CN110003007A - Coal-ethylene glycol carbonylation dimethyl oxalate rectifying and purifying system and method - Google Patents
Coal-ethylene glycol carbonylation dimethyl oxalate rectifying and purifying system and method Download PDFInfo
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- CN110003007A CN110003007A CN201910388744.8A CN201910388744A CN110003007A CN 110003007 A CN110003007 A CN 110003007A CN 201910388744 A CN201910388744 A CN 201910388744A CN 110003007 A CN110003007 A CN 110003007A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/36—Preparation of carboxylic acid esters by reaction with carbon monoxide or formates
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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Abstract
The present invention relates to one kind, and dimethyl oxalate product purity can be improved, it reduces energy consumption and saves the coal-ethylene glycol carbonylation dimethyl oxalate rectifying and purifying system and method for production cost, including dimethyl oxalate feed exchanger, the vacuum rectifying tower being connected with dimethyl phthalate feed exchanger, tower reactor bottom is equipped with reboiler, overhead condenser is connected by evaporation vapor outlet port with rectification under vacuum top of tower, overhead condenser is connected with return tank and tail cooler respectively, return tank is connected with reflux pump, reflux pump is connected with rectification under vacuum column overhead and overhead extraction flow control valve；Rectifying column bottom, which is connected, heavy constituent discharging pump, and heavy constituent discharging pump is connected by pipeline and tower reactor Liquid level adjusting valve through dimethyl oxalate feed exchanger and tower reactor discharge port；Return flow regulating valve is set on reflux pump outlet conduit, the light component impurity in dimethyl oxalate mixed liquor is removed, the dimethyl oxalate intermediate products of high-purity are obtained；Vacuumizing reduces the boiling point of each component, reduces middle pressure steam consumption, reduces cost, tower reactor component and tower top light component continuously produce, and realize heat and material effective recycling, do not have outlet material.
Description
Technical field
The invention belongs to coal-ethylene glycol chemical fields more particularly to one kind, and dimethyl oxalate product purity can be improved,
It reduces energy consumption and saves the coal-ethylene glycol carbonylation dimethyl oxalate rectifying and purifying system and method for production cost.
Background technique
Ethylene glycol is a kind of important industrial chemicals, is mainly used as the original of solvent, antifreezing agent and synthesis polyester resin etc.
Material.Currently, ethylene glycol mainly uses ethylene oxide direct hydration method to prepare.Since the preparation of ethylene oxide is with ethylene for original
Material, mass production depend on petroleum resources.And the total energy feature in China is rich coal, has gas, few oil, therefore coal is efficient
The industrial chemicals such as ethylene glycol are converted into, dependence of the industrial chemicals to petroleum resources is reduced, are conducive to optimize the energy, resource structures,
Have great importance.
In recent years, with the gradually maturation of coal-ethylene glycol technology, the country has built large quantities of coal-ethylene glycol enterprises.
According to reliable statistics, in the coming years, the production capacity of China's coal-ethylene glycol is up to 8,000,000 tons or more.Dimethyl oxalate is coal system
Intermediate product in ethylene glycol production process is prepared by carbonylation reaction, and carbonylation system response is complicated, main
Wanting target product is dimethyl oxalate, wherein there are also a series of side reactions, product includes dimethyl carbonate, methyl formate, second
Sour methyl esters etc. causes larger negative effect to follow-up hydrogenation process catalyst, causes because impurity composition is various and complicated in product
The problems such as catalyst bed layer resistance is high, the service life is short, therefore, for the effective run time for guaranteeing hydrogenation catalyst, reduction is produced into
This, it is necessary to the target product for being refining to obtain high-purity is carried out to dimethyl oxalate product.Current processing method uses often substantially
Atmospheric distillation, compression rectification or the extraction and distillation technology of rule have the drawback that product purity is not high, energy consumption is high, using subtracting
Rectification under vacuum technology is pressed, not only the dimethyl oxalate product of available high-purity, but also plant energy consumption reduces, and has saved device
Production cost.
