90%, NOx and can reduce by 50%, and thermo-efficiency is also higher; (2) there is good engine cold-starting performance, have good lubricity, the wear rate of oil injection pump, engine cylinder-body and connecting rod can be reduced, extend its work-ing life; (3) there is good safety performance.Because flash-point is high, be again apparent in the security of transport, storage, use; (4) readily biodegradable is little to environmental hazard; Need not diesel engine be changed, directly can add use, simultaneously without the need to separately adding the special technique training of bunkering facilities, storage facilities and personnel; (5) with diesel oil have good compatibility, use with certain proportion and diesel oil blending, can oil consumption be reduced, because of but a kind of real green diesel additive.
At present, the synthesis of DMMn and separation method are also in be studied or the pilot scale stage, not yet has industrialized unit to go into operation.The main raw material of DMMn synthesis is methyl alcohol and formaldehyde, and corresponding operational path comprises ionic liquid-catalyzed method, liquid acid catalysis method, solid acid catalysis method etc.
The ionic liquid-catalyzed technique that maximum genus Lanzhou Inst. of Chemical Physics, Chinese Academy of Sciences adopts is reported in the synthesis technique of DMMn.Chinese patent CN104045530A and CN104016838A describes synthesis and the separation method of ionic-liquid catalyst synthesis DMMn.Although this technique has pilot plant to test successfully, domestic also beginning has enterprise to adopt this technique to plan to build industrialization demonstration unit.But the process employs methylal and trioxymethylene is intermediate reaction raw material, corresponding follow-up separation method route is long, and process energy consumption is very high, and adopts extraction agent that toxicity is higher as separate medium, environment and personnel safety are threatened comparatively large simultaneously, need extra emission-control equipment.
US Patent No. 20080207954A1 and US20070260094A1 reports and adopts an acidic catalyst such as sulfuric acid, trifluoromethanesulfonic acid, with methyl alcohol, formaldehyde (or trioxymethylene) for raw material, obtains the DMM of purity>=99%
3and DMM
4product.Although its technical process is simple, reaction conditions is harsher, the target product DMM of reaction
3 ~ 8yield is lower, and the internal circulating load of process need is large, and corresponding energy consumption is also high.In addition, owing to adopting the acid catalyst that boiling point is higher, serious corrosion, involved equipment pipe needs the material adopting expensive resistant to catalyst corrosion.
Chinese patent CN103626640A describes with formaldehyde and methylal for raw material, adopts the fixed-bed reactor being filled with solid acidic resin catalyst to prepare the method for DMMn.Its operational path is relatively simple, and catalyzer cost is low, but Process Energy fails Appropriate application, energy consumption is higher, and the cyclohexane give adopted is extraction agent, threatens larger to environment and personnel safety, introduce a small amount of extraction agent in waste discharge, need extra device to process.
In sum, synthesis route for current DMMn also exists the problems such as process flow routes is long, process energy consumption is high, three-protection design is difficult, consider the defect existed in the market factor of DMMn and the current technique of DMMn, be therefore necessary to develop that a kind of operational path is simple, energy consumption is low, the DMMn of environment-friendly type synthesizes and separation method.
Summary of the invention
The object of the invention is for current DMMn synthesis and Problems existing defect in separation method, the solid acid catalyst technique synthesis DMMn adopted Chinese patent CN103848729A provides that a kind of operational path is simple and direct, energy consumption is low, the DMMn of environment-friendly type synthesizes and separation method.
This technique directly adopts methyl alcohol and formaldehyde solution (concentration >=37%) to be raw material, adopts solid acid catalyst direct one-step synthesis method object product D MMn.From the synthesis crude product of synthesis reactor (containing methyl alcohol, formaldehyde, water and DMM
1-10) after synthetic product tundish, the separation circuit in downstream is delivered to by synthetic product transferpump, realize the refining of DMMn product by a series of rectifying tower system.