Summary of the invention
It is an object of the invention to solve in above-mentioned coal-ethylene glycol production process existing in the prior art because carbonylation closes
A kind of consumption reduction, purification, extension plus the hydrogen provided at the low problem of target product dimethyl oxalate purity caused by side reaction is urged
The coal-ethylene glycol carbonylation dimethyl oxalate rectifying and purifying system and method for agent Acceptable life.
To achieve the goals above, present invention employs such technical solutions:
A kind of coal-ethylene glycol carbonylation dimethyl oxalate rectifying and purifying system, including dimethyl oxalate feed exchanger, with
The vacuum rectifying tower that dimethyl phthalate feed exchanger is connected is provided with reboiler in the tower reactor bottom of vacuum rectifying tower, then boils
The fluid inlet of device and the bottom connection of vacuum rectifying tower are logical, the liquid-phase outlet of reboiler and phase above the bottom of vacuum rectifying tower
It connects；Promising vacuum rectifying tower is opened up at the top of vacuum rectifying tower, and the evaporation vapor outlet port of upflowing vapor, overhead condensation are provided
Device by evaporation vapor outlet port and vacuum rectifying tower at the top of is connected, overhead condenser further through pipeline respectively with return tank and
Tail cooler is connected, and mutually connects again between return tank and tail cooler, and condensate liquid is fallen after rise using gravity to return tank, fixed gas warp
Tail cooler is extracted out by vacuum equipment, and return tank is connected with reflux pump, and reflux pump passes through the tower top of pipeline and vacuum rectifying tower
It is connected, while being also connected by pipeline and overhead extraction flow control valve；The pressure of distillation system by with vacuum equipment
The vacuum degree regulating valve being connected is adjusted；The liquid phase of return tank returns to the tower of vacuum rectifying tower by reflux pump a part
Top, another part adjust extraction system with liquid level through overhead extraction flow control valve and are connected；In the rectifying column of vacuum rectifying tower
There is heavy constituent discharging pump at bottom by pipeline connection, and heavy constituent discharging pump is by pipeline and tower reactor Liquid level adjusting valve through dimethyl oxalate
Feed exchanger and tower reactor discharge port are connected；Dimethyl oxalate feed exchanger use rectifying heat coupling principle, by low temperature into
Expect that dimethyl oxalate liquid phase and the pure dimethyl oxalate discharging of tower reactor high temperature exchange heat, improves feeding temperature, reduce drop temperature；It returns
Flow and return flow regulating valve be set on the outlet conduit of pump, for adjusting distillation operation reflux ratio, stablize tower top operation temperature and
Overhead extraction flow control valve is arranged in product quality, controls return tank level stability by adjusting produced quantity；Vacuum equipment import
Vacuum degree regulating valve is set on pipeline and is stablized by adjusting vacuum equipment air inflow control Rectification column pressure.
Upflowing vapor needed for the reboiler heat source provides rectifying using middle pressure steam heating, according to processing payload
Stablize by adjusting steam addition control rectifying tower reactor constant.
The dimethyl oxalate feed exchanger additionally increase heat supply, using charging with vacuum rectifying tower discharge into
Row heat exchange.
Vacuum system is setting vacuum equipment, keeps certain vacuum degree in rectifying column and return tank, drop using vacuum suction
The boiling point of low each component saves the steam investment of reboiler.
The return-flow system is one of the requirement that distillation process occurs, and light component is cooling through condenser and tail cooler,
Lime set reaches certain temperature and is recovered to return tank, partially realizes mass transfer and diabatic process, another part as the reflux of rectifying column
It is produced as overhead product, and system is reused back to before synthesizing.
The vacuum rectifying tower is capital equipment, is provided with tower tray and packing layer inside it, in certain vacuum degree condition
Under, multiple mass transfer and diabatic process occur for upflowing vapor and dropping liq, realize the purification of dimethyl oxalate product, purified product
Extraction system is pumped by kettle liquid.
A method of it is purified using the coal-ethylene glycol carbonylation dimethyl oxalate rectifying and purifying system,
This method comprises: vacuum system will keep vacuum degree in vacuum rectifying tower using vacuum equipment, vacuum rectifying tower internal pressure is made to try hard to keep
It holds in 40~70KPa vacuum degree, low temperature feeds the pure dimethyl oxalate of high temperature of dimethyl oxalate liquid phase feeding and rectifying tower reactor
After discharging heat exchange, being fed between rectifying column rectifying section and stripping section, the reboiler heated material through tower reactor becomes upflowing vapor,
After rectifying section inversely contacts progress mass transfer and heat transfer exchange with overhead reflux, steam enters overhead condenser and tail cooler, will
Tower top upflowing vapor, which first passes through overhead condenser partial gas phase material is condensed into liquid phase, to be flowed in return tank, uncooled part gas
Mutually using tail cooler, condensate liquid is fallen after rise to return tank, and fixed gas is handled through vacuum equipment；Return tank inner condensat liquid passes through reflux
Pump a part returns to tower top as flowing back, and a part extraction distillation system, tower reactor extraction purification dimethyl oxalate is pumped through kettle liquid
To intermediate products storage tank, supplies hydrogenation system charging and use；
It is provided with tower reactor Liquid level adjusting valve on pipeline after the heavy constituent discharging pump of the vacuum rectifying tower, by adjusting load control
Rectifying tower reactor level stability processed；Return flow regulating valve is set on reflux pump outlet conduit, for adjusting distillation operation reflux ratio,
Stablize tower top operation temperature and product quality；Overhead extraction flow control valve is set, controls return tank liquid by adjusting produced quantity
Stablize position；Vacuum degree regulating valve is set on vacuum equipment inlet pipeline, controls rectifying column pressure by adjusting vacuum equipment air inflow
Power is stablized；
The heat source of reboiler uses middle pressure steam, steady by adjusting steam addition control rectifying tower reactor according to processing payload
It is fixed constant.
The dimethyl oxalate feed composition is dimethyl oxalate content >=95%, and methanol content≤4%, dimethyl carbonate contains
Amount≤1%；The dimethyl oxalate feeding temperature control is 120~140 DEG C；The reboiler temperature control is 130~160 DEG C；
The tower top temperature control is 45~60 DEG C；Tail cooler process stream outlet temperature≤30 DEG C；The rectifying tower vacuum degree
Control is 40~70KPa；The rectifying column Liquid level is 30~80%；The return tank Liquid level is 20~80%；It is described
It is 0 that tower top light component group, which becomes dimethyl oxalate content, methanol content >=50%, DMC addition≤50%；The tower reactor
Product extraction group becomes dimethyl oxalate content >=99.9%, methanol content≤0.1%, DMC addition 0.
The good effect that technical solution of the present invention generates is as follows: disclosed by the invention is a kind of coal-ethylene glycol carbonylation conjunction
At dimethyl oxalate rectifying and purifying system and method, by the way of rectification under vacuum, by light group in dimethyl oxalate mixed liquor
Divide impurity removal, obtains the dimethyl oxalate intermediate products of high-purity；Vacuumizing reduces the boiling point of each component simultaneously, in reduction
Steam consumption is pressed, production cost is reduced, improves the market competitiveness；Tower reactor component and tower top light component continuously produce, and realize heat
Amount and material effective recycling, do not have outlet material.
The system and method for dimethyl oxalate rectification and purification technique of the invention pass through practice operation, greatly solve coal
Preparing ethylene glycol production process dimethyl oxalate in preparation purity is low, the problem more than objectionable impurities, to extending effectively making for hydrogenation catalyst
There is very big benifit with the service life；Simultaneously for producing 200000 tons of glycol units per year, reduces middle pressure steam and consume 8 tons/h, steam list
Valence presses 160 yuan/ton, and the cycle of operation in year calculated by 8000 hours, can save 10,240,000 yuan of steam cost every year.