A kind of clean diesel fuel additive polymethoxy methylal separation method, is characterized in that:
Comprise the following steps:
(1) the synthesis crude product from upstream reaction system delivers to the removal of lightness-removing column system methyl alcohol, formaldehyde, DMM wherein
1 ~ 2light constituent, the light constituent of overhead extraction removes methanol distillation column, and the thick DMMn product of tower reactor goes to product Tower System;
(2) in product Tower System, remove the water in the thick DMMn product of charging, overhead extraction containing micro-DMM
2 ~ 3waste water goes to waste disposal plant, and tower bottoms obtains satisfactory polymethoxy methylal product DMM after cooling
3 ~ 8;
(3) Methanol Recovery Tower System fully reclaims unreacted methyl alcohol, and the recovery methyl alcohol of overhead extraction returns the reactive system recycle of upstream, and the rare formaldehyde of tower reactor delivers to rare aldehyde upgrading tower system in downstream;
(4) rare aldehyde upgrading tower system concentrates rare aldehyde, and concentration 36.5 ~ 37.4% formaldehyde solution that tower top obtains goes to formaldehyde plant or tank field, and tower reactor goes to waste disposal plant containing trace formaldehyde waste water after water cooler cooling.
Described a kind of clean diesel fuel additive polymethoxy methylal separation method, it is characterized in that: described lightness-removing column adopts high-low pressure thermal coupling distillation technology, lightness-removing column adopts two kinds of thermals source, wherein lightness-removing column first reboiler adopts steam or other thermals source, lightness-removing column second reboiler adopts the overhead vapours of rare aldehyde upgrading tower as thermal source, adopts thermal coupling methods to reduce rectifier unit comprehensive energy consumption.
Described a kind of clean diesel fuel additive polymethoxy methylal separation method, it is characterized in that: described product tower have employed tower reactor reboiler and intermediate reboiler, wherein product tower tower reactor reboiler adopts the thermal source of GOOD TASTE, and product tower intermediate reboiler adopts the thermal source of low taste.
Described a kind of clean diesel fuel additive polymethoxy methylal separation method, is characterized in that: wherein lightness-removing column number of theoretical plate 20 ~ 100 pieces, working pressure normal pressure ~ 0.5MPaG; Product tower number of theoretical plate 30 ~ 100 pieces, working pressure-0.09 ~ 0.3MPaG; Methanol distillation column number of theoretical plate 15 ~ 60 pieces, working pressure normal pressure ~ 0.5MPaG; Rare aldehyde upgrading tower theoretical stage 20 ~ 80 pieces, working pressure normal pressure ~ 1.0MPaG.
Described a kind of clean diesel fuel additive polymethoxy methylal separation method, is characterized in that:
Described lightness-removing column system comprises lightness-removing column, lightness-removing column first reboiler, lightness-removing column second reboiler, condenser of light component removal column, lightness-removing column return tank, lightness-removing column reflux pump, product tower fresh feed pump;
Described product Tower System comprises product tower, product tower reboiler, product tower intermediate reboiler, product transferpump and product tower condenser, product tower return tank, product tower reflux pump, reactor product cooler;
Described Methanol Recovery Tower System comprises methanol distillation column, methanol distillation column reboiler, methanol distillation column reflux pump, methanol distillation column condenser and methanol distillation column return tank, rare aldehyde upgrading tower fresh feed pump;
Described rare aldehyde upgrading tower system comprises rare aldehyde upgrading tower, rare aldehyde upgrading tower reboiler, gaseous effluent cooler, rare aldehyde upgrading tower return tank, rare aldehyde upgrading tower reflux pump, waste water transferpump.
Polymethoxy methylal separation method of the present invention comprises following unit:
1) lightness-removing column system
Lightness-removing column C-10001 is mainly used in removing in synthesis crude product and compares DMM
3low-boiling light constituent (methyl alcohol, formaldehyde, DMM
1 ~ 2and part water), reclaim DMM in synthesis crude product as far as possible simultaneously
3 ~ 10.Lightness-removing column overhead vapours removes lightness-removing column return tank V-10001 after condenser of light component removal column E-10001 condensation, and phegma removes methanol distillation column C-10003 through lightness-removing column reflux pump P-10001A/B boosting rear section extraction, and all the other are as backflow.Lightness-removing column adopts two kinds of thermals source, and wherein lightness-removing column first reboiler E-10002 adopts steam or other thermals source, and lightness-removing column second reboiler E-10003 adopts the overhead vapours of rare aldehyde upgrading tower as thermal source, to reduce the consumption of device.The thick product of lightness-removing column tower reactor send derived product tower C-10002 after product tower fresh feed pump P-10002A/B boosts.