Detailed description of the invention
Fig. 1 is the attachment structure schematic diagram of coal-ethylene glycol carbonylation dimethyl oxalate rectifying and purifying system of the present invention.
It is marked in figure are as follows: 1. dimethyl oxalate feed exchangers；2. vacuum rectifying tower；3. reboiler；4. overhead condensation
Device；5. tail cooler；6. return tank；7. reflux pump；8. kettle liquid discharging pump；9. tower reactor Liquid level adjusting valve；10. return flow is adjusted
Valve；11. overhead extraction flow control valve；12. vacuum degree regulating valve.
Specific embodiment
Combined with specific embodiments below and attached drawing is further elaborated and illustrates to the present invention.
As shown in Figure 1, a kind of coal-ethylene glycol carbonylation dimethyl oxalate rectifying and purifying system, including dimethyl oxalate
Feed exchanger 1, the vacuum rectifying tower 2 being connected with dimethyl phthalate feed exchanger 1, in the tower reactor bottom of vacuum rectifying tower 2
Be provided with reboiler 3, the fluid inlet of reboiler 3 and the bottom connection of vacuum rectifying tower 2 are logical, the liquid-phase outlet of reboiler 3 with
It is connected above the bottom of vacuum rectifying tower 2；Promising vacuum rectifying tower is opened up at the top of vacuum rectifying tower 2, and upflowing vapor is provided
Evaporation vapor outlet port, overhead condenser 4 by evaporation vapor outlet port and the top of vacuum rectifying tower 2 be connected, overhead condensation
Device 4 is connected with return tank 6 and tail cooler 5 respectively further through pipeline, mutually connects again between return tank 6 and tail cooler 5, condensation
Liquid is fallen after rise using gravity to return tank 6, and fixed gas is extracted out through tail cooler 5 by vacuum equipment, and return tank 6 connects with reflux pump 7
Logical, reflux pump 7 is connected by the tower top of pipeline and vacuum rectifying tower 2, while also being adjusted by pipeline and overhead extraction flow
Valve 11 is connected；The pressure of distillation system is adjusted by the vacuum degree regulating valve 12 being connected with vacuum equipment；Return tank 6
Liquid phase return to the tower top of vacuum rectifying tower 2 by a part of reflux pump 7, another part through overhead extraction flow control valve 11 with
Liquid level adjusts extraction system and is connected；There is heavy constituent discharging pump 8 by pipeline connection at the rectifying column bottom of vacuum rectifying tower 2, weight
Component discharging pump 8 is connected by pipeline and tower reactor Liquid level adjusting valve 9 through dimethyl oxalate feed exchanger 1 and tower reactor discharge port,
Dimethyl oxalate feed exchanger 1 uses rectifying heat coupling principle, by low temperature charging dimethyl oxalate liquid phase and tower reactor high temperature
Pure dimethyl oxalate discharging heat exchange, improves feeding temperature, reduces drop temperature；Reflux is set on the outlet conduit of reflux pump 7
Flow control valve 10 stablizes tower top operation temperature and product quality, the extraction of tower top setting for adjusting distillation operation reflux ratio
Flow control valve 11 controls return tank level stability by adjusting produced quantity；Vacuum degree is arranged on vacuum equipment inlet pipeline to adjust
Valve 12 is simultaneously stablized by adjusting vacuum equipment air inflow control Rectification column pressure.
Upflowing vapor needed for the reboiler heat source provides rectifying using middle pressure steam heating, according to processing payload
Stablize by adjusting steam addition control rectifying tower reactor constant.
The dimethyl oxalate feed exchanger additionally increase heat supply, using charging with vacuum rectifying tower discharge into
Row heat exchange.
Vacuum system is setting vacuum equipment, keeps certain vacuum degree in rectifying column and return tank, drop using vacuum suction
The boiling point of low each component saves the steam investment of reboiler.