2) product Tower System
Product tower C-10002 is used for removing water in the thick product of lightness-removing column C-10001 tower reactor, to ensure DMM
nin product, water-content is lower than water-content standard in diesel oil.Product tower C-10002 overhead vapours removes product tower return tank V-10002 after product tower condenser E-10004 condensation.Phegma removes gaseous effluent cooler E-10007 through product tower reflux pump P-10003A/B boosting rear section extraction, and all the other are as backflow.Product tower also adopts the thermal source of two kinds of different tastes, and wherein product tower reboiler E-10006 adopts the thermal source of GOOD TASTE, and product tower intermediate reboiler E-10005 adopts the thermal source of low taste.Product tower tower reactor DMMn product delivers to tank field through reactor product cooler E-10007 after product transferpump P-10004A/B boosts.
3) Methanol Recovery Tower System
Methanol distillation column C-10003, for reclaiming unreacted methyl alcohol and a small amount of formaldehyde, reclaims methyl alcohol Returning reacting system after pump boosting, to improve the transformation efficiency of methyl alcohol.Methanol distillation column C-10003 overhead vapours removes methanol distillation column return tank V-10003 after methanol distillation column condenser E-10008 condensation.Phegma is through methanol distillation column reflux pump boosting rear section extraction Returning reacting system, and all the other are as backflow.Thermal source needed for methanol distillation column is separated provides by methanol distillation column reboiler E-10009, and tower reactor rare aldehyde liquid delivers to rare aldehyde upgrading tower C-10004 after rare aldehyde upgrading tower fresh feed pump boosting.
4) rare aldehyde upgrading tower system
Rare formaldehyde of methanol distillation column tower reactor concentrates by rare aldehyde upgrading tower C-10004, and after concentrated, formaldehyde solution (concentration ~ 37wt%) returns formaldehyde plant, improves the transformation efficiency of formaldehyde, is removed to by formaldehyde in waste water simultaneously and reaches wastewater discharge standard.Rare aldehyde upgrading tower C-10004 overhead vapours removes rare aldehyde upgrading tower return tank V-10004 after lightness-removing column second reboiler E-10002 condensation.Phegma goes to formaldehyde plant or tank field through rare aldehyde upgrading tower reflux pump P-10007A/B boosting rare formaldehyde extraction in rear section, and all the other are as backflow.Thermal source needed for rare aldehyde upgrading tower is separated provides by rare aldehyde upgrading tower reboiler E-10010, tower reactor waste water after waste water transferpump P-10008A/B boosts, after merging with the waste water from product tower after gaseous effluent cooler E-10007 cools decontaminated water treatment unit.
In polymethoxy methylal separation method of the present invention, its core apparatus-rectifying tower is tray column or the packing tower of conventional design.
Wherein lightness-removing column number of theoretical plate 20 ~ 100 pieces, working pressure normal pressure ~ 0.5MPaG;
Product tower number of theoretical plate 30 ~ 100 pieces, working pressure-0.09 ~ 0.3MPaG;
Methanol distillation column number of theoretical plate 15 ~ 60 pieces, working pressure normal pressure ~ 0.5MPaG;
Rare aldehyde upgrading tower theoretical stage 20 ~ 80 pieces, working pressure normal pressure ~ 1.0MPaG.
Its technical process of polymethoxy methylal separation method of the present invention is simple and direct; Because process is using the thermal source of the overhead vapours of rare aldehyde upgrading tower as lightness-removing column reboiler, product tower have employed tower reactor reboiler and intermediate reboiler, adopt the thermal source of two kinds of different tastes, exactly because have employed high-low pressure thermal coupling rectifying and intermediate reboiler technique, its process energy consumption is very low, and Energy harvesting is more reasonable; Material benzenemethanol consumes low, DMM in product
3 ~ 8purity is high, and process does not introduce the large extraction agent of toxicity, and the Formaldehyde In Wastewarter of generation meets environmental emission standard, is a kind of environment-friendly type technique being suitable for Large scale processesization and producing.
Accompanying drawing explanation
Fig. 1 is the FB(flow block) of polymethoxy methylal separation method of the present invention;
Fig. 2 is lightness-removing column system flowchart in polymethoxy methylal separation method of the present invention, wherein:
E-10003 is lightness-removing column second reboiler;
C-10001 is lightness-removing column;
E-10002 is lightness-removing column first reboiler;
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 fresh feed pump;
Fig. 3 is product Tower System schema 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 transferpump;
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 flowchart 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 rare aldehyde upgrading tower fresh feed pump;
Fig. 5 is rare aldehyde upgrading tower system flowchart in polymethoxy methylal separation method of the present invention;
E-10010 is rare aldehyde upgrading tower reboiler;
C-10004 is rare aldehyde upgrading tower;
E-10011 is gaseous effluent cooler;
V-10004 is rare aldehyde upgrading tower return tank;
P-10007A/B is rare aldehyde upgrading tower reflux pump;
P-10008A/B is waste water transferpump.