The return-flow system is one of the requirement that distillation process occurs, and light component is cooling through condenser and tail cooler,
Lime set reaches certain temperature and is recovered to return tank, partially realizes mass transfer and diabatic process, another part as the reflux of rectifying column
It is produced as overhead product, and system is reused back to before synthesizing.
The vacuum rectifying tower is capital equipment, is provided with tower tray and packing layer inside it, in certain vacuum degree condition
Under, multiple mass transfer and diabatic process occur for upflowing vapor and dropping liq, realize the purification of dimethyl oxalate product, purified product
Extraction system is pumped by kettle liquid.
A kind of coal-ethylene glycol carbonylation product dimethyl oxalate rectifying and purifying system, including vacuum rectifying tower 2, oxalic acid
Dimethyl ester feed exchanger 1, vacuum system, vapo(u)rization system and condensing reflux system, the dimethyl oxalate feeding preheating are main
Purpose is to improve feeding temperature, reduces steam consumption, and the method that the preheating of preceding system recycles can be used, no longer additional to increase
Energy consumption；The vacuum system will keep certain vacuum degree using vacuum equipment in rectifying column, reduce liquid phase component boiling point, drop
Low operating temperature reduces steam consumption；The vapo(u)rization system be rectifying tower reactor setting reboiler 3 be rectifying tower top provide rising steaming
Vapour；The condensing reflux system is tower top setting overhead condenser 4 and tail cooler 5, and it is cold that tower top upflowing vapor is first passed through tower top
Partial gas phase material is condensed into liquid phase and flowed in return tank 6 by condenser 4, and uncooled partial gas phase is using tail cooler 5, condensate liquid
It falls after rise to return tank 6, fixed gas is handled through vacuum equipment.Its main operational principle are as follows: oxalic acid two is passed through in dimethyl oxalate charging
The preheating of methyl esters feed exchanger 1 enters vacuum rectifying tower 2, and liquid phase flashes to upflowing vapor after the heating of reboiler 3, sprays with tower top
The phegma of stream carries out heat exchange, and light component gas phase is cooling through condenser from tower top, and condensate liquid falls after rise to return tank 6, do not coagulate
Light component gas phase is cooling through tail cooler 5 again, and condensation liquid phase is fallen after rise to return tank 6, and fixed gas is through vacuum equipment pump-and-treat system, vacuum
Equipment controls the vacuum degree of rectifying column, and 6 inner condensat liquid of return tank returns to tower top as reflux, a part by reflux pump a part
Distillation system is produced, tower reactor extraction purification dimethyl oxalate is pumped to product storage tank through kettle liquid, and supply hydrogenation system charging uses.
Dimethyl oxalate feed exchanger described above does not increase heat supply additionally, is gone out using charging with vacuum rectifying tower
Material exchanges heat, and reaches raising feeding temperature, reduces steam investment, reduces the purpose of drop temperature, saves production cost.
Above-mentioned vacuum system is setting vacuum equipment, keeps certain vacuum in rectifying column and return tank using vacuum suction
Degree, reduces the boiling point of each component, saves the steam investment of reboiler.
Above-mentioned vapo(u)rization system is rectification under vacuum tower reactor setting reboiler, is heated using middle pressure steam upper needed for providing rectifying
Rise steam.
Above-mentioned return-flow system is one of the requirement that distillation process occurs, and light component is cooling through condenser and tail cooler,
Lime set reaches certain temperature and is recovered to return tank, partially realizes mass transfer and diabatic process, another part as the reflux of rectifying column
It is produced as overhead product, and system is reused back to before synthesizing.
Above-mentioned vacuum rectifying tower is capital equipment, is provided with tower tray and packing layer inside it, in certain vacuum degree condition
Under, multiple mass transfer and diabatic process occur for upflowing vapor and dropping liq, realize the purification of dimethyl oxalate product, purified product
Extraction system is pumped by kettle liquid.