Embodiment
Embodiment 1,
The raw material of this separation method is from upstream synthesis reactor, and synthesis crude product is mainly containing DMM
3 ~ 10and water, containing a small amount of DMM
1 ~ 2the methyl alcohol complete with unreacted and formaldehyde.Synthesis crude product delivers to lightness-removing column C-10001 by synthetic product transferpump.
Lightness-removing column C-10001 working pressure normal pressure ~ 0.5Mpa.Lightness-removing column adopts two kinds of thermals source, and wherein lightness-removing column first reboiler E-10002 adopts steam or other thermals source, and lightness-removing column second reboiler E-10003 adopts the overhead vapours of rare aldehyde upgrading tower as thermal source.By rectifying separation, by methyl alcohol, formaldehyde, DMM in raw material
1 ~ 2lights removal, the thick product of tower reactor mainly DMM
3 ~ 10, containing a small amount of water.Thick product send derived product tower C-10002 after product tower fresh feed pump P-10002A/B boosts.
Product tower C-10002 working pressure-0.09 ~ 0.3MPaG.Product tower also adopts the thermal source of two kinds of different tastes, and wherein product tower reboiler E-10006 adopts the thermal source of GOOD TASTE, and product tower intermediate reboiler E-10005 adopts the thermal source of low taste.DMM in product tower tower reactor DMMn product
3 ~ 8>=99.5%, containing a small amount of heavy constituent DMM
9 ~ 10and water.DMMn product delivers to tank field through reactor product cooler E-10007 after product transferpump P-10004A/B boosts.DMM in the waste water of simultaneously overhead extraction
3content is lower than industrial wastewater discharge standard.
Recovery methyl alcohol from lightness-removing column tower top delivers to methanol distillation column C-10003, methanol distillation column working pressure normal pressure ~ 0.5MPaG, the recovery methyl alcohol of overhead extraction returns synthesis reaction system to improve the transformation efficiency of methyl alcohol after pump boosting, and the rare formaldehyde of tower reactor delivers to rare aldehyde upgrading tower in downstream.
Rare aldehyde upgrading tower C-10004 working pressure normal pressure ~ 1.0MPaG.Rare aldehyde upgrading tower C-10004 overhead vapours is as the thermal source of lightness-removing column second reboiler E-10003, and tower top obtains concentrated rear rare formaldehyde (concentration 37wt%) and returns formaldehyde plant, improves the transformation efficiency of formaldehyde.Tower reactor formaldehyde in waste water is removed to lower than 1ppm, after merging with the waste water from product tower after gaseous effluent cooler E-10007 cools decontaminated water treatment unit.
Embodiment 2,
A kind of clean diesel fuel additive polymethoxy methylal separation method,
Comprise the following steps:
(1) the synthesis crude product from upstream reaction system delivers to the removal of lightness-removing column system methyl alcohol, formaldehyde, DMM wherein
1 ~ 2light constituent, the light constituent of overhead extraction removes methanol distillation column, and the thick DMMn product of tower reactor goes to product Tower System;
(2) in product Tower System, remove the water in the thick DMMn product of charging, overhead extraction containing micro-DMM
2 ~ 3waste water goes to waste disposal plant, and tower bottoms obtains satisfactory polymethoxy methylal product DMM after cooling
3 ~ 8;
(3) Methanol Recovery Tower System fully reclaims unreacted methyl alcohol, and the recovery methyl alcohol of overhead extraction returns the reactive system recycle of upstream, and the rare formaldehyde of tower reactor delivers to rare aldehyde upgrading tower system in downstream;
(4) rare aldehyde upgrading tower system concentrates rare aldehyde, and concentration 36.5 ~ 37.4% formaldehyde solution that tower top obtains goes to formaldehyde plant or tank field, and tower reactor goes to waste disposal plant containing trace formaldehyde waste water after water cooler cooling.
Described lightness-removing column adopts high-low pressure thermal coupling distillation technology, lightness-removing column adopts two kinds of thermals source, wherein lightness-removing column first reboiler adopts steam or other thermals source, lightness-removing column second reboiler adopts the overhead vapours of rare aldehyde upgrading tower as thermal source, adopts thermal coupling methods to reduce rectifier unit comprehensive energy consumption.