Embodiment 1:
The system of coal-ethylene glycol carbonylation product dimethyl oxalate rectification and purification technique, as shown in Figure 1, including oxalic acid diformazan
Ester feed exchanger 1, vacuum rectifying tower 2, reboiler 3, overhead condenser 4, tail cooler 5, return tank 6, reflux pump 7, heavy constituent
Discharging pump 8, tower reactor Liquid level adjusting valve 9, return flow regulating valve 10, overhead extraction flow control valve 11, vacuum degree regulating valve 12.
The vacuum rectifying tower be distillation operation one of capital equipment, tower reactor be arranged reboiler, reboiler liquid phase into
Mouth is connected with rectifier bottoms, and evaporation vapor outlet port is connected with rectifying tower reactor top, provides upflowing vapor for rectifying column；Tower reactor goes out
Material pump is connected with rectifying column bottom, controls extraction flow by index combustion fan；Feed exchanger uses rectifying heat coupling principle,
Low temperature charging dimethyl oxalate liquid phase and the pure dimethyl oxalate discharging of tower reactor high temperature are exchanged heat, feeding temperature is improved, reduces
Drop temperature；It is connected at the top of overhead condenser and rectifying column, rectifying column steam exchanges heat through condenser and recirculated water, and condensate liquid utilizes
Gravity drops down onto return tank, and uncooled gas phase exchanges heat through tail cooler and chilled water again, and condensate liquid is fallen after rise using gravity to return tank, no
Solidifying gas is extracted out through vacuum equipment, and the pressure of distillation system is adjusted by vacuum equipment；Return tank liquid phase passes through reflux pump one
Divide and return to the top of the distillation column, a part adjusts extraction system through liquid level.
Liquid level adjusting valve is set on pipeline after the tower bottom of rectifying tower discharging pump, controls rectifying tower reactor by adjusting load
Level stability.Return flow regulating valve is set on reflux pump outlet conduit, for adjusting distillation operation reflux ratio, stablizes tower top behaviour
Make temperature and product quality, setting tower top light component produces flow control valve, steady by adjusting produced quantity control return tank liquid level
It is fixed.Pressure-regulating valve is set on vacuum equipment inlet pipeline, is stablized by adjusting vacuum equipment air inflow control Rectification column pressure.
The reboiler heat source uses middle pressure steam, controls rectifying according to processing payload by adjusting steam addition
Tower reactor is stablized constant.
The dimethyl oxalate feed composition is dimethyl oxalate content >=95%, and methanol content≤4%, dimethyl carbonate contains
Amount≤1%.
The dimethyl oxalate feeding temperature control is 120~140 DEG C.
The reboiler temperature control is 130~160 DEG C.
The tower top temperature control is 45~60 DEG C.
Tail cooler process stream outlet temperature≤30 DEG C.
The rectifying tower vacuum degree control is 40~70KPa.
The rectifying column Liquid level is 30~80%.
The return tank Liquid level is 20~80%.
It is 0 that the tower top light component group, which becomes dimethyl oxalate content, methanol content >=50%, DMC addition≤
50%。
The tower reactor product extraction group becomes dimethyl oxalate content >=99.9%, methanol content≤0.1%, dimethyl carbonate
Content is 0.
Claims (8)
1. a kind of coal-ethylene glycol carbonylation dimethyl oxalate rectifying and purifying system, including dimethyl oxalate feed exchanger
(1), the vacuum rectifying tower (2) being connected with dimethyl phthalate feed exchanger (1), it is characterised in that: in vacuum rectifying tower (2)
Tower reactor bottom is provided with reboiler (3), and the fluid inlet of reboiler (3) and the bottom connection of vacuum rectifying tower (2) are logical, reboiler
(3) it is connected above liquid-phase outlet and the bottom of vacuum rectifying tower (2)；It is opened up at the top of vacuum rectifying tower (2) promising true
Empty rectifying column provides the evaporation vapor outlet port of upflowing vapor, and overhead condenser (4) passes through evaporation vapor outlet port and vacuum rectifying tower
(2) it is connected at the top of, overhead condenser (4) is connected with return tank (6) and tail cooler (5) respectively further through pipeline, reflux
It is mutually connected again between tank (6) and tail cooler (5), condensate liquid is fallen after rise using gravity to return tank (6), and fixed gas is through tail cooler
(5) it is extracted out by vacuum equipment, return tank (6) is connected with reflux pump (7), and reflux pump (7) passes through pipeline and vacuum rectifying tower
(2) tower top is connected, while being also connected by pipeline with overhead extraction flow control valve (11)；The pressure of distillation system is logical
The vacuum degree regulating valve (12) being connected with vacuum equipment is crossed to be adjusted；The liquid phase of return tank (6) passes through reflux pump (7) one
Divide the tower top for returning to vacuum rectifying tower (2), another part adjusts extraction system through overhead extraction flow control valve (11) and liquid level
It is connected；Have heavy constituent discharging pump (8) at the rectifying column bottom of vacuum rectifying tower (2) by pipeline connection, heavy constituent discharging pump (8)
It is connected by pipeline and tower reactor Liquid level adjusting valve (9) through dimethyl oxalate feed exchanger (1) and tower reactor discharge port, oxalic acid diformazan
Ester feed exchanger (1) uses rectifying heat coupling principle, by low temperature charging dimethyl oxalate liquid phase and the pure grass of tower reactor high temperature
Dimethyl phthalate discharging heat exchange, improves feeding temperature, reduces drop temperature；Return flow is set on the outlet conduit of reflux pump (7)
Regulating valve (10) stablizes tower top operation temperature and product quality, the extraction stream of tower top setting for adjusting distillation operation reflux ratio
Adjustable valve (11) controls return tank level stability by adjusting produced quantity；Vacuum degree is arranged on vacuum equipment inlet pipeline to adjust
Valve (12) is simultaneously stablized by adjusting vacuum equipment air inflow control Rectification column pressure.
2. coal-ethylene glycol carbonylation product dimethyl oxalate rectifying and purifying system according to claim 1, feature
It is: upflowing vapor needed for the reboiler heat source provides rectifying using middle pressure steam heating is logical according to processing payload
Cross adjustment steam addition control rectifying tower reactor stablize it is constant.
3. coal-ethylene glycol carbonylation product dimethyl oxalate rectifying and purifying system according to claim 1, feature
Be: the dimethyl oxalate feed exchanger does not increase heat supply additionally, is carried out using charging and vacuum rectifying tower discharging
Heat exchange.
4. coal-ethylene glycol carbonylation product dimethyl oxalate rectifying and purifying system according to claim 1, feature
Be: vacuum system is setting vacuum equipment, keeps certain vacuum degree in rectifying column and return tank using vacuum suction, is reduced each
The boiling point of component saves the steam investment of reboiler.
5. coal-ethylene glycol carbonylation product dimethyl oxalate rectifying and purifying system according to claim 1, feature
Be: the return-flow system is one of the requirement that distillation process occurs, and light component is cooling through condenser and tail cooler, lime set
Reach certain temperature and be recovered to return tank, partially realizes mass transfer and diabatic process, another part conduct as the reflux of rectifying column
Overhead product extraction, and system is reused back to before synthesizing.
6. coal-ethylene glycol carbonylation product dimethyl oxalate rectifying and purifying system according to claim 1, feature
Be: the vacuum rectifying tower is capital equipment, is provided with tower tray and packing layer inside it, under the conditions of certain vacuum degree,
Multiple mass transfer and diabatic process occur for upflowing vapor and dropping liq, realize the purification of dimethyl oxalate product, and purified product is logical
Cross kettle liquid pump extraction system.