Described product tower have employed tower reactor reboiler and intermediate reboiler, and wherein product tower tower reactor reboiler adopts the thermal source of GOOD TASTE, and product tower intermediate reboiler adopts the thermal source of low taste.
Wherein lightness-removing column number of theoretical plate 20 ~ 100 pieces, working pressure normal pressure ~ 0.5MPaG; Product tower number of theoretical plate 30 ~ 100 pieces, working pressure-0.09 ~ 0.3MPaG; Methanol distillation column number of theoretical plate 15 ~ 60 pieces, working pressure normal pressure ~ 0.5MPaG; Rare aldehyde upgrading tower theoretical stage 20 ~ 80 pieces, working pressure normal pressure ~ 1.0MPaG.
Described lightness-removing column system comprises lightness-removing column, lightness-removing column first reboiler, lightness-removing column second reboiler, condenser of light component removal column, lightness-removing column return tank, lightness-removing column reflux pump, product tower fresh feed pump;
Described product Tower System comprises product tower, product tower reboiler, product tower intermediate reboiler, product transferpump and product tower condenser, product tower return tank, product tower reflux pump, reactor product cooler;
Described Methanol Recovery Tower System comprises methanol distillation column, methanol distillation column reboiler, methanol distillation column reflux pump, methanol distillation column condenser and methanol distillation column return tank, rare aldehyde upgrading tower fresh feed pump;
Described rare aldehyde upgrading tower system comprises rare aldehyde upgrading tower, rare aldehyde upgrading tower reboiler, gaseous effluent cooler, rare aldehyde upgrading tower return tank, rare aldehyde upgrading tower reflux pump, waste water transferpump.
Polymethoxy methylal separation method described in the present embodiment comprises following unit:
1) lightness-removing column system
Lightness-removing column C-10001 is mainly used in removing in synthesis crude product and compares DMM
3low-boiling light constituent (methyl alcohol, formaldehyde, DMM
1 ~ 2and part water), reclaim DMM in synthesis crude product as far as possible simultaneously
3 ~ 10.Lightness-removing column overhead vapours removes lightness-removing column return tank V-10001 after condenser of light component removal column E-10001 condensation, and phegma removes methanol distillation column C-10003 through lightness-removing column reflux pump P-10001A/B boosting rear section extraction, and all the other are as backflow.Lightness-removing column adopts two kinds of thermals source, and wherein lightness-removing column first reboiler E-10002 adopts steam or other thermals source, and lightness-removing column second reboiler E-10003 adopts the overhead vapours of rare aldehyde upgrading tower as thermal source, to reduce the consumption of device.The thick product of lightness-removing column tower reactor send derived product tower C-10002 after product tower fresh feed pump P-10002A/B boosts.
2) product Tower System
Product tower C-10002 is used for removing water in the thick product of lightness-removing column C-10001 tower reactor, to ensure DMM
nin product, water-content is lower than water-content standard in diesel oil.Product tower C-10002 overhead vapours removes product tower return tank V-10002 after product tower condenser E-10004 condensation.Phegma removes gaseous effluent cooler E-10007 through product tower reflux pump P-10003A/B boosting rear section extraction, and all the other are as backflow.Product tower also adopts the thermal source of two kinds of different tastes, and wherein product tower reboiler E-10006 adopts the thermal source of GOOD TASTE, and product tower intermediate reboiler E-10005 adopts the thermal source of low taste.Product tower tower reactor DMMn product delivers to tank field through reactor product cooler E-10007 after product transferpump P-10004A/B boosts.
3) Methanol Recovery Tower System
Methanol distillation column C-10003, for reclaiming unreacted methyl alcohol and a small amount of formaldehyde, reclaims methyl alcohol Returning reacting system after pump boosting, to improve the transformation efficiency of methyl alcohol.Methanol distillation column C-10003 overhead vapours removes methanol distillation column return tank V-10003 after methanol distillation column condenser E-10008 condensation.Phegma is through methanol distillation column reflux pump boosting rear section extraction Returning reacting system, and all the other are as backflow.Thermal source needed for methanol distillation column is separated provides by methanol distillation column reboiler E-10009, and tower reactor rare aldehyde liquid delivers to rare aldehyde upgrading tower C-10004 after rare aldehyde upgrading tower fresh feed pump boosting.
4) rare aldehyde upgrading tower system
Rare formaldehyde of methanol distillation column tower reactor concentrates by rare aldehyde upgrading tower C-10004, and after concentrated, formaldehyde solution (concentration ~ 37wt%) returns formaldehyde plant, improves the transformation efficiency of formaldehyde, is removed to by formaldehyde in waste water simultaneously and reaches wastewater discharge standard.Rare aldehyde upgrading tower C-10004 overhead vapours removes rare aldehyde upgrading tower return tank V-10004 after lightness-removing column second reboiler E-10002 condensation.Phegma goes to formaldehyde plant or tank field through rare aldehyde upgrading tower reflux pump P-10007A/B boosting rare formaldehyde extraction in rear section, and all the other are as backflow.Thermal source needed for rare aldehyde upgrading tower is separated provides by rare aldehyde upgrading tower reboiler E-10010, tower reactor waste water after waste water transferpump P-10008A/B boosts, after merging with the waste water from product tower after gaseous effluent cooler E-10007 cools decontaminated water treatment unit.
Claims (5)
1. a clean diesel fuel additive polymethoxy methylal separation method, is characterized in that:
Comprise the following steps:
(1) the synthesis crude product from upstream reaction system delivers to the removal of lightness-removing column system methyl alcohol, formaldehyde, DMM wherein
1 ~ 2light constituent, the light constituent of overhead extraction removes methanol distillation column, and the thick DMMn product of tower reactor goes to product Tower System;
(2) in product Tower System, remove the water in the thick DMMn product of charging, overhead extraction containing micro-DMM
2 ~ 3waste water goes to waste disposal plant, and tower bottoms obtains satisfactory polymethoxy methylal product DMM after cooling
3 ~ 8;
(3) Methanol Recovery Tower System fully reclaims unreacted methyl alcohol, and the recovery methyl alcohol of overhead extraction returns the reactive system recycle of upstream, and the rare formaldehyde of tower reactor delivers to rare aldehyde upgrading tower system in downstream;
(4) rare aldehyde upgrading tower system concentrates rare aldehyde, and concentration 36.5 ~ 37.4% formaldehyde solution that tower top obtains goes to formaldehyde plant or tank field, and tower reactor goes to waste disposal plant containing trace formaldehyde waste water after water cooler cooling.
2. a kind of clean diesel fuel additive polymethoxy methylal separation method according to claim 1, it is characterized in that: described lightness-removing column adopts high-low pressure thermal coupling distillation technology, lightness-removing column adopts two kinds of thermals source, wherein lightness-removing column first reboiler adopts steam or other thermals source, lightness-removing column second reboiler adopts the overhead vapours of rare aldehyde upgrading tower as thermal source, adopts thermal coupling methods to reduce rectifier unit comprehensive energy consumption.
3. a kind of clean diesel fuel additive polymethoxy methylal separation method according to claim 1, it is characterized in that: described product tower have employed tower reactor reboiler and intermediate reboiler, wherein product tower tower reactor reboiler adopts the thermal source of GOOD TASTE, and product tower intermediate reboiler adopts the thermal source of low taste.
4. a kind of clean diesel fuel additive polymethoxy methylal separation method according to claim 1, is characterized in that: wherein lightness-removing column number of theoretical plate 20 ~ 100 pieces, working pressure normal pressure ~ 0.5MPaG; Product tower number of theoretical plate 30 ~ 100 pieces, working pressure-0.09 ~ 0.3MPaG; Methanol distillation column number of theoretical plate 15 ~ 60 pieces, working pressure normal pressure ~ 0.5MPaG; Rare aldehyde upgrading tower theoretical stage 20 ~ 80 pieces, working pressure normal pressure ~ 1.0MPaG.
5. a kind of clean diesel fuel additive polymethoxy methylal separation method according to claim 1, is characterized in that:
Described lightness-removing column system comprises lightness-removing column, lightness-removing column first reboiler, lightness-removing column second reboiler, condenser of light component removal column, lightness-removing column return tank, lightness-removing column reflux pump, product tower fresh feed pump;
Described product Tower System comprises product tower, product tower reboiler, product tower intermediate reboiler, product transferpump and product tower condenser, product tower return tank, product tower reflux pump, reactor product cooler;
Described Methanol Recovery Tower System comprises methanol distillation column, methanol distillation column reboiler, methanol distillation column reflux pump, methanol distillation column condenser and methanol distillation column return tank, rare aldehyde upgrading tower fresh feed pump;
Described rare aldehyde upgrading tower system comprises rare aldehyde upgrading tower, rare aldehyde upgrading tower reboiler, gaseous effluent cooler, rare aldehyde upgrading tower return tank, rare aldehyde upgrading tower reflux pump, waste water transferpump.
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