7. a kind of purified using coal-ethylene glycol carbonylation dimethyl oxalate rectifying and purifying system described in claim 1
Method, it is characterised in that: this method comprises: vacuum system will keep vacuum degree in vacuum rectifying tower (2) using vacuum equipment,
Vacuum rectifying tower (2) internal pressure power is set to be maintained at 40~70KPa vacuum degree, low temperature feeds dimethyl oxalate liquid phase feeding and rectifying column
After the pure dimethyl oxalate discharging heat exchange of the high temperature of kettle, fed between rectifying column rectifying section and stripping section, boiling again through tower reactor
Device (3) heated material becomes upflowing vapor, after rectifying section inversely contacts progress mass transfer and heat transfer exchange with overhead reflux, steam
Into overhead condenser (4) and tail cooler (5), tower top upflowing vapor is first passed through into overhead condenser (4) for partial gas phase material
It is condensed into liquid phase to flow in return tank (6), uncooled partial gas phase is fallen after rise using tail cooler (5), condensate liquid to return tank
(6), fixed gas is handled through vacuum equipment；Return tank (6) inner condensat liquid returns to tower top by reflux pump (7) a part and is used as back
Stream, a part extraction distillation system, tower reactor extraction purification dimethyl oxalate are pumped to intermediate products storage tank, supply plus hydrogen through kettle liquid
System feeding uses；
The heavy constituent discharging pump (8) of the vacuum rectifying tower (2) is provided with tower reactor Liquid level adjusting valve (9) on pipeline afterwards, passes through tune
Whole load controls rectifying tower reactor level stability；Return flow regulating valve (10) are set on reflux pump outlet conduit, for adjusting
Distillation operation reflux ratio stablizes tower top operation temperature and product quality；It is arranged overhead extraction flow control valve (11), by adjusting
Produced quantity controls return tank level stability；Vacuum degree regulating valve (12) are set on vacuum equipment inlet pipeline, by adjusting vacuum
Equipment air inflow controls Rectification column pressure and stablizes；
The heat source of reboiler (3) uses middle pressure steam, controls rectifying column according to processing payload by adjusting steam addition
Kettle is stablized constant.
8. coal-ethylene glycol carbonylation product dimethyl oxalate rectification and purification method according to claim 7, feature
Be: the dimethyl oxalate feed composition is dimethyl oxalate content >=95%, methanol content≤4%, DMC addition
≤1%；The dimethyl oxalate feeding temperature control is 120~140 DEG C；The reboiler temperature control is 130~160 DEG C；Institute
Stating tower top temperature control is 45~60 DEG C；Tail cooler process stream outlet temperature≤30 DEG C；The rectifying tower vacuum degree control
It is made as 40~70KPa；The rectifying column Liquid level is 30~80%；The return tank Liquid level is 20~80%；The tower
Pushing up light component group to become dimethyl oxalate content is 0, methanol content >=50%, DMC addition≤50%；The tower reactor produces
Product extraction group becomes dimethyl oxalate content >=99.9%, methanol content≤0.1%, DMC addition 0.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112007371A (en) * | 2020-08-12 | 2020-12-01 | 惠州市华达通气体制造股份有限公司 | Carbon dioxide purification device and feeding method thereof |
| CN112174821A (en) * | 2020-09-04 | 2021-01-05 | 中盐安徽红四方股份有限公司 | Rectification method of dimethyl oxalate |
| CN112479869A (en) * | 2020-12-10 | 2021-03-12 | 新疆天业汇合新材料有限公司 | Method for rectifying dimethyl oxalate in coal chemical industry |
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| CN113599851A (en) * | 2021-08-19 | 2021-11-05 | 南通百川新材料有限公司 | Novel light component removal and rectification system and method for propylene glycol methyl ether acetate |
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| CN113398619B (en) * | 2020-03-17 | 2023-07-25 | 嘉兴金汇石化有限公司 | Method for improving distillation separation effect and distillation system |
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| CN113599851A (en) * | 2021-08-19 | 2021-11-05 | 南通百川新材料有限公司 | Novel light component removal and rectification system and method for propylene glycol methyl ether acetate |
| CN113813623A (en) * | 2021-09-15 | 2021-12-21 | 常州冀德环保科技有限公司 | MVR concentration and rectification system and recovery method of DMAC waste liquid |
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